# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
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data_8280sadabs
_database_code_depnum_ccdc_archive 'CCDC 1407663'
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_audit_block_code KOZ-CA-325-03
_audit_creation_date 2013-05-28
_audit_creation_method
;
Olex2 1.2
(compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_compound_source dimethylsulfoxid,diethylether
_chemical_name_common ?
_chemical_name_systematic
;
Title
;
_chemical_formula_moiety 'C17 H20 N2 P CL3 PT'
_chemical_formula_sum 'C17 H20 Cl3 N2 P Pt'
_chemical_formula_weight 584.76
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
_symmetry_cell_setting MONOCLINIC
_symmetry_space_group_name_H-M P21/n
_symmetry_space_group_name_Hall '-p 2yn'
_symmetry_Int_Tables_number 14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 10.6985(8)
_cell_length_b 17.0969(13)
_cell_length_c 10.7451(11)
_cell_angle_alpha 90
_cell_angle_beta 91.790(7)
_cell_angle_gamma 90
_cell_volume 1964.4(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 24050
_cell_measurement_temperature 150
_cell_measurement_theta_max 33.0995
_cell_measurement_theta_min 2.6407
_exptl_absorpt_coefficient_mu 7.634
_exptl_absorpt_correction_T_max 0.68843
_exptl_absorpt_correction_T_min 0.59913
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.977
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 0.00 0.0300
0.00 1.00 0.00 0.0300
1.00 0.00 -1.00 0.0350
-1.00 0.00 1.00 0.0350
-1.00 0.00 -1.00 0.0350
1.00 0.00 1.00 0.0350
-1.00 2.00 -1.00 0.0300
1.00 -2.00 1.00 0.0300
-1.00 -2.00 -1.00 0.0300
1.00 2.00 1.00 0.0300
_exptl_crystal_description prism
_exptl_crystal_F_000 1120
_exptl_crystal_size_max 0.07
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.06
_exptl_special_details
;
Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0627
_diffrn_reflns_av_unetI/netI 0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 22176
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 33.166
_diffrn_reflns_theta_min 2.646
_diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method 'CCD \f- and \w-scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5707
_reflns_number_total 7474
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'DENZO (Bruker AXS, 2006)'
_computing_data_collection 'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction 'DENZO (Bruker AXS, 2006)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 2005)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max 2.540
_refine_diff_density_min -6.738
_refine_diff_density_rms 0.323
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 219
_refine_ls_number_reflns 7474
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0775
_refine_ls_R_factor_gt 0.0563
_refine_ls_restrained_S_all 1.033
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0919P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1374
_refine_ls_wR_factor_ref 0.1527
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The minimum and maximum estimated transmissions from the multi-scan
scaling are 0.4414 and 0.8480 (SADABS).
Highest peak ?
Deepest hole ?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C2(H2A,H2B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.25056(2) 0.35776(2) 0.85610(2) 0.02098(8) Uani 1 1 d . . . . .
Cl1 Cl 0.37739(12) 0.39858(9) 0.69859(14) 0.0283(3) Uani 1 1 d . . . . .
Cl2 Cl 0.40468(14) 0.40070(10) 1.00036(16) 0.0352(3) Uani 1 1 d . . . . .
Cl3 Cl 0.13824(15) 0.30648(10) 1.01707(14) 0.0349(3) Uani 1 1 d . . . . .
P1 P 0.09346(12) 0.32165(8) 0.73021(13) 0.0195(3) Uani 1 1 d . . . . .
N1 N 0.1763(4) 0.1702(3) 0.6892(4) 0.0232(9) Uani 1 1 d . . . . .
N2 N 0.0085(5) 0.1689(3) 0.8026(5) 0.0255(9) Uani 1 1 d . . . . .
C1 C 0.0875(5) 0.2123(3) 0.7396(5) 0.0205(10) Uani 1 1 d . . . . .
C2 C 0.1559(6) 0.0852(3) 0.7111(6) 0.0269(11) Uani 1 1 d . . . . .
H2A H 0.2298 0.0608 0.7530 0.032 Uiso 1 1 calc R U . . .
H2B H 0.1365 0.0572 0.6322 0.032 Uiso 1 1 calc R U . . .
C3 C 0.0447(6) 0.0860(4) 0.7948(7) 0.0336(13) Uani 1 1 d . . . . .
H3A H -0.0248 0.0543 0.7585 0.040 Uiso 1 1 calc R U . . .
H3B H 0.0679 0.0651 0.8783 0.040 Uiso 1 1 calc R U . . .
C4 C 0.2801(5) 0.1952(4) 0.6129(6) 0.0291(12) Uani 1 1 d . . . . .
H4A H 0.3554 0.1655 0.6368 0.044 Uiso 1 1 calc R U . . .
H4B H 0.2957 0.2512 0.6260 0.044 Uiso 1 1 calc R U . . .
H4C H 0.2587 0.1858 0.5248 0.044 Uiso 1 1 calc R U . . .
C5 C -0.0974(6) 0.1892(4) 0.8743(7) 0.0389(15) Uani 1 1 d . . . . .
H5A H -0.1733 0.1876 0.8209 0.058 Uiso 1 1 calc R U . . .
H5B H -0.0861 0.2420 0.9083 0.058 Uiso 1 1 calc R U . . .
H5C H -0.1051 0.1518 0.9427 0.058 Uiso 1 1 calc R U . . .
C6 C 0.0930(5) 0.3411(3) 0.5634(5) 0.0224(10) Uani 1 1 d . . . . .
C7 C 0.0516(5) 0.2868(4) 0.4745(5) 0.0268(11) Uani 1 1 d . . . . .
H7 H 0.0294 0.2354 0.4992 0.032 Uiso 1 1 calc R U . . .
C8 C 0.0429(6) 0.3082(4) 0.3492(6) 0.0333(13) Uani 1 1 d . . . . .
H8 H 0.0183 0.2710 0.2874 0.040 Uiso 1 1 calc R U . . .
C9 C 0.0713(6) 0.3856(4) 0.3159(6) 0.0352(14) Uani 1 1 d . . . . .
H9 H 0.0636 0.4008 0.2310 0.042 Uiso 1 1 calc R U . . .
C10 C 0.1099(6) 0.4394(4) 0.4034(6) 0.0317(12) Uani 1 1 d . . . . .
H10 H 0.1287 0.4914 0.3791 0.038 Uiso 1 1 calc R U . . .
C11 C 0.1216(5) 0.4174(3) 0.5293(6) 0.0262(11) Uani 1 1 d . . . . .
H11 H 0.1487 0.4543 0.5905 0.031 Uiso 1 1 calc R U . . .
C12 C -0.0595(5) 0.3603(3) 0.7676(6) 0.0238(11) Uani 1 1 d . . . . .
C13 C -0.0699(5) 0.4203(3) 0.8570(5) 0.0251(11) Uani 1 1 d . . . . .
H13 H 0.0025 0.4383 0.9016 0.030 Uiso 1 1 calc R U . . .
C14 C -0.1849(6) 0.4528(4) 0.8795(6) 0.0285(12) Uani 1 1 d . . . . .
H14 H -0.1912 0.4940 0.9384 0.034 Uiso 1 1 calc R U . . .
C15 C -0.2927(5) 0.4253(4) 0.8157(7) 0.0330(14) Uani 1 1 d . . . . .
H15 H -0.3722 0.4467 0.8336 0.040 Uiso 1 1 calc R U . . .
C16 C -0.2834(6) 0.3673(4) 0.7272(7) 0.0338(14) Uani 1 1 d . . . . .
H16 H -0.3569 0.3489 0.6848 0.041 Uiso 1 1 calc R U . . .
C17 C -0.1669(5) 0.3349(4) 0.6988(6) 0.0287(12) Uani 1 1 d . . . . .
H17 H -0.1604 0.2969 0.6348 0.034 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.01382(10) 0.02446(12) 0.02438(12) -0.00300(7) -0.00409(7) 0.00208(6)
Cl1 0.0168(5) 0.0332(7) 0.0350(7) -0.0027(6) 0.0020(5) -0.0044(5)
Cl2 0.0243(6) 0.0401(8) 0.0402(8) -0.0127(6) -0.0141(6) 0.0059(6)
Cl3 0.0301(7) 0.0492(9) 0.0253(7) 0.0061(6) -0.0007(6) 0.0030(6)
P1 0.0131(5) 0.0229(6) 0.0224(6) -0.0012(5) -0.0014(5) 0.0006(4)
N1 0.021(2) 0.025(2) 0.024(2) 0.0010(18) 0.0008(18) 0.0009(17)
N2 0.019(2) 0.028(2) 0.028(2) 0.003(2) 0.0010(18) -0.0012(18)
C1 0.017(2) 0.022(2) 0.022(2) -0.0009(19) -0.0049(18) 0.0001(18)
C2 0.026(3) 0.023(3) 0.031(3) 0.002(2) -0.003(2) 0.002(2)
C3 0.031(3) 0.030(3) 0.040(3) 0.007(3) -0.001(3) -0.001(2)
C4 0.017(2) 0.039(3) 0.032(3) -0.005(3) 0.005(2) 0.001(2)
C5 0.027(3) 0.041(4) 0.049(4) 0.006(3) 0.015(3) 0.000(3)
C6 0.017(2) 0.028(2) 0.022(2) 0.002(2) -0.0015(19) -0.0013(19)
C7 0.021(2) 0.031(3) 0.028(3) 0.000(2) 0.001(2) 0.000(2)
C8 0.033(3) 0.037(3) 0.030(3) -0.002(3) -0.005(3) 0.003(3)
C9 0.032(3) 0.047(4) 0.027(3) 0.011(3) -0.002(2) 0.006(3)
C10 0.033(3) 0.034(3) 0.029(3) 0.006(2) 0.004(2) 0.003(2)
C11 0.021(2) 0.027(3) 0.030(3) 0.000(2) 0.000(2) 0.002(2)
C12 0.017(2) 0.027(3) 0.027(3) 0.005(2) -0.002(2) -0.0007(18)
C13 0.019(2) 0.029(3) 0.027(3) 0.001(2) 0.001(2) 0.001(2)
C14 0.025(3) 0.028(3) 0.033(3) 0.003(2) 0.007(2) 0.007(2)
C15 0.018(2) 0.035(3) 0.046(4) 0.010(3) 0.008(2) 0.005(2)
C16 0.015(2) 0.042(4) 0.044(4) 0.001(3) -0.002(2) 0.005(2)
C17 0.014(2) 0.032(3) 0.040(3) 0.002(3) -0.001(2) -0.002(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 Cl1 2.3100(15) . ?
Pt1 Cl2 2.3454(14) . ?
Pt1 Cl3 2.3097(16) . ?
Pt1 P1 2.2122(13) . ?
P1 C1 1.874(5) . ?
P1 C6 1.823(6) . ?
P1 C12 1.821(6) . ?
N1 C1 1.322(7) . ?
N1 C2 1.489(7) . ?
N1 C4 1.465(8) . ?
N2 C1 1.325(7) . ?
N2 C3 1.472(8) . ?
N2 C5 1.432(8) . ?
C2 C3 1.515(9) . ?
C6 C7 1.394(8) . ?
C6 C11 1.392(8) . ?
C7 C8 1.395(9) . ?
C8 C9 1.407(10) . ?
C9 C10 1.370(10) . ?
C10 C11 1.406(8) . ?
C12 C13 1.412(8) . ?
C12 C17 1.414(8) . ?
C13 C14 1.378(8) . ?
C14 C15 1.405(10) . ?
C15 C16 1.381(10) . ?
C16 C17 1.406(8) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pt1 Cl2 88.44(6) . . ?
Cl3 Pt1 Cl1 174.07(5) . . ?
Cl3 Pt1 Cl2 89.73(6) . . ?
P1 Pt1 Cl1 95.09(5) . . ?
P1 Pt1 Cl2 175.21(5) . . ?
P1 Pt1 Cl3 87.07(5) . . ?
C1 P1 Pt1 105.79(16) . . ?
C6 P1 Pt1 121.93(18) . . ?
C6 P1 C1 103.6(3) . . ?
C12 P1 Pt1 115.8(2) . . ?
C12 P1 C1 108.5(2) . . ?
C12 P1 C6 100.1(3) . . ?
C1 N1 C2 110.8(5) . . ?
C1 N1 C4 129.7(5) . . ?
C4 N1 C2 119.4(5) . . ?
C1 N2 C3 109.7(5) . . ?
C1 N2 C5 131.8(5) . . ?
C5 N2 C3 118.5(5) . . ?
N1 C1 P1 119.6(4) . . ?
N1 C1 N2 112.5(5) . . ?
N2 C1 P1 127.5(4) . . ?
N1 C2 C3 101.9(5) . . ?
N2 C3 C2 104.8(5) . . ?
C7 C6 P1 122.9(4) . . ?
C11 C6 P1 115.8(4) . . ?
C11 C6 C7 120.8(5) . . ?
C6 C7 C8 119.8(6) . . ?
C7 C8 C9 118.9(6) . . ?
C10 C9 C8 121.3(6) . . ?
C9 C10 C11 119.8(6) . . ?
C6 C11 C10 119.4(5) . . ?
C13 C12 P1 120.2(4) . . ?
C13 C12 C17 119.9(5) . . ?
C17 C12 P1 119.6(5) . . ?
C14 C13 C12 120.2(5) . . ?
C13 C14 C15 120.2(6) . . ?
C16 C15 C14 120.1(6) . . ?
C15 C16 C17 121.1(6) . . ?
C16 C17 C12 118.5(6) . . ?
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_shelx_res_checksum 4755
_shelx_res_file
;
TITL
CELL 0.71073 10.6985 17.0969 10.7451 90 91.79 90
ZERR 4 0.0008 0.0013 0.0011 0 0.007 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N P Cl Pt
UNIT 68 80 8 4 12 4
L.S. 10 0 0 511
PLAN 20
TEMP -173
fmap 2
acta
REM Z:/8280/8280sadabs.hkl
WGHT 0.091900
FVAR 0.07915
PT1 6 0.250564 0.357760 0.856099 11.00000 0.01382 0.02446 =
0.02438 -0.00300 -0.00409 0.00208
CL1 5 0.377391 0.398577 0.698587 11.00000 0.01679 0.03322 =
0.03502 -0.00271 0.00204 -0.00445
CL2 5 0.404681 0.400701 1.000360 11.00000 0.02429 0.04005 =
0.04023 -0.01269 -0.01411 0.00591
CL3 5 0.138238 0.306475 1.017073 11.00000 0.03006 0.04917 =
0.02529 0.00613 -0.00070 0.00300
P1 4 0.093456 0.321648 0.730213 11.00000 0.01309 0.02289 =
0.02245 -0.00124 -0.00136 0.00055
N1 3 0.176332 0.170214 0.689174 11.00000 0.02123 0.02491 =
0.02355 0.00099 0.00078 0.00085
N2 3 0.008494 0.168928 0.802558 11.00000 0.01945 0.02844 =
0.02849 0.00254 0.00095 -0.00119
C1 1 0.087474 0.212278 0.739634 11.00000 0.01726 0.02205 =
0.02195 -0.00087 -0.00487 0.00009
C2 1 0.155948 0.085231 0.711069 11.00000 0.02578 0.02320 =
0.03137 0.00179 -0.00325 0.00185
AFIX 23
H2A 2 0.229830 0.060814 0.753033 11.00000 -1.20000
H2B 2 0.136475 0.057224 0.632185 11.00000 -1.20000
AFIX 0
C3 1 0.044657 0.086039 0.794787 11.00000 0.03100 0.03020 =
0.03960 0.00671 -0.00091 -0.00111
AFIX 23
H3A 2 -0.024755 0.054290 0.758492 11.00000 -1.20000
H3B 2 0.067904 0.065149 0.878267 11.00000 -1.20000
AFIX 0
C4 1 0.280116 0.195245 0.612875 11.00000 0.01664 0.03896 =
0.03207 -0.00527 0.00525 0.00068
AFIX 137
H4A 2 0.355437 0.165538 0.636789 11.00000 -1.50000
H4B 2 0.295693 0.251174 0.625954 11.00000 -1.50000
H4C 2 0.258664 0.185773 0.524828 11.00000 -1.50000
AFIX 0
C5 1 -0.097369 0.189165 0.874309 11.00000 0.02715 0.04108 =
0.04943 0.00633 0.01461 0.00025
AFIX 137
H5A 2 -0.173295 0.187615 0.820928 11.00000 -1.50000
H5B 2 -0.086107 0.241964 0.908346 11.00000 -1.50000
H5C 2 -0.105141 0.151763 0.942746 11.00000 -1.50000
AFIX 0
C6 1 0.093028 0.341065 0.563415 11.00000 0.01692 0.02801 =
0.02208 0.00199 -0.00151 -0.00134
C7 1 0.051616 0.286780 0.474513 11.00000 0.02124 0.03109 =
0.02799 -0.00048 0.00086 -0.00042
AFIX 43
H7 2 0.029369 0.235397 0.499165 11.00000 -1.20000
AFIX 0
C8 1 0.042949 0.308153 0.349233 11.00000 0.03277 0.03655 =
0.03019 -0.00151 -0.00491 0.00348
AFIX 43
H8 2 0.018287 0.271029 0.287432 11.00000 -1.20000
AFIX 0
C9 1 0.071318 0.385557 0.315914 11.00000 0.03197 0.04684 =
0.02655 0.01059 -0.00169 0.00631
AFIX 43
H9 2 0.063580 0.400815 0.231009 11.00000 -1.20000
AFIX 0
C10 1 0.109886 0.439404 0.403409 11.00000 0.03250 0.03351 =
0.02931 0.00598 0.00441 0.00276
AFIX 43
H10 2 0.128667 0.491409 0.379087 11.00000 -1.20000
AFIX 0
C11 1 0.121563 0.417411 0.529307 11.00000 0.02079 0.02732 =
0.03046 -0.00004 0.00013 0.00156
AFIX 43
H11 2 0.148666 0.454295 0.590524 11.00000 -1.20000
AFIX 0
C12 1 -0.059521 0.360259 0.767571 11.00000 0.01702 0.02699 =
0.02735 0.00484 -0.00174 -0.00071
C13 1 -0.069920 0.420283 0.856957 11.00000 0.01874 0.02918 =
0.02745 0.00105 0.00065 0.00058
AFIX 43
H13 2 0.002522 0.438269 0.901640 11.00000 -1.20000
AFIX 0
C14 1 -0.184864 0.452841 0.879548 11.00000 0.02477 0.02829 =
0.03291 0.00256 0.00682 0.00694
AFIX 43
H14 2 -0.191171 0.494001 0.938413 11.00000 -1.20000
AFIX 0
C15 1 -0.292715 0.425312 0.815749 11.00000 0.01756 0.03539 =
0.04640 0.01032 0.00786 0.00461
AFIX 43
H15 2 -0.372163 0.446662 0.833562 11.00000 -1.20000
AFIX 0
C16 1 -0.283393 0.367262 0.727183 11.00000 0.01485 0.04220 =
0.04412 0.00105 -0.00169 0.00466
AFIX 43
H16 2 -0.356896 0.348882 0.684764 11.00000 -1.20000
AFIX 0
C17 1 -0.166857 0.334912 0.698762 11.00000 0.01425 0.03172 =
0.04005 0.00174 -0.00052 -0.00207
AFIX 43
H17 2 -0.160377 0.296898 0.634802 11.00000 -1.20000
AFIX 0
HKLF 4
REM
REM R1 = 0.0563 for 5707 Fo > 4sig(Fo) and 0.0775 for all 7474 data
REM 219 parameters refined using 0 restraints
END
WGHT 0.0919 0.0000
REM Highest difference peak 2.540, deepest hole -6.738, 1-sigma level 0.323
Q1 1 0.2586 0.3568 0.7556 11.00000 0.05 2.54
Q2 1 0.3038 0.3875 0.7817 11.00000 0.05 2.32
Q3 1 0.3010 0.3295 0.7842 11.00000 0.05 2.15
Q4 1 0.2067 0.3213 0.9265 11.00000 0.05 2.06
Q5 1 0.2545 0.3571 0.9606 11.00000 0.05 2.00
Q6 1 0.2629 0.4109 0.8171 11.00000 0.05 1.88
Q7 1 0.1974 0.3898 0.9264 11.00000 0.05 1.88
Q8 1 0.2349 0.4082 0.8960 11.00000 0.05 1.56
Q9 1 -0.2516 0.1406 0.9353 11.00000 0.05 1.55
Q10 1 0.2583 0.3060 0.8133 11.00000 0.05 1.54
Q11 1 0.2510 0.4271 0.6382 11.00000 0.05 1.20
Q12 1 0.1674 0.2773 0.9240 11.00000 0.05 1.09
Q13 1 0.2748 0.2741 0.9227 11.00000 0.05 1.05
Q14 1 0.1817 0.3706 0.7203 11.00000 0.05 1.02
Q15 1 0.2920 0.2689 0.7843 11.00000 0.05 1.02
Q16 1 0.1124 0.3311 0.6343 11.00000 0.05 1.02
Q17 1 0.4065 0.3227 0.9895 11.00000 0.05 0.94
Q18 1 0.2908 0.4460 0.7849 11.00000 0.05 0.91
Q19 1 -0.1185 0.4190 0.9288 11.00000 0.05 0.88
Q20 1 0.4590 0.4323 0.9132 11.00000 0.05 0.86
;
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number 2013-3
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_8585sadabs
_database_code_depnum_ccdc_archive 'CCDC 1407664'
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_audit_block_code KOZ-KB-089-01
_audit_creation_date 2013-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_chemical_name_common ?
_chemical_name_systematic
;
Title
;
_chemical_formula_moiety 'C17 H32 N2 P, B F4 '
_chemical_formula_sum 'C17 H32 B F4 N2 P'
_chemical_formula_weight 382.22
_chemical_compound_source dichloromethane
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
_symmetry_cell_setting MONOCLINIC
_symmetry_space_group_name_H-M P21/n
_symmetry_space_group_name_Hall '-p 2yn'
_symmetry_Int_Tables_number 14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.3705(5)
_cell_length_b 22.6919(9)
_cell_length_c 15.1987(6)
_cell_angle_alpha 90
_cell_angle_beta 113.6237(13)
_cell_angle_gamma 90
_cell_volume 3908.9(3)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9903
_cell_measurement_temperature 100
_cell_measurement_theta_max 67.4594
_cell_measurement_theta_min 3.7243
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.598
_exptl_absorpt_correction_T_max 0.89377
_exptl_absorpt_correction_T_min 0.65311
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.299
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 -1.00 0.00 0.0500
0.00 2.00 1.00 0.1100
0.00 -2.00 -1.00 0.1600
3.00 2.00 0.00 0.0400
0.00 1.00 0.00 0.0200
0.00 -1.00 0.00 0.0800
-1.00 0.00 1.00 0.1500
1.00 0.00 -1.00 0.1800
-1.00 -2.00 2.00 0.1700
1.00 2.00 -2.00 0.1700
_exptl_crystal_description needle
_exptl_crystal_F_000 1632
_exptl_crystal_size_max 0.33
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.10
_exptl_special_details
;
Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0467
_diffrn_reflns_av_unetI/netI 0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 92285
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 67.698
_diffrn_reflns_theta_min 3.724
_diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_monochromator 'focusing multilayer optic'
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker AXS X8 Proteum'
_diffrn_measurement_method 'CCD \f- and \w-scans'
_diffrn_radiation_type Cu-K\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6294
_reflns_number_total 7040
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT software (Bruker AXS, 2004)'
_computing_data_collection 'PROTEUM2 (Bruker AXS, 2008)'
_computing_data_reduction 'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 2005)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick, 2008)'
_computing_structure_solution 'SHELXS-97 (G. M. Sheldrick, 2008)'
_refine_diff_density_max 0.639
_refine_diff_density_min -0.495
_refine_diff_density_rms 0.053
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 455
_refine_ls_number_reflns 7040
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0464
_refine_ls_R_factor_gt 0.0409
_refine_ls_restrained_S_all 1.055
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+3.5018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1005
_refine_ls_wR_factor_ref 0.1046
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The minimum and maximum estimated transmissions from the multi-scan
scaling are 0.6025 and 0.8997 (SADABS).
Highest peak ?
Deepest hole ?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C26(H26), C32(H32), C6(H6), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
C22(H22A,H22B), C23(H23A,H23B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B),
C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C2(H2A,H2B), C3(H3A,H3B),
C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B)
2.c Idealised Me refined as rotating group:
C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P11 P 0.02536(4) 0.41654(2) 0.72706(3) 0.01715(11) Uani 1 1 d . . . . .
N11 N 0.11497(13) 0.29796(6) 0.74576(11) 0.0195(3) Uani 1 1 d . . . . .
N12 N 0.24812(13) 0.36617(7) 0.80815(11) 0.0221(3) Uani 1 1 d . . . . .
C21 C 0.13390(15) 0.35498(8) 0.76070(12) 0.0177(4) Uani 1 1 d . . . . .
C22 C 0.22581(16) 0.26415(9) 0.78369(14) 0.0256(4) Uani 1 1 d . . . . .
H22A H 0.2410 0.2450 0.7312 0.031 Uiso 1 1 calc R . . . .
H22B H 0.2242 0.2337 0.8298 0.031 Uiso 1 1 calc R . . . .
C23 C 0.31806(16) 0.31128(9) 0.83351(14) 0.0262(4) Uani 1 1 d . . . . .
H23A H 0.3541 0.3052 0.9039 0.031 Uiso 1 1 calc R . . . .
H23B H 0.3810 0.3116 0.8089 0.031 Uiso 1 1 calc R . . . .
C24 C 0.00513(16) 0.26600(8) 0.69813(14) 0.0232(4) Uani 1 1 d . . . . .
H24A H -0.0615 0.2926 0.6871 0.035 Uiso 1 1 calc GR . . . .
H24B H 0.0019 0.2331 0.7387 0.035 Uiso 1 1 calc GR . . . .
H24C H 0.0009 0.2508 0.6365 0.035 Uiso 1 1 calc GR . . . .
C25 C 0.30492(17) 0.42344(9) 0.83494(14) 0.0272(4) Uani 1 1 d . . . . .
H25A H 0.2768 0.4495 0.7789 0.041 Uiso 1 1 calc GR . . . .
H25B H 0.3906 0.4187 0.8580 0.041 Uiso 1 1 calc GR . . . .
H25C H 0.2856 0.4406 0.8860 0.041 Uiso 1 1 calc GR . . . .
C26 C -0.04875(15) 0.39547(7) 0.80833(12) 0.0182(4) Uani 1 1 d . . . . .
H26 H -0.0507 0.3515 0.8123 0.022 Uiso 1 1 calc R . . . .
C27 C 0.02557(16) 0.42022(9) 0.90846(13) 0.0238(4) Uani 1 1 d . . . . .
H27A H 0.1047 0.4017 0.9333 0.029 Uiso 1 1 calc R . . . .
H27B H 0.0359 0.4632 0.9036 0.029 Uiso 1 1 calc R . . . .
C28 C -0.03224(16) 0.40880(9) 0.97863(13) 0.0260(4) Uani 1 1 d . . . . .
H28A H 0.0155 0.4274 1.0411 0.031 Uiso 1 1 calc R . . . .
H28B H -0.0344 0.3658 0.9892 0.031 Uiso 1 1 calc R . . . .
C29 C -0.15763(16) 0.43338(8) 0.94071(13) 0.0229(4) Uani 1 1 d . . . . .
H29A H -0.1943 0.4236 0.9860 0.028 Uiso 1 1 calc R . . . .
H29B H -0.1552 0.4768 0.9360 0.028 Uiso 1 1 calc R . . . .
C30 C -0.23138(15) 0.40765(8) 0.84250(13) 0.0202(4) Uani 1 1 d . . . . .
H30A H -0.3112 0.4253 0.8180 0.024 Uiso 1 1 calc R . . . .
H30B H -0.2399 0.3646 0.8487 0.024 Uiso 1 1 calc R . . . .
C31 C -0.17563(15) 0.41902(8) 0.77066(13) 0.0204(4) Uani 1 1 d . . . . .
H31A H -0.1753 0.4619 0.7588 0.024 Uiso 1 1 calc R . . . .
H31B H -0.2235 0.3996 0.7089 0.024 Uiso 1 1 calc R . . . .
C32 C -0.07526(15) 0.39766(8) 0.60164(12) 0.0184(4) Uani 1 1 d . . . . .
H32 H -0.1284 0.3646 0.6021 0.022 Uiso 1 1 calc R . . . .
C33 C -0.14950(16) 0.45276(8) 0.55615(13) 0.0226(4) Uani 1 1 d . . . . .
H33A H -0.1964 0.4640 0.5932 0.027 Uiso 1 1 calc R . . . .
H33B H -0.0965 0.4860 0.5587 0.027 Uiso 1 1 calc R . . . .
C34 C -0.23229(16) 0.44066(9) 0.45176(13) 0.0256(4) Uani 1 1 d . . . . .
H34A H -0.2888 0.4093 0.4497 0.031 Uiso 1 1 calc R . . . .
H34B H -0.2779 0.4767 0.4233 0.031 Uiso 1 1 calc R . . . .
C35 C -0.16319(17) 0.42164(9) 0.39279(13) 0.0269(4) Uani 1 1 d . . . . .
H35A H -0.2189 0.4116 0.3267 0.032 Uiso 1 1 calc R . . . .
H35B H -0.1129 0.4546 0.3888 0.032 Uiso 1 1 calc R . . . .
C36 C -0.08615(17) 0.36833(9) 0.43859(13) 0.0254(4) Uani 1 1 d . . . . .
H36A H -0.0383 0.3583 0.4018 0.030 Uiso 1 1 calc R . . . .
H36B H -0.1373 0.3341 0.4354 0.030 Uiso 1 1 calc R . . . .
C37 C -0.00420(15) 0.37980(8) 0.54310(13) 0.0201(4) Uani 1 1 d . . . . .
H37A H 0.0519 0.4116 0.5461 0.024 Uiso 1 1 calc R . . . .
H37B H 0.0419 0.3438 0.5711 0.024 Uiso 1 1 calc R . . . .
P1 P 0.73352(4) 0.59438(2) 0.68283(3) 0.01650(11) Uani 1 1 d . . . . .
N1 N 0.95570(13) 0.64598(7) 0.76433(11) 0.0215(3) Uani 1 1 d . . . . .
N2 N 0.81833(12) 0.71342(6) 0.72508(11) 0.0192(3) Uani 1 1 d . . . . .
C1 C 0.84017(15) 0.65631(8) 0.72797(12) 0.0176(4) Uani 1 1 d . . . . .
C2 C 1.02372(16) 0.70107(9) 0.79207(15) 0.0289(4) Uani 1 1 d . . . . .
H2A H 1.0776 0.7053 0.7588 0.035 Uiso 1 1 calc R . . . .
H2B H 1.0703 0.7028 0.8623 0.035 Uiso 1 1 calc R . . . .
C3 C 0.92787(16) 0.74823(8) 0.75964(14) 0.0265(4) Uani 1 1 d . . . . .
H3A H 0.9334 0.7741 0.8138 0.032 Uiso 1 1 calc R . . . .
H3B H 0.9330 0.7727 0.7075 0.032 Uiso 1 1 calc R . . . .
C4 C 1.01687(17) 0.58971(9) 0.77900(14) 0.0265(4) Uani 1 1 d . . . . .
H4A H 0.9595 0.5575 0.7647 0.040 Uiso 1 1 calc GR . . . .
H4B H 1.0737 0.5867 0.8459 0.040 Uiso 1 1 calc GR . . . .
H4C H 1.0586 0.5870 0.7363 0.040 Uiso 1 1 calc GR . . . .
C5 C 0.70613(15) 0.74406(8) 0.69097(14) 0.0215(4) Uani 1 1 d . . . . .
H5A H 0.6914 0.7627 0.6291 0.032 Uiso 1 1 calc GR . . . .
H5B H 0.7082 0.7743 0.7376 0.032 Uiso 1 1 calc GR . . . .
H5C H 0.6429 0.7159 0.6832 0.032 Uiso 1 1 calc GR . . . .
C6 C 0.63574(15) 0.60602(7) 0.74812(13) 0.0183(4) Uani 1 1 d . . . . .
H6 H 0.5812 0.6397 0.7186 0.022 Uiso 1 1 calc R . . . .
C7 C 0.70902(16) 0.61888(8) 0.85459(13) 0.0236(4) Uani 1 1 d . . . . .
H7A H 0.7705 0.5882 0.8810 0.028 Uiso 1 1 calc R . . . .
H7B H 0.7492 0.6573 0.8605 0.028 Uiso 1 1 calc R . . . .
C8 C 0.63422(17) 0.62040(8) 0.91345(14) 0.0246(4) Uani 1 1 d . . . . .
H8A H 0.6866 0.6255 0.9821 0.030 Uiso 1 1 calc R . . . .
H8B H 0.5806 0.6548 0.8935 0.030 Uiso 1 1 calc R . . . .
C9 C 0.56135(18) 0.56469(9) 0.90170(14) 0.0278(4) Uani 1 1 d . . . . .
H9A H 0.5094 0.5690 0.9367 0.033 Uiso 1 1 calc R . . . .
H9B H 0.6143 0.5307 0.9291 0.033 Uiso 1 1 calc R . . . .
C10 C 0.48691(19) 0.55387(11) 0.79561(15) 0.0372(5) Uani 1 1 d . . . . .
H10A H 0.4298 0.5865 0.7698 0.045 Uiso 1 1 calc R . . . .
H10B H 0.4417 0.5169 0.7882 0.045 Uiso 1 1 calc R . . . .
C11 C 0.56375(18) 0.54950(9) 0.73861(14) 0.0301(5) Uani 1 1 d . . . . .
H11A H 0.5130 0.5425 0.6701 0.036 Uiso 1 1 calc R . . . .
H11B H 0.6181 0.5156 0.7622 0.036 Uiso 1 1 calc R . . . .
C12 C 0.65176(15) 0.62160(7) 0.55820(12) 0.0178(4) Uani 1 1 d . . . . .
H12 H 0.6148 0.6605 0.5603 0.021 Uiso 1 1 calc R . . . .
C13 C 0.55459(15) 0.57713(8) 0.50304(13) 0.0208(4) Uani 1 1 d . . . . .
H13A H 0.5903 0.5378 0.5055 0.025 Uiso 1 1 calc R . . . .
H13B H 0.4981 0.5741 0.5341 0.025 Uiso 1 1 calc R . . . .
C14 C 0.48895(15) 0.59579(8) 0.39844(13) 0.0218(4) Uani 1 1 d . . . . .
H14A H 0.4300 0.5653 0.3639 0.026 Uiso 1 1 calc R . . . .
H14B H 0.4461 0.6330 0.3959 0.026 Uiso 1 1 calc R . . . .
C15 C 0.57264(16) 0.60456(8) 0.34852(13) 0.0235(4) Uani 1 1 d . . . . .
H15A H 0.5279 0.6196 0.2827 0.028 Uiso 1 1 calc R . . . .
H15B H 0.6080 0.5662 0.3435 0.028 Uiso 1 1 calc R . . . .
C16 C 0.67067(16) 0.64809(8) 0.40383(13) 0.0235(4) Uani 1 1 d . . . . .
H16A H 0.6360 0.6876 0.4018 0.028 Uiso 1 1 calc R . . . .
H16B H 0.7269 0.6508 0.3725 0.028 Uiso 1 1 calc R . . . .
C17 C 0.73697(15) 0.62929(8) 0.50845(13) 0.0208(4) Uani 1 1 d . . . . .
H17A H 0.7968 0.6595 0.5429 0.025 Uiso 1 1 calc R . . . .
H17B H 0.7786 0.5917 0.5109 0.025 Uiso 1 1 calc R . . . .
F5 F 0.24167(11) 0.20718(6) 0.49333(10) 0.0454(3) Uani 1 1 d . . . . .
F6 F 0.08256(10) 0.14672(6) 0.44161(10) 0.0425(3) Uani 1 1 d . . . . .
F7 F 0.07044(14) 0.23759(8) 0.49681(17) 0.0898(7) Uani 1 1 d . . . . .
F8 F 0.17932(18) 0.16819(9) 0.60012(11) 0.0832(6) Uani 1 1 d . . . . .
B2 B 0.1431(2) 0.19000(11) 0.50743(18) 0.0311(5) Uani 1 1 d . . . . .
F1 F 0.41118(10) 0.69202(5) 0.57748(8) 0.0331(3) Uani 1 1 d . . . . .
F2 F 0.46648(11) 0.75173(6) 0.48285(9) 0.0401(3) Uani 1 1 d . . . . .
F3 F 0.28425(11) 0.71275(7) 0.42447(9) 0.0514(4) Uani 1 1 d . . . . .
F4 F 0.33481(15) 0.78381(6) 0.54020(11) 0.0579(4) Uani 1 1 d . . . . .
B1 B 0.37328(19) 0.73522(10) 0.50603(16) 0.0247(5) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P11 0.0168(2) 0.0148(2) 0.0194(2) -0.00068(17) 0.00677(18) -0.00034(16)
N11 0.0164(7) 0.0187(7) 0.0226(8) 0.0012(6) 0.0072(6) 0.0030(6)
N12 0.0164(7) 0.0273(8) 0.0210(8) -0.0001(6) 0.0059(6) -0.0006(6)
C21 0.0153(8) 0.0228(9) 0.0159(8) 0.0008(7) 0.0073(7) -0.0005(7)
C22 0.0219(9) 0.0264(10) 0.0290(10) 0.0055(8) 0.0106(8) 0.0108(8)
C23 0.0174(9) 0.0351(11) 0.0250(10) 0.0056(8) 0.0073(8) 0.0073(8)
C24 0.0221(9) 0.0173(9) 0.0309(10) -0.0014(8) 0.0113(8) -0.0025(7)
C25 0.0198(9) 0.0339(11) 0.0254(10) -0.0018(8) 0.0065(8) -0.0088(8)
C26 0.0172(8) 0.0150(8) 0.0214(9) -0.0002(7) 0.0069(7) 0.0009(7)
C27 0.0177(9) 0.0311(10) 0.0216(9) -0.0031(8) 0.0069(8) 0.0006(7)
C28 0.0214(10) 0.0362(11) 0.0196(9) -0.0005(8) 0.0075(8) 0.0025(8)
C29 0.0230(9) 0.0233(9) 0.0242(10) -0.0029(8) 0.0112(8) 0.0011(7)
C30 0.0179(9) 0.0196(9) 0.0232(9) 0.0010(7) 0.0084(7) 0.0021(7)
C31 0.0189(9) 0.0209(9) 0.0203(9) -0.0001(7) 0.0067(7) 0.0021(7)
C32 0.0175(8) 0.0169(8) 0.0200(9) 0.0008(7) 0.0068(7) 0.0011(7)
C33 0.0235(9) 0.0211(9) 0.0244(10) 0.0030(7) 0.0107(8) 0.0054(7)
C34 0.0208(9) 0.0308(10) 0.0236(10) 0.0047(8) 0.0071(8) 0.0076(8)
C35 0.0239(10) 0.0357(11) 0.0191(9) 0.0023(8) 0.0066(8) 0.0055(8)
C36 0.0245(10) 0.0296(10) 0.0209(9) -0.0029(8) 0.0079(8) 0.0038(8)
C37 0.0169(8) 0.0222(9) 0.0214(9) 0.0006(7) 0.0079(7) 0.0030(7)
P1 0.0161(2) 0.0130(2) 0.0191(2) -0.00069(16) 0.00556(18) 0.00011(16)
N1 0.0146(7) 0.0257(8) 0.0223(8) -0.0009(6) 0.0056(6) 0.0004(6)
N2 0.0169(7) 0.0161(7) 0.0246(8) -0.0036(6) 0.0085(6) -0.0041(6)
C1 0.0161(8) 0.0211(9) 0.0154(8) -0.0010(7) 0.0061(7) 0.0005(7)
C2 0.0178(9) 0.0347(11) 0.0321(11) -0.0071(9) 0.0078(8) -0.0096(8)
C3 0.0226(9) 0.0246(10) 0.0308(10) -0.0061(8) 0.0093(8) -0.0115(8)
C4 0.0199(9) 0.0347(11) 0.0248(10) 0.0050(8) 0.0088(8) 0.0099(8)
C5 0.0213(9) 0.0146(8) 0.0280(10) -0.0009(7) 0.0093(8) 0.0003(7)
C6 0.0182(8) 0.0144(8) 0.0209(9) 0.0016(7) 0.0063(7) -0.0004(7)
C7 0.0230(9) 0.0241(9) 0.0228(9) -0.0041(8) 0.0083(8) -0.0070(7)
C8 0.0289(10) 0.0227(9) 0.0245(10) -0.0010(8) 0.0130(8) -0.0025(8)
C9 0.0304(10) 0.0287(10) 0.0264(10) 0.0014(8) 0.0137(8) -0.0059(8)
C10 0.0337(11) 0.0517(14) 0.0279(11) -0.0054(10) 0.0140(9) -0.0242(10)
C11 0.0352(11) 0.0284(11) 0.0268(10) -0.0056(8) 0.0125(9) -0.0166(9)
C12 0.0170(8) 0.0153(8) 0.0202(9) -0.0021(7) 0.0066(7) -0.0004(7)
C13 0.0191(9) 0.0197(9) 0.0221(9) -0.0025(7) 0.0066(7) -0.0037(7)
C14 0.0179(9) 0.0221(9) 0.0213(9) -0.0031(7) 0.0034(7) -0.0013(7)
C15 0.0235(9) 0.0255(9) 0.0185(9) -0.0006(7) 0.0055(7) 0.0032(7)
C16 0.0211(9) 0.0279(10) 0.0216(9) 0.0042(8) 0.0086(8) 0.0003(7)
C17 0.0175(9) 0.0224(9) 0.0212(9) 0.0006(7) 0.0065(7) -0.0006(7)
F5 0.0331(7) 0.0645(9) 0.0446(8) -0.0096(7) 0.0218(6) -0.0137(6)
F6 0.0270(6) 0.0430(7) 0.0482(8) -0.0188(6) 0.0054(6) -0.0014(5)
F7 0.0420(9) 0.0589(11) 0.1559(19) -0.0513(12) 0.0266(11) 0.0052(8)
F8 0.1025(14) 0.1092(15) 0.0375(9) -0.0077(9) 0.0277(9) -0.0542(12)
B2 0.0219(11) 0.0382(13) 0.0348(13) -0.0127(10) 0.0129(10) -0.0043(9)
F1 0.0347(6) 0.0277(6) 0.0326(6) 0.0076(5) 0.0089(5) 0.0073(5)
F2 0.0337(7) 0.0410(7) 0.0476(8) 0.0012(6) 0.0186(6) -0.0064(5)
F3 0.0329(7) 0.0731(10) 0.0337(7) 0.0061(7) -0.0021(6) -0.0192(7)
F4 0.0975(12) 0.0419(8) 0.0518(9) 0.0161(7) 0.0481(9) 0.0381(8)
B1 0.0233(11) 0.0257(11) 0.0237(11) 0.0026(9) 0.0079(9) 0.0059(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11 C21 1.8616(18) . ?
P11 C26 1.8715(18) . ?
P11 C32 1.8614(18) . ?
N11 C21 1.318(2) . ?
N11 C22 1.472(2) . ?
N11 C24 1.452(2) . ?
N12 C21 1.328(2) . ?
N12 C23 1.477(2) . ?
N12 C25 1.456(2) . ?
C22 C23 1.525(3) . ?
C26 C27 1.535(2) . ?
C26 C31 1.535(2) . ?
C27 C28 1.526(3) . ?
C28 C29 1.527(3) . ?
C29 C30 1.520(3) . ?
C30 C31 1.529(2) . ?
C32 C33 1.541(2) . ?
C32 C37 1.535(2) . ?
C33 C34 1.529(3) . ?
C34 C35 1.528(3) . ?
C35 C36 1.525(3) . ?
C36 C37 1.526(2) . ?
P1 C1 1.8603(18) . ?
P1 C6 1.8653(18) . ?
P1 C12 1.8593(18) . ?
N1 C1 1.330(2) . ?
N1 C2 1.471(2) . ?
N1 C4 1.455(2) . ?
N2 C1 1.321(2) . ?
N2 C3 1.472(2) . ?
N2 C5 1.450(2) . ?
C2 C3 1.525(3) . ?
C6 C7 1.533(2) . ?
C6 C11 1.535(2) . ?
C7 C8 1.524(3) . ?
C8 C9 1.521(3) . ?
C9 C10 1.522(3) . ?
C10 C11 1.524(3) . ?
C12 C13 1.536(2) . ?
C12 C17 1.534(2) . ?
C13 C14 1.527(2) . ?
C14 C15 1.522(3) . ?
C15 C16 1.528(3) . ?
C16 C17 1.529(2) . ?
F5 B2 1.376(3) . ?
F6 B2 1.388(3) . ?
F7 B2 1.372(3) . ?
F8 B2 1.387(3) . ?
F1 B1 1.397(2) . ?
F2 B1 1.385(3) . ?
F3 B1 1.384(3) . ?
F4 B1 1.382(3) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 P11 C26 96.73(8) . . ?
C32 P11 C21 102.79(8) . . ?
C32 P11 C26 108.28(8) . . ?
C21 N11 C22 111.76(15) . . ?
C21 N11 C24 129.97(15) . . ?
C24 N11 C22 118.27(15) . . ?
C21 N12 C23 111.39(15) . . ?
C21 N12 C25 127.73(16) . . ?
C25 N12 C23 120.88(15) . . ?
N11 C21 P11 129.08(13) . . ?
N11 C21 N12 110.99(15) . . ?
N12 C21 P11 119.92(13) . . ?
N11 C22 C23 102.90(15) . . ?
N12 C23 C22 102.60(14) . . ?
C27 C26 P11 107.68(12) . . ?
C27 C26 C31 111.04(14) . . ?
C31 C26 P11 111.28(12) . . ?
C28 C27 C26 111.64(15) . . ?
C27 C28 C29 111.34(15) . . ?
C30 C29 C28 110.46(15) . . ?
C29 C30 C31 111.81(15) . . ?
C30 C31 C26 111.18(14) . . ?
C33 C32 P11 107.85(12) . . ?
C37 C32 P11 110.56(12) . . ?
C37 C32 C33 109.32(14) . . ?
C34 C33 C32 110.53(15) . . ?
C35 C34 C33 111.09(15) . . ?
C36 C35 C34 110.52(16) . . ?
C35 C36 C37 111.90(15) . . ?
C36 C37 C32 110.65(14) . . ?
C1 P1 C6 102.25(8) . . ?
C12 P1 C1 98.08(8) . . ?
C12 P1 C6 106.92(8) . . ?
C1 N1 C2 111.43(15) . . ?
C1 N1 C4 128.63(16) . . ?
C4 N1 C2 119.94(15) . . ?
C1 N2 C3 111.59(15) . . ?
C1 N2 C5 129.50(15) . . ?
C5 N2 C3 118.87(14) . . ?
N1 C1 P1 120.34(13) . . ?
N2 C1 P1 128.57(13) . . ?
N2 C1 N1 110.97(15) . . ?
N1 C2 C3 102.84(14) . . ?
N2 C3 C2 102.95(15) . . ?
C7 C6 P1 110.69(12) . . ?
C7 C6 C11 109.51(15) . . ?
C11 C6 P1 107.89(12) . . ?
C8 C7 C6 112.50(15) . . ?
C9 C8 C7 112.53(16) . . ?
C8 C9 C10 109.68(16) . . ?
C9 C10 C11 111.23(17) . . ?
C10 C11 C6 111.26(17) . . ?
C13 C12 P1 108.97(12) . . ?
C17 C12 P1 109.84(11) . . ?
C17 C12 C13 110.36(14) . . ?
C14 C13 C12 111.07(15) . . ?
C15 C14 C13 111.78(15) . . ?
C14 C15 C16 111.01(15) . . ?
C15 C16 C17 111.62(15) . . ?
C16 C17 C12 110.87(14) . . ?
F5 B2 F6 110.12(18) . . ?
F5 B2 F8 108.26(18) . . ?
F7 B2 F5 109.8(2) . . ?
F7 B2 F6 109.47(18) . . ?
F7 B2 F8 109.3(2) . . ?
F8 B2 F6 109.9(2) . . ?
F2 B1 F1 109.46(16) . . ?
F3 B1 F1 109.65(17) . . ?
F3 B1 F2 108.46(17) . . ?
F4 B1 F1 109.06(17) . . ?
F4 B1 F2 109.08(18) . . ?
F4 B1 F3 111.11(18) . . ?
_shelx_res_file
;
TITL
CELL 1.54178 12.3705 22.6919 15.1987 90 113.6237 90
ZERR 8 0.0005 0.0009 0.0006 0 0.0013 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H B N F P
UNIT 136 256 8 16 32 8
L.S. 4 0 0
PLAN 20
TEMP -173
fmap 2 53
acta
REM Z:/8585/8585sadabs.hkl
WGHT 0.044100 3.501800
FVAR 0.08728
P11 6 0.025363 0.416537 0.727059 11.00000 0.01684 0.01480 =
0.01936 -0.00068 0.00677 -0.00034
N11 4 0.114968 0.297962 0.745758 11.00000 0.01644 0.01873 =
0.02260 0.00121 0.00716 0.00300
N12 4 0.248120 0.366174 0.808152 11.00000 0.01639 0.02725 =
0.02100 -0.00007 0.00590 -0.00060
C21 1 0.133903 0.354976 0.760701 11.00000 0.01533 0.02281 =
0.01592 0.00083 0.00734 -0.00055
C22 1 0.225806 0.264153 0.783687 11.00000 0.02188 0.02642 =
0.02901 0.00551 0.01058 0.01079
AFIX 23
H22A 2 0.241046 0.245006 0.731243 11.00000 -1.20000
H22B 2 0.224203 0.233687 0.829775 11.00000 -1.20000
AFIX 0
C23 1 0.318063 0.311276 0.833514 11.00000 0.01736 0.03507 =
0.02496 0.00559 0.00732 0.00735
AFIX 23
H23A 2 0.354107 0.305208 0.903907 11.00000 -1.20000
H23B 2 0.380982 0.311587 0.808856 11.00000 -1.20000
AFIX 0
C24 1 0.005132 0.266004 0.698130 11.00000 0.02212 0.01734 =
0.03091 -0.00137 0.01129 -0.00248
AFIX 137
H24A 2 -0.061525 0.292567 0.687063 11.00000 -1.50000
H24B 2 0.001891 0.233065 0.738705 11.00000 -1.50000
H24C 2 0.000890 0.250808 0.636474 11.00000 -1.50000
AFIX 0
C25 1 0.304923 0.423436 0.834936 11.00000 0.01978 0.03392 =
0.02539 -0.00180 0.00651 -0.00881
AFIX 137
H25A 2 0.276834 0.449547 0.778880 11.00000 -1.50000
H25B 2 0.390611 0.418674 0.857985 11.00000 -1.50000
H25C 2 0.285568 0.440641 0.885977 11.00000 -1.50000
AFIX 0
C26 1 -0.048749 0.395465 0.808330 11.00000 0.01719 0.01503 =
0.02142 -0.00024 0.00688 0.00089
AFIX 13
H26 2 -0.050665 0.351515 0.812302 11.00000 -1.20000
AFIX 0
C27 1 0.025571 0.420216 0.908458 11.00000 0.01772 0.03106 =
0.02157 -0.00305 0.00691 0.00058
AFIX 23
H27A 2 0.104668 0.401717 0.933266 11.00000 -1.20000
H27B 2 0.035935 0.463182 0.903594 11.00000 -1.20000
AFIX 0
C28 1 -0.032241 0.408803 0.978634 11.00000 0.02137 0.03624 =
0.01961 -0.00046 0.00751 0.00251
AFIX 23
H28A 2 0.015515 0.427433 1.041124 11.00000 -1.20000
H28B 2 -0.034382 0.365850 0.989235 11.00000 -1.20000
AFIX 0
C29 1 -0.157628 0.433376 0.940710 11.00000 0.02299 0.02331 =
0.02420 -0.00289 0.01120 0.00107
AFIX 23
H29A 2 -0.194315 0.423571 0.986016 11.00000 -1.20000
H29B 2 -0.155156 0.476827 0.935955 11.00000 -1.20000
AFIX 0
C30 1 -0.231376 0.407652 0.842496 11.00000 0.01786 0.01958 =
0.02323 0.00098 0.00845 0.00210
AFIX 23
H30A 2 -0.311196 0.425344 0.817959 11.00000 -1.20000
H30B 2 -0.239854 0.364648 0.848706 11.00000 -1.20000
AFIX 0
C31 1 -0.175625 0.419023 0.770661 11.00000 0.01888 0.02091 =
0.02025 -0.00012 0.00672 0.00211
AFIX 23
H31A 2 -0.175312 0.461905 0.758769 11.00000 -1.20000
H31B 2 -0.223484 0.399597 0.708922 11.00000 -1.20000
AFIX 0
C32 1 -0.075262 0.397661 0.601641 11.00000 0.01748 0.01691 =
0.02005 0.00079 0.00684 0.00106
AFIX 13
H32 2 -0.128412 0.364573 0.602129 11.00000 -1.20000
AFIX 0
C33 1 -0.149499 0.452756 0.556147 11.00000 0.02347 0.02112 =
0.02441 0.00301 0.01072 0.00541
AFIX 23
H33A 2 -0.196400 0.464046 0.593152 11.00000 -1.20000
H33B 2 -0.096514 0.485999 0.558656 11.00000 -1.20000
AFIX 0
C34 1 -0.232286 0.440657 0.451762 11.00000 0.02076 0.03077 =
0.02360 0.00475 0.00715 0.00759
AFIX 23
H34A 2 -0.288798 0.409256 0.449734 11.00000 -1.20000
H34B 2 -0.277934 0.476725 0.423300 11.00000 -1.20000
AFIX 0
C35 1 -0.163193 0.421635 0.392792 11.00000 0.02392 0.03567 =
0.01906 0.00232 0.00656 0.00549
AFIX 23
H35A 2 -0.218870 0.411620 0.326722 11.00000 -1.20000
H35B 2 -0.112932 0.454615 0.388847 11.00000 -1.20000
AFIX 0
C36 1 -0.086151 0.368332 0.438594 11.00000 0.02453 0.02964 =
0.02091 -0.00288 0.00790 0.00384
AFIX 23
H36A 2 -0.038333 0.358337 0.401763 11.00000 -1.20000
H36B 2 -0.137276 0.334133 0.435420 11.00000 -1.20000
AFIX 0
C37 1 -0.004203 0.379799 0.543095 11.00000 0.01695 0.02221 =
0.02135 0.00058 0.00795 0.00300
AFIX 23
H37A 2 0.051924 0.411627 0.546142 11.00000 -1.20000
H37B 2 0.041861 0.343758 0.571061 11.00000 -1.20000
AFIX 0
P1 6 0.733518 0.594377 0.682832 11.00000 0.01607 0.01296 =
0.01907 -0.00069 0.00556 0.00011
N1 4 0.955698 0.645983 0.764327 11.00000 0.01457 0.02575 =
0.02234 -0.00089 0.00559 0.00038
N2 4 0.818332 0.713418 0.725084 11.00000 0.01695 0.01606 =
0.02465 -0.00360 0.00852 -0.00411
C1 1 0.840166 0.656308 0.727967 11.00000 0.01614 0.02114 =
0.01540 -0.00100 0.00613 0.00048
C2 1 1.023724 0.701069 0.792065 11.00000 0.01784 0.03469 =
0.03211 -0.00712 0.00776 -0.00959
AFIX 23
H2A 2 1.077593 0.705338 0.758758 11.00000 -1.20000
H2B 2 1.070277 0.702803 0.862304 11.00000 -1.20000
AFIX 0
C3 1 0.927872 0.748230 0.759637 11.00000 0.02260 0.02459 =
0.03081 -0.00609 0.00927 -0.01153
AFIX 23
H3A 2 0.933377 0.774058 0.813769 11.00000 -1.20000
H3B 2 0.933044 0.772713 0.707549 11.00000 -1.20000
AFIX 0
C4 1 1.016868 0.589707 0.779000 11.00000 0.01990 0.03470 =
0.02480 0.00502 0.00881 0.00988
AFIX 137
H4A 2 0.959457 0.557548 0.764689 11.00000 -1.50000
H4B 2 1.073742 0.586689 0.845908 11.00000 -1.50000
H4C 2 1.058597 0.586986 0.736283 11.00000 -1.50000
AFIX 0
C5 1 0.706127 0.744058 0.690967 11.00000 0.02133 0.01456 =
0.02801 -0.00092 0.00935 0.00032
AFIX 137
H5A 2 0.691407 0.762703 0.629050 11.00000 -1.50000
H5B 2 0.708215 0.774316 0.737630 11.00000 -1.50000
H5C 2 0.642916 0.715867 0.683159 11.00000 -1.50000
AFIX 0
C6 1 0.635740 0.606017 0.748119 11.00000 0.01819 0.01444 =
0.02092 0.00164 0.00629 -0.00039
AFIX 13
H6 2 0.581152 0.639740 0.718612 11.00000 -1.20000
AFIX 0
C7 1 0.709023 0.618883 0.854591 11.00000 0.02305 0.02406 =
0.02275 -0.00410 0.00827 -0.00703
AFIX 23
H7A 2 0.770547 0.588204 0.880981 11.00000 -1.20000
H7B 2 0.749193 0.657327 0.860547 11.00000 -1.20000
AFIX 0
C8 1 0.634220 0.620396 0.913449 11.00000 0.02888 0.02271 =
0.02448 -0.00103 0.01297 -0.00245
AFIX 23
H8A 2 0.686558 0.625478 0.982114 11.00000 -1.20000
H8B 2 0.580633 0.654808 0.893454 11.00000 -1.20000
AFIX 0
C9 1 0.561354 0.564692 0.901699 11.00000 0.03043 0.02871 =
0.02636 0.00138 0.01368 -0.00588
AFIX 23
H9A 2 0.509388 0.568956 0.936718 11.00000 -1.20000
H9B 2 0.614312 0.530671 0.929131 11.00000 -1.20000
AFIX 0
C10 1 0.486913 0.553875 0.795615 11.00000 0.03367 0.05166 =
0.02794 -0.00537 0.01400 -0.02419
AFIX 23
H10A 2 0.429787 0.586526 0.769790 11.00000 -1.20000
H10B 2 0.441734 0.516857 0.788177 11.00000 -1.20000
AFIX 0
C11 1 0.563747 0.549505 0.738611 11.00000 0.03522 0.02840 =
0.02685 -0.00563 0.01253 -0.01661
AFIX 23
H11A 2 0.513024 0.542531 0.670070 11.00000 -1.20000
H11B 2 0.618070 0.515569 0.762223 11.00000 -1.20000
AFIX 0
C12 1 0.651764 0.621600 0.558200 11.00000 0.01700 0.01529 =
0.02023 -0.00211 0.00661 -0.00037
AFIX 13
H12 2 0.614791 0.660468 0.560330 11.00000 -1.20000
AFIX 0
C13 1 0.554594 0.577127 0.503041 11.00000 0.01912 0.01972 =
0.02215 -0.00251 0.00664 -0.00370
AFIX 23
H13A 2 0.590262 0.537778 0.505504 11.00000 -1.20000
H13B 2 0.498078 0.574144 0.534073 11.00000 -1.20000
AFIX 0
C14 1 0.488952 0.595792 0.398440 11.00000 0.01789 0.02213 =
0.02128 -0.00312 0.00342 -0.00127
AFIX 23
H14A 2 0.430038 0.565269 0.363860 11.00000 -1.20000
H14B 2 0.446115 0.633029 0.395938 11.00000 -1.20000
AFIX 0
C15 1 0.572638 0.604555 0.348525 11.00000 0.02353 0.02553 =
0.01849 -0.00060 0.00547 0.00319
AFIX 23
H15A 2 0.527910 0.619553 0.282663 11.00000 -1.20000
H15B 2 0.607965 0.566219 0.343531 11.00000 -1.20000
AFIX 0
C16 1 0.670673 0.648086 0.403833 11.00000 0.02111 0.02789 =
0.02162 0.00421 0.00856 0.00031
AFIX 23
H16A 2 0.636000 0.687644 0.401800 11.00000 -1.20000
H16B 2 0.726876 0.650771 0.372463 11.00000 -1.20000
AFIX 0
C17 1 0.736966 0.629294 0.508448 11.00000 0.01748 0.02243 =
0.02119 0.00061 0.00653 -0.00062
AFIX 23
H17A 2 0.796776 0.659468 0.542928 11.00000 -1.20000
H17B 2 0.778557 0.591664 0.510856 11.00000 -1.20000
AFIX 0
F5 5 0.241666 0.207185 0.493330 11.00000 0.03314 0.06448 =
0.04459 -0.00964 0.02175 -0.01366
F6 5 0.082560 0.146717 0.441608 11.00000 0.02702 0.04305 =
0.04817 -0.01875 0.00539 -0.00141
F7 5 0.070444 0.237585 0.496808 11.00000 0.04203 0.05894 =
0.15586 -0.05135 0.02665 0.00520
F8 5 0.179320 0.168189 0.600117 11.00000 0.10252 0.10916 =
0.03749 -0.00771 0.02773 -0.05417
B2 3 0.143094 0.189997 0.507433 11.00000 0.02189 0.03819 =
0.03482 -0.01269 0.01293 -0.00434
F1 5 0.411179 0.692018 0.577477 11.00000 0.03472 0.02769 =
0.03257 0.00757 0.00890 0.00732
F2 5 0.466478 0.751727 0.482855 11.00000 0.03374 0.04101 =
0.04765 0.00119 0.01860 -0.00641
F3 5 0.284248 0.712752 0.424472 11.00000 0.03287 0.07307 =
0.03366 0.00606 -0.00209 -0.01920
F4 5 0.334812 0.783812 0.540197 11.00000 0.09746 0.04193 =
0.05180 0.01606 0.04813 0.03812
B1 3 0.373283 0.735224 0.506028 11.00000 0.02330 0.02573 =
0.02365 0.00256 0.00787 0.00593
HKLF 4
REM
REM R1 = 0.0409 for 6294 Fo > 4sig(Fo) and 0.0464 for all 7040 data
REM 455 parameters refined using 0 restraints
END
WGHT 0.0441 3.4993
REM Highest difference peak 0.639, deepest hole -0.495, 1-sigma level 0.053
Q1 1 0.0792 0.2406 0.4360 11.00000 0.05 0.64
Q2 1 0.2613 0.7586 0.5078 11.00000 0.05 0.53
Q3 1 0.1149 0.1962 0.5652 11.00000 0.05 0.51
Q4 1 0.3010 0.5620 0.8972 11.00000 0.05 0.30
Q5 1 0.2185 0.1558 0.5760 11.00000 0.05 0.29
Q6 1 0.0572 0.2039 0.5214 11.00000 0.05 0.28
Q7 1 0.2445 0.7245 0.4609 11.00000 0.05 0.27
Q8 1 0.1217 0.2432 0.5381 11.00000 0.05 0.25
Q9 1 0.0829 0.3788 0.7419 11.00000 0.05 0.24
Q10 1 0.2813 0.3417 0.8201 11.00000 0.05 0.22
Q11 1 0.5949 0.5813 0.7477 11.00000 0.05 0.22
Q12 1 -0.1103 0.4205 0.5765 11.00000 0.05 0.21
Q13 1 0.5994 0.6000 0.5252 11.00000 0.05 0.21
Q14 1 0.2422 0.4576 0.8214 11.00000 0.05 0.21
Q15 1 -0.0536 0.3788 0.4955 11.00000 0.05 0.20
Q16 1 0.5960 0.5967 0.9069 11.00000 0.05 0.19
Q17 1 0.8207 0.6822 0.7223 11.00000 0.05 0.18
Q18 1 0.4227 0.7808 0.4975 11.00000 0.05 0.18
Q19 1 -0.0274 0.4036 0.6396 11.00000 0.05 0.18
Q20 1 0.9838 0.6210 0.7717 11.00000 0.05 0.17
;
_shelx_res_checksum 76125
_shelxl_version_number 2013-3
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_8708sadabs
_database_code_depnum_ccdc_archive 'CCDC 1407665'
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_audit_block_code HAI-HA-120-01
_audit_creation_date 2014-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4813)
;
_chemical_name_common ?
_chemical_name_systematic
;
Title
;
_chemical_formula_moiety 'C17 H32 Au Cl N2 P, F6 Sb, C2 H3 N'
_chemical_formula_sum 'C19 H35 Au Cl F6 N3 P Sb'
_chemical_formula_weight 804.65
_chemical_compound_source dichlormethane
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_symmetry_cell_setting TRICLINIC
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-p 1'
_symmetry_Int_Tables_number 2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.4612(9)
_cell_length_b 8.9156(9)
_cell_length_c 19.0961(19)
_cell_angle_alpha 83.9995(16)
_cell_angle_beta 81.0351(17)
_cell_angle_gamma 64.5960(15)
_cell_volume 1284.2(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9701
_cell_measurement_temperature 100
_cell_measurement_theta_max 36.9545
_cell_measurement_theta_min 2.6855
_shelx_estimated_absorpt_T_max 0.517
_shelx_estimated_absorpt_T_min 0.421
_exptl_absorpt_coefficient_mu 6.982
_exptl_absorpt_correction_T_max 0.63018
_exptl_absorpt_correction_T_min 0.49558
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details 'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.081
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.0500
0.00 -1.00 0.00 0.0700
-1.00 0.00 0.00 0.0700
1.00 0.00 0.00 0.0200
0.00 0.00 -1.00 0.0400
0.00 0.00 1.00 0.0500
-1.00 -1.00 0.00 0.0640
_exptl_crystal_description prism
_exptl_crystal_F_000 772
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.09
_exptl_special_details
;
Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0184
_diffrn_reflns_av_unetI/netI 0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 42921
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 33.139
_diffrn_reflns_theta_min 2.161
_diffrn_radiation_monochromator 'Incoatec Helios mirrors'
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method 'CCD \f- and \w-scans'
_diffrn_radiation_type Mo-K\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 1\mS
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 9598
_reflns_number_total 9751
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT software (Bruker AXS, 2004)'
_computing_data_collection 'APEX2 (Bruker AXS, 2005-2013)'
_computing_data_reduction 'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 1997-2012)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL (G. M. Sheldrick, 2013)'
_computing_structure_solution 'SHELXS (G. M. Sheldrick, 2013)'
_refine_diff_density_max 2.023
_refine_diff_density_min -1.582
_refine_diff_density_rms 0.099
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.157
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 292
_refine_ls_number_reflns 9751
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0165
_refine_ls_R_factor_gt 0.0160
_refine_ls_restrained_S_all 1.157
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+1.4566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0392
_refine_ls_wR_factor_ref 0.0393
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The minimum and maximum estimated transmissions from the multi-scan
scaling are 0.4963 and 0.6304 (SADABS).
Highest peak ?
Deepest hole ?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C6(H6), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
C16(H16A,H16B), C17(H17A,H17B)
2.c Idealised Me refined as rotating group:
C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C97(H97A,H97B,H97C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.38113(2) 0.71990(2) 0.15482(2) 0.01033(2) Uani 1 1 d . . . . .
Cl1 Cl 0.15550(6) 0.69770(5) 0.11061(2) 0.01683(7) Uani 1 1 d . . . . .
P1 P 0.60941(5) 0.74166(5) 0.19149(2) 0.00883(6) Uani 1 1 d . . . . .
N1 N 0.44622(19) 0.79945(18) 0.33347(8) 0.0132(2) Uani 1 1 d . . . . .
N2 N 0.71916(19) 0.77303(19) 0.31963(8) 0.0133(2) Uani 1 1 d . . . . .
C1 C 0.5891(2) 0.77594(19) 0.28787(8) 0.0104(2) Uani 1 1 d . . . . .
C2 C 0.4768(2) 0.8116(2) 0.40644(9) 0.0156(3) Uani 1 1 d . . . . .
H2A H 0.4653 0.7206 0.4381 0.019 Uiso 1 1 calc R . . . .
H2B H 0.3930 0.9196 0.4263 0.019 Uiso 1 1 calc R . . . .
C3 C 0.6657(2) 0.7959(2) 0.39660(9) 0.0158(3) Uani 1 1 d . . . . .
H3A H 0.6701 0.8976 0.4108 0.019 Uiso 1 1 calc R . . . .
H3B H 0.7421 0.6990 0.4245 0.019 Uiso 1 1 calc R . . . .
C4 C 0.2704(2) 0.8257(3) 0.32175(10) 0.0194(3) Uani 1 1 d . . . . .
H4A H 0.2086 0.9389 0.3022 0.029 Uiso 1 1 calc GR . . . .
H4B H 0.2049 0.8106 0.3669 0.029 Uiso 1 1 calc GR . . . .
H4C H 0.2793 0.7455 0.2883 0.029 Uiso 1 1 calc GR . . . .
C5 C 0.8948(2) 0.7594(3) 0.29134(10) 0.0186(3) Uani 1 1 d . . . . .
H5A H 0.9836 0.6590 0.3119 0.028 Uiso 1 1 calc GR . . . .
H5B H 0.9079 0.8572 0.3035 0.028 Uiso 1 1 calc GR . . . .
H5C H 0.9111 0.7527 0.2396 0.028 Uiso 1 1 calc GR . . . .
C6 C 0.6396(2) 0.92609(19) 0.15175(8) 0.0106(2) Uani 1 1 d . . . . .
H6 H 0.7378 0.9335 0.1721 0.013 Uiso 1 1 calc R . . . .
C7 C 0.4684(2) 1.0813(2) 0.17074(9) 0.0137(3) Uani 1 1 d . . . . .
H7A H 0.3696 1.0729 0.1523 0.016 Uiso 1 1 calc R . . . .
H7B H 0.4414 1.0876 0.2230 0.016 Uiso 1 1 calc R . . . .
C8 C 0.4867(3) 1.2393(2) 0.13894(9) 0.0160(3) Uani 1 1 d . . . . .
H8A H 0.3735 1.3371 0.1499 0.019 Uiso 1 1 calc R . . . .
H8B H 0.5780 1.2530 0.1608 0.019 Uiso 1 1 calc R . . . .
C9 C 0.5369(3) 1.2313(2) 0.05872(10) 0.0192(3) Uani 1 1 d . . . . .
H9A H 0.5590 1.3296 0.0406 0.023 Uiso 1 1 calc R . . . .
H9B H 0.4373 1.2349 0.0363 0.023 Uiso 1 1 calc R . . . .
C10 C 0.7014(3) 1.0733(2) 0.03787(10) 0.0187(3) Uani 1 1 d . . . . .
H10A H 0.8050 1.0789 0.0533 0.022 Uiso 1 1 calc R . . . .
H10B H 0.7214 1.0674 -0.0144 0.022 Uiso 1 1 calc R . . . .
C11 C 0.6849(2) 0.9156(2) 0.07098(9) 0.0145(3) Uani 1 1 d . . . . .
H11A H 0.5916 0.9013 0.0507 0.017 Uiso 1 1 calc R . . . .
H11B H 0.7975 0.8176 0.0594 0.017 Uiso 1 1 calc R . . . .
C12 C 0.8109(2) 0.5464(2) 0.17822(9) 0.0120(3) Uani 1 1 d . . . . .
H12 H 0.9164 0.5695 0.1785 0.014 Uiso 1 1 calc R . . . .
C13 C 0.8220(3) 0.4757(2) 0.10615(10) 0.0175(3) Uani 1 1 d . . . . .
H13A H 0.7146 0.4585 0.1045 0.021 Uiso 1 1 calc R . . . .
H13B H 0.8281 0.5564 0.0673 0.021 Uiso 1 1 calc R . . . .
C14 C 0.9852(3) 0.3102(2) 0.09542(12) 0.0228(4) Uani 1 1 d . . . . .
H14A H 0.9872 0.2648 0.0500 0.027 Uiso 1 1 calc R . . . .
H14B H 1.0928 0.3295 0.0927 0.027 Uiso 1 1 calc R . . . .
C15 C 0.9852(2) 0.1842(2) 0.15597(12) 0.0213(4) Uani 1 1 d . . . . .
H15A H 0.8850 0.1551 0.1552 0.026 Uiso 1 1 calc R . . . .
H15B H 1.0955 0.0815 0.1491 0.026 Uiso 1 1 calc R . . . .
C16 C 0.9704(3) 0.2527(2) 0.22764(12) 0.0238(4) Uani 1 1 d . . . . .
H16A H 1.0778 0.2689 0.2306 0.029 Uiso 1 1 calc R . . . .
H16B H 0.9624 0.1712 0.2658 0.029 Uiso 1 1 calc R . . . .
C17 C 0.8078(2) 0.4186(2) 0.23871(10) 0.0171(3) Uani 1 1 d . . . . .
H17A H 0.8052 0.4626 0.2846 0.021 Uiso 1 1 calc R . . . .
H17B H 0.6997 0.4005 0.2405 0.021 Uiso 1 1 calc R . . . .
Sb1 Sb 0.38054(2) 0.31933(2) 0.36708(2) 0.01424(2) Uani 1 1 d . . . . .
F1 F 0.16930(18) 0.47095(17) 0.41509(8) 0.0295(3) Uani 1 1 d . . . . .
F2 F 0.4984(2) 0.44153(18) 0.38979(8) 0.0320(3) Uani 1 1 d . . . . .
F3 F 0.26081(19) 0.19730(17) 0.34591(7) 0.0269(3) Uani 1 1 d . . . . .
F4 F 0.3250(2) 0.45055(16) 0.28336(7) 0.0306(3) Uani 1 1 d . . . . .
F5 F 0.58871(17) 0.16835(16) 0.31756(7) 0.0245(2) Uani 1 1 d . . . . .
F6 F 0.4344(2) 0.18911(17) 0.45094(6) 0.0279(3) Uani 1 1 d . . . . .
N99 N 0.8948(3) 1.0188(3) 0.42403(15) 0.0433(6) Uani 1 1 d . . . A 1
C97 C 0.8745(4) 1.3011(3) 0.45668(16) 0.0366(5) Uani 1 1 d . . . A 1
H97A H 0.9308 1.3463 0.4166 0.055 Uiso 1 1 calc GR . . A 1
H97B H 0.9353 1.2849 0.4984 0.055 Uiso 1 1 calc GR . . A 1
H97C H 0.7506 1.3789 0.4672 0.055 Uiso 1 1 calc GR . . A 1
C98 C 0.8845(3) 1.1453(3) 0.43882(13) 0.0321(5) Uani 1 1 d . . . A 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.00972(3) 0.01141(3) 0.01105(3) 0.00003(2) -0.00202(2) -0.00542(2)
Cl1 0.01501(17) 0.02172(18) 0.01831(18) 0.00227(14) -0.00569(14) -0.01149(15)
P1 0.00867(16) 0.00976(15) 0.00824(15) -0.00098(12) -0.00076(12) -0.00401(13)
N1 0.0130(6) 0.0168(6) 0.0102(6) -0.0026(5) 0.0012(5) -0.0071(5)
N2 0.0133(6) 0.0174(6) 0.0097(6) -0.0019(5) -0.0019(5) -0.0066(5)
C1 0.0104(6) 0.0100(6) 0.0102(6) -0.0011(5) -0.0005(5) -0.0037(5)
C2 0.0204(8) 0.0183(7) 0.0090(6) -0.0030(5) 0.0015(6) -0.0097(6)
C3 0.0198(8) 0.0189(7) 0.0095(6) -0.0015(5) -0.0016(6) -0.0087(6)
C4 0.0130(7) 0.0262(9) 0.0199(8) -0.0039(7) 0.0018(6) -0.0097(6)
C5 0.0121(7) 0.0285(9) 0.0162(7) -0.0046(6) -0.0025(6) -0.0084(6)
C6 0.0118(6) 0.0115(6) 0.0099(6) -0.0006(5) -0.0013(5) -0.0062(5)
C7 0.0136(7) 0.0108(6) 0.0157(7) -0.0022(5) 0.0002(5) -0.0046(5)
C8 0.0217(8) 0.0116(6) 0.0162(7) -0.0008(5) -0.0045(6) -0.0077(6)
C9 0.0299(9) 0.0150(7) 0.0147(7) 0.0028(6) -0.0071(7) -0.0107(7)
C10 0.0261(9) 0.0198(8) 0.0126(7) 0.0012(6) 0.0005(6) -0.0134(7)
C11 0.0181(7) 0.0151(7) 0.0103(6) -0.0013(5) 0.0011(5) -0.0078(6)
C12 0.0095(6) 0.0119(6) 0.0143(7) -0.0036(5) 0.0003(5) -0.0039(5)
C13 0.0200(8) 0.0153(7) 0.0149(7) -0.0052(6) 0.0006(6) -0.0050(6)
C14 0.0184(8) 0.0205(8) 0.0270(9) -0.0131(7) 0.0064(7) -0.0060(7)
C15 0.0139(7) 0.0136(7) 0.0341(10) -0.0085(7) -0.0054(7) -0.0012(6)
C16 0.0224(9) 0.0136(7) 0.0298(10) -0.0025(7) -0.0111(7) 0.0006(7)
C17 0.0187(8) 0.0117(7) 0.0166(7) -0.0003(6) -0.0031(6) -0.0019(6)
Sb1 0.01815(5) 0.01261(5) 0.01148(5) -0.00158(3) -0.00184(4) -0.00576(4)
F1 0.0262(6) 0.0259(6) 0.0293(7) -0.0126(5) 0.0060(5) -0.0050(5)
F2 0.0368(8) 0.0283(7) 0.0408(8) -0.0059(6) -0.0068(6) -0.0213(6)
F3 0.0312(7) 0.0297(6) 0.0274(6) -0.0078(5) -0.0045(5) -0.0182(5)
F4 0.0401(8) 0.0218(6) 0.0184(6) 0.0062(5) -0.0053(5) -0.0032(5)
F5 0.0210(6) 0.0221(6) 0.0215(6) -0.0035(4) 0.0015(4) -0.0014(4)
F6 0.0440(8) 0.0258(6) 0.0123(5) 0.0024(4) -0.0062(5) -0.0130(6)
N99 0.0348(12) 0.0482(14) 0.0502(14) -0.0179(11) -0.0045(10) -0.0173(10)
C97 0.0318(12) 0.0328(12) 0.0476(15) -0.0064(11) 0.0013(11) -0.0169(10)
C98 0.0259(10) 0.0424(13) 0.0293(11) -0.0093(10) 0.0016(8) -0.0155(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Cl1 2.2931(5) . ?
Au1 P1 2.2428(5) . ?
P1 C1 1.8667(16) . ?
P1 C6 1.8393(16) . ?
P1 C12 1.8471(16) . ?
N1 C1 1.325(2) . ?
N1 C2 1.479(2) . ?
N1 C4 1.453(2) . ?
N2 C1 1.327(2) . ?
N2 C3 1.477(2) . ?
N2 C5 1.458(2) . ?
C2 C3 1.527(3) . ?
C6 C7 1.538(2) . ?
C6 C11 1.533(2) . ?
C7 C8 1.535(2) . ?
C8 C9 1.525(3) . ?
C9 C10 1.530(3) . ?
C10 C11 1.534(2) . ?
C12 C13 1.546(2) . ?
C12 C17 1.541(2) . ?
C13 C14 1.534(3) . ?
C14 C15 1.525(3) . ?
C15 C16 1.522(3) . ?
C16 C17 1.534(3) . ?
Sb1 F1 1.8809(13) . ?
Sb1 F2 1.8800(13) . ?
Sb1 F3 1.8810(13) . ?
Sb1 F4 1.8754(12) . ?
Sb1 F5 1.8765(12) . ?
Sb1 F6 1.8721(12) . ?
N99 C98 1.154(4) . ?
C97 C98 1.429(4) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Au1 Cl1 176.634(15) . . ?
C1 P1 Au1 116.22(5) . . ?
C6 P1 Au1 112.35(5) . . ?
C6 P1 C1 100.75(7) . . ?
C6 P1 C12 113.25(7) . . ?
C12 P1 Au1 110.54(6) . . ?
C12 P1 C1 103.19(7) . . ?
C1 N1 C2 111.04(14) . . ?
C1 N1 C4 130.63(15) . . ?
C4 N1 C2 118.16(14) . . ?
C1 N2 C3 111.19(14) . . ?
C1 N2 C5 131.41(15) . . ?
C5 N2 C3 117.34(14) . . ?
N1 C1 P1 124.43(13) . . ?
N1 C1 N2 111.67(14) . . ?
N2 C1 P1 123.84(12) . . ?
N1 C2 C3 103.10(13) . . ?
N2 C3 C2 102.98(14) . . ?
C7 C6 P1 108.54(11) . . ?
C11 C6 P1 110.99(11) . . ?
C11 C6 C7 110.25(13) . . ?
C8 C7 C6 110.68(14) . . ?
C9 C8 C7 111.28(14) . . ?
C8 C9 C10 111.97(15) . . ?
C9 C10 C11 112.31(15) . . ?
C6 C11 C10 110.69(14) . . ?
C13 C12 P1 109.93(12) . . ?
C17 C12 P1 109.73(11) . . ?
C17 C12 C13 109.70(14) . . ?
C14 C13 C12 110.64(16) . . ?
C15 C14 C13 111.31(15) . . ?
C16 C15 C14 111.42(16) . . ?
C15 C16 C17 111.42(16) . . ?
C16 C17 C12 110.94(15) . . ?
F1 Sb1 F3 89.64(6) . . ?
F2 Sb1 F1 89.70(7) . . ?
F2 Sb1 F3 179.06(6) . . ?
F4 Sb1 F1 89.19(6) . . ?
F4 Sb1 F2 90.24(7) . . ?
F4 Sb1 F3 90.41(7) . . ?
F4 Sb1 F5 89.92(6) . . ?
F5 Sb1 F1 178.79(6) . . ?
F5 Sb1 F2 91.13(7) . . ?
F5 Sb1 F3 89.55(6) . . ?
F6 Sb1 F1 90.44(6) . . ?
F6 Sb1 F2 89.84(7) . . ?
F6 Sb1 F3 89.49(6) . . ?
F6 Sb1 F4 179.62(7) . . ?
F6 Sb1 F5 90.45(6) . . ?
N99 C98 C97 179.1(3) . . ?
_shelx_res_file
;
TITL
CELL 0.71073 8.4612 8.9156 19.0961 83.9995 81.0351 64.596
ZERR 2 0.0009 0.0009 0.0019 0.0016 0.0017 0.0015
LATT 1
SFAC C H Au Cl F N P Sb O
UNIT 38 70 2 2 12 6 2 2 1
L.S. 10
PLAN 20
SIZE 0.109 0.13 0.15
TEMP -173
fmap 2 53
acta
OMIT 0 0 1
OMIT -1 -3 2
OMIT -1 1 0
OMIT 10 -2 10
OMIT 8 -2 1
OMIT 0 1 9
OMIT -1 -7 1
OMIT 2 1 15
REM V:/8708/8708sadabs.hkl
WGHT 0.013600 1.456600
FVAR 0.10708
AU1 3 0.381134 0.719899 0.154818 11.00000 0.00972 0.01141 =
0.01105 0.00003 -0.00202 -0.00542
CL1 4 0.155495 0.697697 0.110612 11.00000 0.01501 0.02172 =
0.01831 0.00227 -0.00569 -0.01149
P1 7 0.609413 0.741665 0.191488 11.00000 0.00867 0.00976 =
0.00824 -0.00098 -0.00076 -0.00401
N1 6 0.446220 0.799455 0.333471 11.00000 0.01303 0.01684 =
0.01016 -0.00259 0.00120 -0.00706
N2 6 0.719160 0.773035 0.319633 11.00000 0.01334 0.01741 =
0.00973 -0.00190 -0.00188 -0.00660
C1 1 0.589095 0.775940 0.287871 11.00000 0.01038 0.01002 =
0.01015 -0.00107 -0.00049 -0.00374
C2 1 0.476760 0.811571 0.406443 11.00000 0.02040 0.01829 =
0.00903 -0.00300 0.00153 -0.00968
AFIX 23
H2A 2 0.465300 0.720594 0.438134 11.00000 -1.20000
H2B 2 0.392995 0.919593 0.426266 11.00000 -1.20000
AFIX 0
C3 1 0.665745 0.795893 0.396598 11.00000 0.01977 0.01893 =
0.00955 -0.00151 -0.00160 -0.00867
AFIX 23
H3A 2 0.670120 0.897588 0.410786 11.00000 -1.20000
H3B 2 0.742146 0.699000 0.424504 11.00000 -1.20000
AFIX 0
C4 1 0.270448 0.825734 0.321753 11.00000 0.01303 0.02621 =
0.01987 -0.00392 0.00182 -0.00973
AFIX 137
H4A 2 0.208587 0.938861 0.302160 11.00000 -1.50000
H4B 2 0.204896 0.810563 0.366908 11.00000 -1.50000
H4C 2 0.279294 0.745506 0.288286 11.00000 -1.50000
AFIX 0
C5 1 0.894836 0.759374 0.291340 11.00000 0.01207 0.02850 =
0.01619 -0.00461 -0.00252 -0.00843
AFIX 137
H5A 2 0.983553 0.659007 0.311899 11.00000 -1.50000
H5B 2 0.907944 0.857232 0.303467 11.00000 -1.50000
H5C 2 0.911130 0.752698 0.239631 11.00000 -1.50000
AFIX 0
C6 1 0.639553 0.926095 0.151751 11.00000 0.01181 0.01151 =
0.00988 -0.00063 -0.00134 -0.00619
AFIX 13
H6 2 0.737841 0.933538 0.172076 11.00000 -1.20000
AFIX 0
C7 1 0.468440 1.081304 0.170742 11.00000 0.01364 0.01083 =
0.01566 -0.00220 0.00023 -0.00463
AFIX 23
H7A 2 0.369564 1.072922 0.152320 11.00000 -1.20000
H7B 2 0.441423 1.087618 0.222978 11.00000 -1.20000
AFIX 0
C8 1 0.486658 1.239282 0.138935 11.00000 0.02169 0.01161 =
0.01624 -0.00080 -0.00452 -0.00771
AFIX 23
H8A 2 0.373536 1.337099 0.149907 11.00000 -1.20000
H8B 2 0.578025 1.253041 0.160819 11.00000 -1.20000
AFIX 0
C9 1 0.536945 1.231255 0.058724 11.00000 0.02995 0.01497 =
0.01465 0.00277 -0.00708 -0.01069
AFIX 23
H9A 2 0.558961 1.329590 0.040555 11.00000 -1.20000
H9B 2 0.437342 1.234934 0.036319 11.00000 -1.20000
AFIX 0
C10 1 0.701377 1.073325 0.037873 11.00000 0.02613 0.01978 =
0.01263 0.00118 0.00050 -0.01339
AFIX 23
H10A 2 0.805036 1.078914 0.053328 11.00000 -1.20000
H10B 2 0.721424 1.067358 -0.014440 11.00000 -1.20000
AFIX 0
C11 1 0.684931 0.915555 0.070984 11.00000 0.01809 0.01506 =
0.01033 -0.00127 0.00105 -0.00777
AFIX 23
H11A 2 0.591629 0.901315 0.050743 11.00000 -1.20000
H11B 2 0.797536 0.817590 0.059429 11.00000 -1.20000
AFIX 0
C12 1 0.810853 0.546391 0.178222 11.00000 0.00947 0.01188 =
0.01427 -0.00355 0.00031 -0.00394
AFIX 13
H12 2 0.916441 0.569479 0.178492 11.00000 -1.20000
AFIX 0
C13 1 0.822008 0.475698 0.106148 11.00000 0.01999 0.01532 =
0.01485 -0.00516 0.00061 -0.00502
AFIX 23
H13A 2 0.714568 0.458509 0.104534 11.00000 -1.20000
H13B 2 0.828138 0.556427 0.067274 11.00000 -1.20000
AFIX 0
C14 1 0.985165 0.310177 0.095424 11.00000 0.01840 0.02045 =
0.02696 -0.01308 0.00639 -0.00602
AFIX 23
H14A 2 0.987187 0.264753 0.049985 11.00000 -1.20000
H14B 2 1.092832 0.329476 0.092705 11.00000 -1.20000
AFIX 0
C15 1 0.985209 0.184210 0.155971 11.00000 0.01394 0.01356 =
0.03413 -0.00851 -0.00536 -0.00115
AFIX 23
H15A 2 0.885003 0.155089 0.155194 11.00000 -1.20000
H15B 2 1.095510 0.081533 0.149117 11.00000 -1.20000
AFIX 0
C16 1 0.970378 0.252687 0.227639 11.00000 0.02241 0.01365 =
0.02977 -0.00245 -0.01113 0.00065
AFIX 23
H16A 2 1.077765 0.268886 0.230617 11.00000 -1.20000
H16B 2 0.962397 0.171244 0.265847 11.00000 -1.20000
AFIX 0
C17 1 0.807810 0.418596 0.238714 11.00000 0.01867 0.01170 =
0.01656 -0.00029 -0.00313 -0.00189
AFIX 23
H17A 2 0.805195 0.462564 0.284594 11.00000 -1.20000
H17B 2 0.699681 0.400479 0.240521 11.00000 -1.20000
AFIX 0
SB1 8 0.380538 0.319326 0.367083 11.00000 0.01815 0.01261 =
0.01148 -0.00158 -0.00184 -0.00576
F1 5 0.169299 0.470953 0.415094 11.00000 0.02622 0.02589 =
0.02934 -0.01258 0.00602 -0.00500
F2 5 0.498354 0.441532 0.389790 11.00000 0.03679 0.02825 =
0.04076 -0.00591 -0.00677 -0.02134
F3 5 0.260813 0.197305 0.345910 11.00000 0.03125 0.02970 =
0.02739 -0.00779 -0.00448 -0.01823
F4 5 0.325040 0.450548 0.283357 11.00000 0.04007 0.02179 =
0.01842 0.00616 -0.00528 -0.00315
F5 5 0.588714 0.168350 0.317564 11.00000 0.02096 0.02207 =
0.02147 -0.00350 0.00146 -0.00139
F6 5 0.434387 0.189112 0.450944 11.00000 0.04396 0.02585 =
0.01233 0.00241 -0.00617 -0.01304
PART 1
N99 6 0.894762 1.018842 0.424033 11.00000 0.03482 0.04816 =
0.05020 -0.01794 -0.00452 -0.01725
C97 1 0.874512 1.301076 0.456678 11.00000 0.03179 0.03284 =
0.04762 -0.00639 0.00127 -0.01686
AFIX 137
H97A 2 0.930757 1.346298 0.416639 11.00000 -1.50000
H97B 2 0.935322 1.284879 0.498402 11.00000 -1.50000
H97C 2 0.750607 1.378894 0.467235 11.00000 -1.50000
AFIX 0
C98 1 0.884499 1.145272 0.438823 11.00000 0.02590 0.04242 =
0.02932 -0.00935 0.00164 -0.01550
HKLF 4
REM
REM R1 = 0.0160 for 9598 Fo > 4sig(Fo) and 0.0165 for all 9751 data
REM 292 parameters refined using 0 restraints
END
WGHT 0.0136 1.4566
REM Highest difference peak 2.023, deepest hole -1.582, 1-sigma level 0.099
Q1 1 0.9842 1.1976 0.4995 11.00000 0.05 2.02
Q2 1 0.9374 0.8809 0.4586 11.00000 0.05 2.01
Q3 1 0.9065 0.2004 -0.0144 11.00000 0.05 0.86
Q4 1 0.4261 0.6264 0.1633 11.00000 0.05 0.80
Q5 1 0.4429 0.7196 0.1216 11.00000 0.05 0.79
Q6 1 0.4365 0.3160 0.3728 11.00000 0.05 0.74
Q7 1 0.3887 0.2656 0.3806 11.00000 0.05 0.70
Q8 1 0.9016 0.7996 0.1992 11.00000 0.05 0.67
Q9 1 0.3424 0.3191 0.3925 11.00000 0.05 0.64
Q10 1 0.3374 0.3533 0.3737 11.00000 0.05 0.59
Q11 1 0.3648 0.8139 0.1437 11.00000 0.05 0.59
Q12 1 0.8826 1.2448 0.4410 11.00000 0.05 0.52
Q13 1 0.3291 0.8221 0.1561 11.00000 0.05 0.51
Q14 1 0.5071 1.2425 0.0999 11.00000 0.05 0.47
Q15 1 0.1493 0.5607 0.2486 11.00000 0.05 0.47
Q16 1 0.5146 0.8009 0.3076 11.00000 0.05 0.47
Q17 1 0.4437 0.7820 0.1591 11.00000 0.05 0.45
Q18 1 0.6381 1.1512 0.0431 11.00000 0.05 0.44
Q19 1 0.6597 0.7838 0.3020 11.00000 0.05 0.44
Q20 1 0.5762 0.8043 0.4036 11.00000 0.05 0.44
;
_shelx_res_checksum 86765
_shelxl_version_number 2014-1
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_8725sadabs
_database_code_depnum_ccdc_archive 'CCDC 1407666'
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_audit_block_code HAI-HA-114-01
_audit_creation_date 2014-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4813)
;
_shelxl_version_number 2013-4
_chemical_name_common ?
_chemical_name_systematic
;
Title
;
_chemical_formula_moiety 'C17 H32 N2 P, F6 Sb'
_chemical_formula_sum 'C17 H32 F6 N2 P Sb'
_chemical_formula_weight 531.16
_chemical_compound_source dichloromethane
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt P-1
_space_group_name_Hall '-P 1'
_symmetry_cell_setting TRICLINIC
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-p 1'
_symmetry_Int_Tables_number 2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 15.028(3)
_cell_length_b 15.072(3)
_cell_length_c 15.430(3)
_cell_angle_alpha 75.926(3)
_cell_angle_beta 82.983(3)
_cell_angle_gamma 74.157(3)
_cell_volume 3255.4(10)
_cell_formula_units_Z 6
_cell_measurement_reflns_used 9887
_cell_measurement_temperature 100
_cell_measurement_theta_max 28.4371
_cell_measurement_theta_min 2.5136
_shelx_estimated_absorpt_T_max 0.986
_shelx_estimated_absorpt_T_min 0.678
_exptl_absorpt_coefficient_mu 1.400
_exptl_absorpt_correction_T_max 0.986
_exptl_absorpt_correction_T_min 0.678
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details 'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.626
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 -2.00 1.00 0.1400
1.00 2.00 -1.00 0.1200
-1.00 1.00 1.00 0.0700
1.00 -1.00 -1.00 0.0700
1.00 0.00 1.00 0.0050
-1.00 0.00 -1.00 0.0050
_exptl_crystal_description plate
_exptl_crystal_F_000 1608
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.01
_exptl_special_details
;
Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0710
_diffrn_reflns_av_unetI/netI 0.0562
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 79160
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.512
_diffrn_reflns_theta_min 1.363
_diffrn_ambient_temperature 100
_diffrn_radiation_monochromator 'Incoatec Helios mirrors'
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method 'CCD \f- and \w-scans'
_diffrn_radiation_type Mo-K\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 1\mS
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 11965
_reflns_number_total 16429
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT software (Bruker AXS, 2004)'
_computing_data_collection 'APEX2 (Bruker AXS, 2005-2013)'
_computing_data_reduction 'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 1997-2012)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL (G. M. Sheldrick, 2013)'
_computing_structure_solution 'SHELXS (G. M. Sheldrick, 2013)'
_refine_diff_density_max 1.100
_refine_diff_density_min -1.660
_refine_diff_density_rms 0.188
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.041
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 754
_refine_ls_number_reflns 16429
_refine_ls_number_restraints 171
_refine_ls_R_factor_all 0.0674
_refine_ls_R_factor_gt 0.0376
_refine_ls_restrained_S_all 1.087
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+3.9758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0854
_refine_ls_wR_factor_ref 0.1053
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The minimum and maximum estimated transmissions from the multi-scan
scaling are and (SADABS).
Highest peak ?
Deepest hole ?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
F15C-F17C \\sim F15C-F16C \\sim F15C-F14C \\sim F16A-F15A \\sim F16A-F14A
\\sim F16A-F18A \\sim F13B-
F15B \\sim F13B-F16B \\sim F13B-F14B \\sim F15B-F16B \\sim F15B-F14B \\sim
F17C-F16C \\sim F17C-F14C ~
F15A-F14A \\sim F14A-F18A
with sigma of 0.02
Sb3-F15C \\sim Sb3-F16A \\sim Sb3-F13B \\sim Sb3-F15B \\sim Sb3-F17C \\sim
Sb3-F16C \\sim Sb3-F16B ~
Sb3-F15A \\sim Sb3-F14A \\sim Sb3-F18A \\sim Sb3-F14C \\sim Sb3-F14B
with sigma of 0.01
3. Others
Fixed Sof: F13C(0.25) F14C(0.25) F15C(0.25) F16C(0.25) F17C(0.25) F18C(0.25)
F16A(0.5) F15A(0.5) F14B(0.25) F17A(0.5) F15B(0.25) F18A(0.5) F16B(0.25)
F13A(0.5) F17B(0.25) F13B(0.25) F14A(0.5) F18B(0.25)
4.a Ternary CH refined with riding coordinates:
C6(H6), C12(H12), C26(H26), C32(H32), C46(H46), C52(H52)
4.b Secondary CH2 refined with riding coordinates:
C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
C16(H16A,H16B), C17(H17A,H17B), C22(H22A,H22B), C23(H23A,H23B), C27(H27A,H27B),
C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,
H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
C42(H42A,H42B), C43(H43A,H43B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B),
C50(H50A,H50B), C51(H51A,H51B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
H55B), C56(H56A,H56B), C57(H57A,H57B)
4.c Idealised Me refined as rotating group:
C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.44016(2) 0.26893(2) 0.95313(2) 0.01818(6) Uani 1 1 d . . . . .
F1 F 0.37745(17) 0.23260(16) 1.06363(16) 0.0286(5) Uani 1 1 d . . . . .
F2 F 0.50419(18) 0.30505(17) 0.84354(16) 0.0325(6) Uani 1 1 d . . . . .
F3 F 0.54128(17) 0.16523(17) 0.98587(17) 0.0318(6) Uani 1 1 d . . . . .
F4 F 0.3896(2) 0.1942(2) 0.90275(18) 0.0412(7) Uani 1 1 d . . . . .
F5 F 0.33953(17) 0.37311(18) 0.92155(19) 0.0384(6) Uani 1 1 d . . . . .
F6 F 0.49149(17) 0.34293(17) 1.00415(17) 0.0321(6) Uani 1 1 d . . . . .
Sb2 Sb 0.18176(2) 0.57194(2) 0.34412(2) 0.01837(7) Uani 1 1 d . . . . .
F7 F 0.21735(18) 0.62540(19) 0.42757(18) 0.0383(6) Uani 1 1 d . . . . .
F8 F 0.24425(18) 0.45016(17) 0.40105(17) 0.0339(6) Uani 1 1 d . . . . .
F9 F 0.07350(16) 0.56058(16) 0.41554(16) 0.0268(5) Uani 1 1 d . . . . .
F10 F 0.14598(16) 0.51925(17) 0.25937(15) 0.0277(5) Uani 1 1 d . . . . .
F11 F 0.28872(18) 0.58593(18) 0.27155(19) 0.0382(7) Uani 1 1 d . . . . .
F12 F 0.11646(19) 0.69235(16) 0.28505(18) 0.0370(6) Uani 1 1 d . . . . .
Sb3 Sb 0.22324(2) 0.05565(2) 0.40945(2) 0.02511(7) Uani 1 1 d . . . . .
F13C F 0.2664(11) 0.0945(11) 0.2783(11) 0.075(4) Uiso 0.25 1 d . . P A 3
F14C F 0.2198(10) -0.0495(7) 0.3677(10) 0.084(5) Uiso 0.25 1 d . . P B 3
F15C F 0.1948(10) 0.0070(9) 0.5257(5) 0.078(4) Uiso 0.25 1 d . . P B 3
F16C F 0.2482(10) 0.1621(7) 0.4289(10) 0.082(5) Uiso 0.25 1 d . . P B 3
F17C F 0.1035(6) 0.1162(9) 0.3794(9) 0.075(4) Uiso 0.25 1 d . . P B 3
F18C F 0.3553(10) -0.0005(11) 0.4134(10) 0.061(4) Uiso 0.25 1 d . . P C 3
P1 P 0.08669(7) 0.61059(7) 0.73949(6) 0.01647(19) Uani 1 1 d . . . . .
N1 N 0.1169(2) 0.7514(2) 0.5940(2) 0.0205(7) Uani 1 1 d . . . . .
N2 N 0.0044(2) 0.6967(2) 0.5696(2) 0.0167(6) Uani 1 1 d . . . . .
C1 C 0.0659(2) 0.6894(2) 0.6259(2) 0.0151(7) Uani 1 1 d . . . . .
C2 C 0.0899(3) 0.8073(3) 0.5047(3) 0.0238(8) Uani 1 1 d . . . . .
H2A H 0.1424 0.7979 0.4595 0.029 Uiso 1 1 calc R . . . .
H2B H 0.0676 0.8755 0.5046 0.029 Uiso 1 1 calc R . . . .
C3 C 0.0121(3) 0.7681(3) 0.4868(3) 0.0204(8) Uani 1 1 d . . . . .
H3A H -0.0464 0.8181 0.4771 0.024 Uiso 1 1 calc R . . . .
H3B H 0.0287 0.7390 0.4341 0.024 Uiso 1 1 calc R . . . .
C4 C 0.1962(3) 0.7621(3) 0.6313(3) 0.0308(10) Uani 1 1 d . . . . .
H4A H 0.1988 0.7285 0.6942 0.046 Uiso 1 1 calc GR . . . .
H4B H 0.1905 0.8293 0.6271 0.046 Uiso 1 1 calc GR . . . .
H4C H 0.2530 0.7357 0.5978 0.046 Uiso 1 1 calc GR . . . .
C5 C -0.0631(3) 0.6417(3) 0.5771(3) 0.0195(8) Uani 1 1 d . . . . .
H5A H -0.1256 0.6841 0.5734 0.029 Uiso 1 1 calc GR . . . .
H5B H -0.0587 0.5959 0.6347 0.029 Uiso 1 1 calc GR . . . .
H5C H -0.0506 0.6080 0.5283 0.029 Uiso 1 1 calc GR . . . .
C6 C 0.0984(3) 0.4898(2) 0.7207(2) 0.0166(7) Uani 1 1 d . . . . .
H6 H 0.0355 0.4798 0.7198 0.020 Uiso 1 1 calc R . . . .
C7 C 0.1546(3) 0.4746(3) 0.6332(3) 0.0216(8) Uani 1 1 d . . . . .
H7A H 0.1205 0.5175 0.5818 0.026 Uiso 1 1 calc R . . . .
H7B H 0.2147 0.4903 0.6319 0.026 Uiso 1 1 calc R . . . .
C8 C 0.1721(3) 0.3724(3) 0.6247(3) 0.0237(8) Uani 1 1 d . . . . .
H8A H 0.1122 0.3588 0.6201 0.028 Uiso 1 1 calc R . . . .
H8B H 0.2106 0.3639 0.5690 0.028 Uiso 1 1 calc R . . . .
C9 C 0.2207(3) 0.3030(3) 0.7041(3) 0.0247(9) Uani 1 1 d . . . . .
H9A H 0.2831 0.3124 0.7055 0.030 Uiso 1 1 calc R . . . .
H9B H 0.2281 0.2376 0.6977 0.030 Uiso 1 1 calc R . . . .
C10 C 0.1652(3) 0.3171(3) 0.7911(3) 0.0272(9) Uani 1 1 d . . . . .
H10A H 0.1991 0.2735 0.8424 0.033 Uiso 1 1 calc R . . . .
H10B H 0.1048 0.3021 0.7921 0.033 Uiso 1 1 calc R . . . .
C11 C 0.1490(3) 0.4191(3) 0.8002(3) 0.0242(9) Uani 1 1 d . . . . .
H11A H 0.2094 0.4323 0.8034 0.029 Uiso 1 1 calc R . . . .
H11B H 0.1117 0.4274 0.8565 0.029 Uiso 1 1 calc R . . . .
C12 C -0.0312(3) 0.6471(2) 0.7945(2) 0.0178(7) Uani 1 1 d . . . . .
H12 H -0.0789 0.6518 0.7526 0.021 Uiso 1 1 calc R . . . .
C13 C -0.0425(3) 0.5736(3) 0.8801(2) 0.0200(8) Uani 1 1 d . . . . .
H13A H 0.0096 0.5624 0.9183 0.024 Uiso 1 1 calc R . . . .
H13B H -0.0406 0.5131 0.8646 0.024 Uiso 1 1 calc R . . . .
C14 C -0.1343(3) 0.6068(3) 0.9322(2) 0.0206(8) Uani 1 1 d . . . . .
H14A H -0.1865 0.6120 0.8962 0.025 Uiso 1 1 calc R . . . .
H14B H -0.1386 0.5595 0.9886 0.025 Uiso 1 1 calc R . . . .
C15 C -0.1420(3) 0.7021(3) 0.9536(3) 0.0222(8) Uani 1 1 d . . . . .
H15A H -0.0921 0.6962 0.9926 0.027 Uiso 1 1 calc R . . . .
H15B H -0.2022 0.7225 0.9862 0.027 Uiso 1 1 calc R . . . .
C16 C -0.1342(3) 0.7757(3) 0.8677(3) 0.0266(9) Uani 1 1 d . . . . .
H16A H -0.1379 0.8370 0.8826 0.032 Uiso 1 1 calc R . . . .
H16B H -0.1866 0.7846 0.8306 0.032 Uiso 1 1 calc R . . . .
C17 C -0.0424(3) 0.7449(3) 0.8143(3) 0.0223(8) Uani 1 1 d . . . . .
H17A H 0.0098 0.7427 0.8489 0.027 Uiso 1 1 calc R . . . .
H17B H -0.0406 0.7920 0.7573 0.027 Uiso 1 1 calc R . . . .
P2 P 0.44899(7) 0.74029(7) 0.66369(7) 0.0190(2) Uani 1 1 d . . . . .
N3 N 0.4913(2) 0.5792(2) 0.7989(2) 0.0226(7) Uani 1 1 d . . . . .
N4 N 0.6087(2) 0.6434(2) 0.7684(2) 0.0194(7) Uani 1 1 d . . . . .
C21 C 0.5239(3) 0.6499(2) 0.7473(3) 0.0179(8) Uani 1 1 d . . . . .
C22 C 0.5610(3) 0.5134(3) 0.8585(3) 0.0273(9) Uani 1 1 d . . . . .
H22A H 0.5833 0.4518 0.8408 0.033 Uiso 1 1 calc R . . . .
H22B H 0.5361 0.5029 0.9216 0.033 Uiso 1 1 calc R . . . .
C23 C 0.6383(3) 0.5647(3) 0.8452(3) 0.0238(8) Uani 1 1 d . . . . .
H23A H 0.6422 0.5882 0.8989 0.029 Uiso 1 1 calc R . . . .
H23B H 0.6991 0.5230 0.8314 0.029 Uiso 1 1 calc R . . . .
C24 C 0.4088(3) 0.5519(3) 0.7876(3) 0.0322(10) Uani 1 1 d . . . . .
H24A H 0.3662 0.6056 0.7516 0.048 Uiso 1 1 calc GR . . . .
H24B H 0.3784 0.5324 0.8464 0.048 Uiso 1 1 calc GR . . . .
H24C H 0.4262 0.4991 0.7571 0.048 Uiso 1 1 calc GR . . . .
C25 C 0.6693(3) 0.7055(3) 0.7302(3) 0.0206(8) Uani 1 1 d . . . . .
H25A H 0.6496 0.7418 0.6708 0.031 Uiso 1 1 calc GR . . . .
H25B H 0.7332 0.6675 0.7249 0.031 Uiso 1 1 calc GR . . . .
H25C H 0.6659 0.7490 0.7692 0.031 Uiso 1 1 calc GR . . . .
C26 C 0.4655(3) 0.8520(2) 0.6817(2) 0.0171(7) Uani 1 1 d . . . . .
H26 H 0.5298 0.8570 0.6600 0.021 Uiso 1 1 calc R . . . .
C27 C 0.4510(3) 0.8542(3) 0.7804(3) 0.0239(8) Uani 1 1 d . . . . .
H27A H 0.4982 0.8021 0.8143 0.029 Uiso 1 1 calc R . . . .
H27B H 0.3892 0.8445 0.8032 0.029 Uiso 1 1 calc R . . . .
C28 C 0.4584(3) 0.9492(3) 0.7953(3) 0.0274(9) Uani 1 1 d . . . . .
H28A H 0.4466 0.9495 0.8598 0.033 Uiso 1 1 calc R . . . .
H28B H 0.5220 0.9563 0.7772 0.033 Uiso 1 1 calc R . . . .
C29 C 0.3898(3) 1.0317(3) 0.7423(3) 0.0294(10) Uani 1 1 d . . . . .
H29A H 0.3987 1.0917 0.7507 0.035 Uiso 1 1 calc R . . . .
H29B H 0.3259 1.0284 0.7645 0.035 Uiso 1 1 calc R . . . .
C30 C 0.4028(4) 1.0302(3) 0.6433(3) 0.0367(11) Uani 1 1 d . . . . .
H30A H 0.4642 1.0406 0.6196 0.044 Uiso 1 1 calc R . . . .
H30B H 0.3549 1.0822 0.6103 0.044 Uiso 1 1 calc R . . . .
C31 C 0.3956(4) 0.9352(3) 0.6280(3) 0.0357(11) Uani 1 1 d . . . . .
H31A H 0.3321 0.9278 0.6462 0.043 Uiso 1 1 calc R . . . .
H31B H 0.4073 0.9350 0.5635 0.043 Uiso 1 1 calc R . . . .
C32 C 0.5177(3) 0.7138(3) 0.5603(3) 0.0212(8) Uani 1 1 d . . . . .
H32 H 0.5791 0.7286 0.5575 0.025 Uiso 1 1 calc R . . . .
C33 C 0.4641(3) 0.7744(3) 0.4784(3) 0.0335(10) Uani 1 1 d . . . . .
H33A H 0.4009 0.7644 0.4848 0.040 Uiso 1 1 calc R . . . .
H33B H 0.4581 0.8421 0.4757 0.040 Uiso 1 1 calc R . . . .
C34 C 0.5134(3) 0.7490(3) 0.3911(3) 0.0337(10) Uani 1 1 d . . . . .
H34A H 0.4763 0.7877 0.3400 0.040 Uiso 1 1 calc R . . . .
H34B H 0.5745 0.7638 0.3823 0.040 Uiso 1 1 calc R . . . .
C35 C 0.5267(3) 0.6448(3) 0.3933(3) 0.0307(10) Uani 1 1 d . . . . .
H35A H 0.5608 0.6298 0.3374 0.037 Uiso 1 1 calc R . . . .
H35B H 0.4655 0.6308 0.3972 0.037 Uiso 1 1 calc R . . . .
C36 C 0.5807(3) 0.5844(3) 0.4735(3) 0.0279(9) Uani 1 1 d . . . . .
H36A H 0.6437 0.5946 0.4667 0.033 Uiso 1 1 calc R . . . .
H36B H 0.5868 0.5168 0.4756 0.033 Uiso 1 1 calc R . . . .
C37 C 0.5323(3) 0.6086(3) 0.5614(3) 0.0254(9) Uani 1 1 d . . . . .
H37A H 0.5703 0.5697 0.6118 0.030 Uiso 1 1 calc R . . . .
H37B H 0.4715 0.5929 0.5708 0.030 Uiso 1 1 calc R . . . .
P3 P 0.13625(7) 0.90825(7) 0.07460(7) 0.0185(2) Uani 1 1 d . . . . .
N5 N 0.2935(2) 0.8870(2) 0.1762(2) 0.0182(6) Uani 1 1 d . . . . .
N6 N 0.2757(2) 1.0005(2) 0.0571(2) 0.0196(7) Uani 1 1 d . . . . .
C41 C 0.2424(3) 0.9311(2) 0.1073(3) 0.0178(8) Uani 1 1 d . . . . .
C42 C 0.3719(3) 0.9282(3) 0.1763(3) 0.0206(8) Uani 1 1 d . . . . .
H42A H 0.4320 0.8816 0.1710 0.025 Uiso 1 1 calc R . . . .
H42B H 0.3690 0.9519 0.2314 0.025 Uiso 1 1 calc R . . . .
C43 C 0.3580(3) 1.0092(3) 0.0937(3) 0.0232(8) Uani 1 1 d . . . . .
H43A H 0.3467 1.0710 0.1102 0.028 Uiso 1 1 calc R . . . .
H43B H 0.4124 1.0016 0.0505 0.028 Uiso 1 1 calc R . . . .
C44 C 0.2820(3) 0.8085(3) 0.2489(3) 0.0263(9) Uani 1 1 d . . . . .
H44A H 0.2273 0.7888 0.2403 0.039 Uiso 1 1 calc GR . . . .
H44B H 0.2738 0.8283 0.3059 0.039 Uiso 1 1 calc GR . . . .
H44C H 0.3370 0.7555 0.2494 0.039 Uiso 1 1 calc GR . . . .
C45 C 0.2446(3) 1.0614(3) -0.0284(3) 0.0263(9) Uani 1 1 d . . . . .
H45A H 0.2919 1.0467 -0.0761 0.039 Uiso 1 1 calc GR . . . .
H45B H 0.2347 1.1277 -0.0256 0.039 Uiso 1 1 calc GR . . . .
H45C H 0.1865 1.0507 -0.0408 0.039 Uiso 1 1 calc GR . . . .
C46 C 0.0596(3) 0.9099(3) 0.1786(3) 0.0207(8) Uani 1 1 d . . . . .
H46 H 0.0860 0.8543 0.2268 0.025 Uiso 1 1 calc R . . . .
C47 C 0.0497(3) 1.0013(3) 0.2093(3) 0.0280(9) Uani 1 1 d . . . . .
H47A H 0.0293 1.0560 0.1593 0.034 Uiso 1 1 calc R . . . .
H47B H 0.1108 1.0030 0.2257 0.034 Uiso 1 1 calc R . . . .
C48 C -0.0200(3) 1.0097(3) 0.2896(3) 0.0339(10) Uani 1 1 d . . . . .
H48A H 0.0038 0.9590 0.3417 0.041 Uiso 1 1 calc R . . . .
H48B H -0.0271 1.0712 0.3054 0.041 Uiso 1 1 calc R . . . .
C49 C -0.1139(3) 1.0021(3) 0.2696(3) 0.0310(10) Uani 1 1 d . . . . .
H49A H -0.1563 1.0036 0.3239 0.037 Uiso 1 1 calc R . . . .
H49B H -0.1410 1.0568 0.2220 0.037 Uiso 1 1 calc R . . . .
C50 C -0.1047(3) 0.9115(3) 0.2397(3) 0.0329(10) Uani 1 1 d . . . . .
H50A H -0.1660 0.9092 0.2245 0.039 Uiso 1 1 calc R . . . .
H50B H -0.0828 0.8568 0.2893 0.039 Uiso 1 1 calc R . . . .
C51 C -0.0360(3) 0.9050(3) 0.1578(3) 0.0325(10) Uani 1 1 d . . . . .
H51A H -0.0302 0.8448 0.1399 0.039 Uiso 1 1 calc R . . . .
H51B H -0.0598 0.9576 0.1071 0.039 Uiso 1 1 calc R . . . .
C52 C 0.1846(3) 0.7835(3) 0.0632(3) 0.0195(8) Uani 1 1 d . . . . .
H52 H 0.2168 0.7451 0.1182 0.023 Uiso 1 1 calc R . . . .
C53 C 0.1073(3) 0.7410(3) 0.0490(3) 0.0267(9) Uani 1 1 d . . . . .
H53A H 0.0659 0.7352 0.1040 0.032 Uiso 1 1 calc R . . . .
H53B H 0.0700 0.7841 -0.0003 0.032 Uiso 1 1 calc R . . . .
C54 C 0.1454(3) 0.6446(3) 0.0267(3) 0.0295(10) Uani 1 1 d . . . . .
H54A H 0.1751 0.5994 0.0796 0.035 Uiso 1 1 calc R . . . .
H54B H 0.0935 0.6221 0.0137 0.035 Uiso 1 1 calc R . . . .
C55 C 0.2156(3) 0.6454(3) -0.0526(3) 0.0291(9) Uani 1 1 d . . . . .
H55A H 0.1844 0.6836 -0.1075 0.035 Uiso 1 1 calc R . . . .
H55B H 0.2421 0.5801 -0.0611 0.035 Uiso 1 1 calc R . . . .
C56 C 0.2927(3) 0.6865(3) -0.0378(3) 0.0344(11) Uani 1 1 d . . . . .
H56A H 0.3357 0.6902 -0.0919 0.041 Uiso 1 1 calc R . . . .
H56B H 0.3282 0.6441 0.0130 0.041 Uiso 1 1 calc R . . . .
C57 C 0.2547(3) 0.7848(3) -0.0183(3) 0.0293(10) Uani 1 1 d . . . . .
H57A H 0.2242 0.8286 -0.0714 0.035 Uiso 1 1 calc R . . . .
H57B H 0.3065 0.8083 -0.0067 0.035 Uiso 1 1 calc R . . . .
F16A F 0.2273(5) 0.0190(5) 0.3047(4) 0.036(2) Uiso 0.5 1 d . . P B 1
F15A F 0.2487(4) -0.0688(3) 0.4772(4) 0.0341(13) Uiso 0.5 1 d . . P B 1
F14B F 0.2482(5) -0.0769(4) 0.4445(6) 0.0119(17) Uiso 0.25 1 d . . P B 2
F17A F 0.0955(4) 0.0556(4) 0.4338(4) 0.0275(18) Uiso 0.5 1 d . . P D 1
F15B F 0.2141(7) 0.0711(7) 0.5239(4) 0.016(2) Uiso 0.25 1 d . . P B 2
F18A F 0.1961(5) 0.1854(3) 0.3576(4) 0.0234(19) Uiso 0.5 1 d . . P B 1
F16B F 0.1814(9) 0.1808(5) 0.3529(8) 0.033(5) Uiso 0.25 1 d . . P B 2
F13A F 0.2118(4) 0.0988(5) 0.5210(4) 0.0322(16) Uiso 0.5 1 d . . P E 1
F17B F 0.0932(7) 0.0668(8) 0.4102(8) 0.011(2) Uiso 0.25 1 d . . P F 2
F13B F 0.3462(4) 0.0514(7) 0.3839(7) 0.017(3) Uiso 0.25 1 d . . P B 2
F14A F 0.3483(3) 0.0543(4) 0.4049(4) 0.0250(16) Uiso 0.5 1 d . . P B 1
F18B F 0.2285(8) 0.0422(9) 0.2875(8) 0.020(3) Uiso 0.25 1 d . . P G 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.01981(13) 0.01449(12) 0.02116(13) -0.00300(10) 0.00216(10) -0.00813(10)
F1 0.0315(13) 0.0244(12) 0.0269(13) -0.0026(10) 0.0093(10) -0.0097(10)
F2 0.0385(15) 0.0326(14) 0.0251(13) -0.0024(11) 0.0085(11) -0.0149(11)
F3 0.0320(14) 0.0268(13) 0.0306(14) -0.0086(11) 0.0013(11) 0.0031(11)
F4 0.0523(18) 0.0482(16) 0.0391(16) -0.0153(13) -0.0017(13) -0.0348(14)
F5 0.0244(13) 0.0312(14) 0.0479(17) 0.0093(12) -0.0010(12) -0.0039(11)
F6 0.0293(13) 0.0329(13) 0.0437(16) -0.0218(12) 0.0070(11) -0.0160(11)
Sb2 0.02198(13) 0.01342(12) 0.02030(13) -0.00524(10) 0.00554(10) -0.00702(10)
F7 0.0398(16) 0.0409(15) 0.0442(16) -0.0253(13) 0.0019(12) -0.0143(12)
F8 0.0391(15) 0.0226(12) 0.0359(15) -0.0052(11) -0.0077(12) 0.0003(11)
F9 0.0316(13) 0.0224(12) 0.0274(13) -0.0081(10) 0.0137(10) -0.0128(10)
F10 0.0306(13) 0.0348(13) 0.0220(12) -0.0102(10) 0.0040(10) -0.0144(11)
F11 0.0349(15) 0.0338(14) 0.0531(17) -0.0221(13) 0.0244(13) -0.0211(12)
F12 0.0432(16) 0.0178(12) 0.0399(16) 0.0051(11) 0.0049(12) -0.0044(11)
Sb3 0.02345(14) 0.01699(13) 0.03231(16) -0.00073(11) -0.00231(11) -0.00472(10)
P1 0.0185(5) 0.0165(4) 0.0149(5) -0.0037(4) 0.0003(4) -0.0057(4)
N1 0.0204(17) 0.0196(16) 0.0220(17) -0.0033(13) 0.0024(13) -0.0085(13)
N2 0.0214(16) 0.0152(15) 0.0125(15) -0.0013(12) 0.0001(12) -0.0051(12)
C1 0.0153(17) 0.0133(16) 0.0168(18) -0.0059(14) 0.0042(14) -0.0036(13)
C2 0.030(2) 0.0169(18) 0.022(2) 0.0006(16) 0.0033(17) -0.0080(16)
C3 0.028(2) 0.0133(17) 0.0162(18) 0.0002(14) 0.0017(15) -0.0033(15)
C4 0.026(2) 0.034(2) 0.036(3) -0.002(2) -0.0022(19) -0.0186(19)
C5 0.0212(19) 0.0221(19) 0.0184(19) -0.0051(15) -0.0025(15) -0.0094(15)
C6 0.0208(19) 0.0169(17) 0.0109(17) -0.0031(14) 0.0016(14) -0.0038(14)
C7 0.027(2) 0.0186(18) 0.0150(18) -0.0023(15) 0.0027(15) -0.0016(16)
C8 0.028(2) 0.024(2) 0.0184(19) -0.0090(16) 0.0045(16) -0.0035(16)
C9 0.026(2) 0.0187(19) 0.026(2) -0.0054(16) 0.0016(17) -0.0018(16)
C10 0.037(2) 0.0181(19) 0.019(2) -0.0003(16) 0.0039(17) -0.0004(17)
C11 0.034(2) 0.0200(19) 0.0155(19) -0.0032(15) -0.0021(16) -0.0016(17)
C12 0.0195(18) 0.0173(17) 0.0178(18) -0.0050(15) 0.0025(14) -0.0072(14)
C13 0.026(2) 0.0169(18) 0.0171(19) -0.0032(15) 0.0026(15) -0.0075(15)
C14 0.025(2) 0.025(2) 0.0128(18) -0.0051(15) 0.0064(15) -0.0122(16)
C15 0.022(2) 0.024(2) 0.022(2) -0.0109(16) 0.0065(16) -0.0071(16)
C16 0.030(2) 0.0200(19) 0.027(2) -0.0057(17) 0.0094(18) -0.0061(17)
C17 0.026(2) 0.0174(18) 0.025(2) -0.0067(16) 0.0091(16) -0.0100(16)
P2 0.0184(5) 0.0170(5) 0.0234(5) -0.0064(4) 0.0021(4) -0.0072(4)
N3 0.0252(18) 0.0145(15) 0.0263(18) -0.0031(13) 0.0088(14) -0.0080(13)
N4 0.0183(16) 0.0154(15) 0.0228(17) -0.0041(13) 0.0032(13) -0.0037(12)
C21 0.0198(19) 0.0145(17) 0.0206(19) -0.0084(15) 0.0071(15) -0.0060(14)
C22 0.035(2) 0.0181(19) 0.023(2) -0.0024(16) 0.0098(18) -0.0052(17)
C23 0.030(2) 0.0179(18) 0.0184(19) -0.0025(15) 0.0045(16) -0.0012(16)
C24 0.032(2) 0.021(2) 0.046(3) -0.0094(19) 0.012(2) -0.0147(18)
C25 0.0193(19) 0.0168(18) 0.026(2) -0.0051(16) 0.0024(16) -0.0057(15)
C26 0.0174(18) 0.0119(16) 0.0218(19) -0.0041(14) 0.0009(15) -0.0040(14)
C27 0.034(2) 0.0149(18) 0.022(2) -0.0038(15) 0.0000(17) -0.0045(16)
C28 0.036(2) 0.0176(19) 0.029(2) -0.0099(17) -0.0048(18) -0.0029(17)
C29 0.032(2) 0.019(2) 0.036(2) -0.0118(18) -0.0012(19) -0.0001(17)
C30 0.055(3) 0.016(2) 0.032(3) -0.0054(18) -0.015(2) 0.007(2)
C31 0.050(3) 0.021(2) 0.034(3) -0.0122(19) -0.016(2) 0.006(2)
C32 0.022(2) 0.0198(18) 0.025(2) -0.0097(16) 0.0015(16) -0.0075(15)
C33 0.038(3) 0.029(2) 0.026(2) -0.0034(19) 0.0058(19) -0.0018(19)
C34 0.045(3) 0.030(2) 0.019(2) -0.0017(18) 0.0056(19) -0.004(2)
C35 0.035(2) 0.039(2) 0.022(2) -0.0123(19) 0.0014(18) -0.013(2)
C36 0.036(2) 0.025(2) 0.028(2) -0.0147(18) 0.0023(18) -0.0093(18)
C37 0.030(2) 0.022(2) 0.028(2) -0.0117(17) 0.0004(17) -0.0069(17)
P3 0.0177(5) 0.0156(4) 0.0231(5) -0.0020(4) -0.0006(4) -0.0080(4)
N5 0.0180(16) 0.0161(15) 0.0224(17) -0.0048(13) 0.0014(13) -0.0083(12)
N6 0.0185(16) 0.0161(15) 0.0252(18) -0.0044(13) 0.0010(13) -0.0072(13)
C41 0.0190(18) 0.0122(16) 0.024(2) -0.0084(15) 0.0039(15) -0.0050(14)
C42 0.0167(18) 0.0206(19) 0.029(2) -0.0114(16) 0.0005(16) -0.0082(15)
C43 0.0180(19) 0.0202(19) 0.037(2) -0.0123(17) 0.0032(17) -0.0108(15)
C44 0.028(2) 0.023(2) 0.028(2) 0.0023(17) -0.0070(17) -0.0129(17)
C45 0.031(2) 0.0203(19) 0.027(2) -0.0020(17) 0.0024(18) -0.0107(17)
C46 0.0200(19) 0.0184(18) 0.022(2) 0.0013(15) 0.0009(15) -0.0073(15)
C47 0.028(2) 0.025(2) 0.035(2) -0.0115(18) 0.0049(18) -0.0114(17)
C48 0.031(2) 0.037(2) 0.038(3) -0.014(2) 0.008(2) -0.014(2)
C49 0.023(2) 0.032(2) 0.034(2) -0.006(2) 0.0082(18) -0.0057(18)
C50 0.021(2) 0.034(2) 0.045(3) -0.006(2) 0.0067(19) -0.0148(18)
C51 0.023(2) 0.032(2) 0.049(3) -0.018(2) 0.006(2) -0.0137(18)
C52 0.0221(19) 0.0170(18) 0.023(2) -0.0047(15) -0.0023(15) -0.0091(15)
C53 0.023(2) 0.027(2) 0.036(2) -0.0146(19) 0.0067(18) -0.0125(17)
C54 0.030(2) 0.029(2) 0.038(3) -0.0160(19) 0.0090(19) -0.0187(18)
C55 0.027(2) 0.035(2) 0.033(2) -0.019(2) 0.0033(18) -0.0133(19)
C56 0.025(2) 0.038(3) 0.047(3) -0.024(2) 0.011(2) -0.0130(19)
C57 0.023(2) 0.034(2) 0.039(3) -0.015(2) 0.0121(18) -0.0197(18)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F1 1.879(2) . ?
Sb1 F2 1.877(2) . ?
Sb1 F3 1.875(2) . ?
Sb1 F4 1.867(2) . ?
Sb1 F5 1.871(2) . ?
Sb1 F6 1.872(2) . ?
Sb2 F7 1.871(2) . ?
Sb2 F8 1.871(2) . ?
Sb2 F9 1.874(2) . ?
Sb2 F10 1.881(2) . ?
Sb2 F11 1.874(2) . ?
Sb2 F12 1.879(2) . ?
Sb3 F14C 1.865(7) . ?
Sb3 F15C 1.812(7) . ?
Sb3 F16C 1.843(7) . ?
Sb3 F17C 1.841(7) . ?
Sb3 F16A 1.820(5) . ?
Sb3 F15A 1.874(4) . ?
Sb3 F14B 1.881(5) . ?
Sb3 F15B 1.821(6) . ?
Sb3 F18A 1.875(4) . ?
Sb3 F16B 1.845(6) . ?
Sb3 F13B 1.828(6) . ?
Sb3 F14A 1.866(4) . ?
P1 C1 1.870(4) . ?
P1 C6 1.870(4) . ?
P1 C12 1.867(4) . ?
N1 C1 1.334(5) . ?
N1 C2 1.469(5) . ?
N1 C4 1.448(5) . ?
N2 C1 1.310(5) . ?
N2 C3 1.472(5) . ?
N2 C5 1.454(5) . ?
C2 C3 1.525(6) . ?
C6 C7 1.535(5) . ?
C6 C11 1.538(5) . ?
C7 C8 1.527(5) . ?
C8 C9 1.520(6) . ?
C9 C10 1.520(5) . ?
C10 C11 1.529(5) . ?
C12 C13 1.530(5) . ?
C12 C17 1.539(5) . ?
C13 C14 1.532(5) . ?
C14 C15 1.522(5) . ?
C15 C16 1.523(6) . ?
C16 C17 1.534(5) . ?
P2 C21 1.857(4) . ?
P2 C26 1.857(4) . ?
P2 C32 1.858(4) . ?
N3 C21 1.337(5) . ?
N3 C22 1.468(5) . ?
N3 C24 1.450(5) . ?
N4 C21 1.326(5) . ?
N4 C23 1.472(5) . ?
N4 C25 1.455(5) . ?
C22 C23 1.531(6) . ?
C26 C27 1.518(5) . ?
C26 C31 1.533(5) . ?
C27 C28 1.538(5) . ?
C28 C29 1.514(6) . ?
C29 C30 1.520(6) . ?
C30 C31 1.540(6) . ?
C32 C33 1.539(6) . ?
C32 C37 1.538(5) . ?
C33 C34 1.537(6) . ?
C34 C35 1.520(6) . ?
C35 C36 1.521(6) . ?
C36 C37 1.534(5) . ?
P3 C41 1.870(4) . ?
P3 C46 1.859(4) . ?
P3 C52 1.865(4) . ?
N5 C41 1.320(5) . ?
N5 C42 1.474(5) . ?
N5 C44 1.451(5) . ?
N6 C41 1.320(5) . ?
N6 C43 1.470(5) . ?
N6 C45 1.458(5) . ?
C42 C43 1.525(6) . ?
C46 C47 1.527(5) . ?
C46 C51 1.535(6) . ?
C47 C48 1.528(6) . ?
C48 C49 1.522(6) . ?
C49 C50 1.510(6) . ?
C50 C51 1.535(6) . ?
C52 C53 1.531(5) . ?
C52 C57 1.539(5) . ?
C53 C54 1.516(5) . ?
C54 C55 1.515(6) . ?
C55 C56 1.518(6) . ?
C56 C57 1.524(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 Sb1 F1 179.25(11) . . ?
F3 Sb1 F1 89.95(11) . . ?
F3 Sb1 F2 89.56(11) . . ?
F4 Sb1 F1 90.35(11) . . ?
F4 Sb1 F2 90.21(11) . . ?
F4 Sb1 F3 89.43(12) . . ?
F4 Sb1 F5 91.23(13) . . ?
F4 Sb1 F6 179.55(13) . . ?
F5 Sb1 F1 89.77(11) . . ?
F5 Sb1 F2 90.71(11) . . ?
F5 Sb1 F3 179.29(12) . . ?
F5 Sb1 F6 89.20(12) . . ?
F6 Sb1 F1 89.51(11) . . ?
F6 Sb1 F2 89.92(11) . . ?
F6 Sb1 F3 90.14(11) . . ?
F7 Sb2 F9 89.89(11) . . ?
F7 Sb2 F10 179.46(11) . . ?
F7 Sb2 F11 90.03(12) . . ?
F7 Sb2 F12 90.18(12) . . ?
F8 Sb2 F7 91.71(12) . . ?
F8 Sb2 F9 90.83(11) . . ?
F8 Sb2 F10 88.76(11) . . ?
F8 Sb2 F11 90.39(12) . . ?
F8 Sb2 F12 177.98(12) . . ?
F9 Sb2 F10 90.38(10) . . ?
F9 Sb2 F12 88.46(11) . . ?
F11 Sb2 F9 178.78(11) . . ?
F11 Sb2 F10 89.69(11) . . ?
F11 Sb2 F12 90.32(12) . . ?
F12 Sb2 F10 89.35(12) . . ?
F15C Sb3 F14C 95.6(5) . . ?
F15C Sb3 F16C 96.0(5) . . ?
F15C Sb3 F17C 96.3(5) . . ?
F16C Sb3 F14C 166.3(7) . . ?
F17C Sb3 F14C 91.8(5) . . ?
F17C Sb3 F16C 94.2(5) . . ?
F16A Sb3 F15A 93.2(3) . . ?
F16A Sb3 F18A 95.1(3) . . ?
F16A Sb3 F14A 96.7(3) . . ?
F15A Sb3 F18A 171.6(3) . . ?
F15B Sb3 F14B 93.6(4) . . ?
F15B Sb3 F16B 98.3(5) . . ?
F15B Sb3 F13B 98.5(4) . . ?
F16B Sb3 F14B 164.9(5) . . ?
F13B Sb3 F14B 92.0(4) . . ?
F13B Sb3 F16B 95.3(5) . . ?
F14A Sb3 F15A 90.3(2) . . ?
F14A Sb3 F18A 89.2(3) . . ?
C6 P1 C1 103.76(15) . . ?
C12 P1 C1 98.95(16) . . ?
C12 P1 C6 106.41(16) . . ?
C1 N1 C2 111.3(3) . . ?
C1 N1 C4 128.8(3) . . ?
C4 N1 C2 119.6(3) . . ?
C1 N2 C3 112.1(3) . . ?
C1 N2 C5 128.9(3) . . ?
C5 N2 C3 118.9(3) . . ?
N1 C1 P1 119.2(3) . . ?
N2 C1 P1 129.8(3) . . ?
N2 C1 N1 111.0(3) . . ?
N1 C2 C3 103.0(3) . . ?
N2 C3 C2 102.6(3) . . ?
C7 C6 P1 112.1(2) . . ?
C7 C6 C11 109.3(3) . . ?
C11 C6 P1 106.6(2) . . ?
C8 C7 C6 110.9(3) . . ?
C9 C8 C7 111.8(3) . . ?
C8 C9 C10 110.6(3) . . ?
C9 C10 C11 110.3(3) . . ?
C10 C11 C6 111.6(3) . . ?
C13 C12 P1 109.8(3) . . ?
C13 C12 C17 111.4(3) . . ?
C17 C12 P1 108.1(2) . . ?
C12 C13 C14 111.0(3) . . ?
C15 C14 C13 111.2(3) . . ?
C14 C15 C16 110.2(3) . . ?
C15 C16 C17 110.9(3) . . ?
C16 C17 C12 111.2(3) . . ?
C21 P2 C26 101.99(17) . . ?
C21 P2 C32 98.54(17) . . ?
C26 P2 C32 108.66(17) . . ?
C21 N3 C22 111.5(3) . . ?
C21 N3 C24 127.4(4) . . ?
C24 N3 C22 119.4(3) . . ?
C21 N4 C23 111.8(3) . . ?
C21 N4 C25 128.9(3) . . ?
C25 N4 C23 119.2(3) . . ?
N3 C21 P2 119.3(3) . . ?
N4 C21 P2 130.2(3) . . ?
N4 C21 N3 110.4(3) . . ?
N3 C22 C23 102.7(3) . . ?
N4 C23 C22 102.5(3) . . ?
C27 C26 P2 110.6(3) . . ?
C27 C26 C31 109.9(3) . . ?
C31 C26 P2 108.6(3) . . ?
C26 C27 C28 111.0(3) . . ?
C29 C28 C27 111.6(3) . . ?
C28 C29 C30 110.6(3) . . ?
C29 C30 C31 111.1(4) . . ?
C26 C31 C30 111.2(4) . . ?
C33 C32 P2 109.0(3) . . ?
C37 C32 P2 109.1(3) . . ?
C37 C32 C33 109.4(3) . . ?
C34 C33 C32 111.3(4) . . ?
C35 C34 C33 111.3(4) . . ?
C34 C35 C36 110.0(4) . . ?
C35 C36 C37 111.4(4) . . ?
C36 C37 C32 111.5(3) . . ?
C46 P3 C41 102.23(17) . . ?
C46 P3 C52 109.17(17) . . ?
C52 P3 C41 99.32(16) . . ?
C41 N5 C42 111.8(3) . . ?
C41 N5 C44 129.7(3) . . ?
C44 N5 C42 118.4(3) . . ?
C41 N6 C43 112.0(3) . . ?
C41 N6 C45 128.3(3) . . ?
C45 N6 C43 119.6(3) . . ?
N5 C41 P3 129.8(3) . . ?
N5 C41 N6 110.8(3) . . ?
N6 C41 P3 119.5(3) . . ?
N5 C42 C43 102.6(3) . . ?
N6 C43 C42 102.8(3) . . ?
C47 C46 P3 110.1(3) . . ?
C47 C46 C51 109.2(3) . . ?
C51 C46 P3 108.0(3) . . ?
C46 C47 C48 111.7(3) . . ?
C49 C48 C47 111.4(4) . . ?
C50 C49 C48 110.7(4) . . ?
C49 C50 C51 110.8(3) . . ?
C46 C51 C50 110.9(4) . . ?
C53 C52 P3 110.6(3) . . ?
C53 C52 C57 110.0(3) . . ?
C57 C52 P3 107.3(3) . . ?
C54 C53 C52 111.9(3) . . ?
C55 C54 C53 112.9(3) . . ?
C54 C55 C56 110.5(3) . . ?
C55 C56 C57 111.5(4) . . ?
C56 C57 C52 111.4(3) . . ?
_shelx_res_file
;
TITL
CELL 0.71073 15.0277 15.0725 15.4298 75.9265 82.9831 74.1574
ZERR 6 0.0026 0.0027 0.0027 0.0032 0.0034 0.003
LATT 1
SFAC C H F N P Sb
UNIT 102 192 36 12 6 6
SADI F15C F17C F15C F16C F15C F14C F16A F15A F16A F14A F16A F18A F13B F15B =
F13B F16B F13B F14B F15B F16B F15B F14B F17C F16C F17C F14C F15A F14A F14A F18A
SADI 0.01 Sb3 F15C Sb3 F16A Sb3 F13B Sb3 F15B Sb3 F17C Sb3 F16C Sb3 F16B Sb3 =
F15A SB3 F14A SB3 F18A SB3 F14C SB3 F14B
L.S. 20
PLAN 20
SIZE 0.01 0.147 0.301
TEMP -173
fmap 2 53
acta
REM V:/8725/8725sadabs.hkl
WGHT 0.046500 3.975800
FVAR 0.06773
SB1 6 0.440164 0.268925 0.953129 11.00000 0.01981 0.01449 =
0.02116 -0.00300 0.00216 -0.00813
F1 3 0.377451 0.232605 1.063630 11.00000 0.03145 0.02440 =
0.02689 -0.00256 0.00934 -0.00974
F2 3 0.504192 0.305048 0.843539 11.00000 0.03851 0.03262 =
0.02515 -0.00244 0.00846 -0.01491
F3 3 0.541281 0.165226 0.985869 11.00000 0.03195 0.02678 =
0.03060 -0.00855 0.00132 0.00313
F4 3 0.389561 0.194240 0.902748 11.00000 0.05230 0.04824 =
0.03913 -0.01528 -0.00173 -0.03480
F5 3 0.339526 0.373112 0.921555 11.00000 0.02440 0.03117 =
0.04790 0.00926 -0.00105 -0.00392
F6 3 0.491487 0.342928 1.004150 11.00000 0.02931 0.03289 =
0.04367 -0.02177 0.00699 -0.01597
SB2 6 0.181759 0.571941 0.344119 11.00000 0.02198 0.01342 =
0.02030 -0.00524 0.00554 -0.00702
F7 3 0.217349 0.625396 0.427575 11.00000 0.03976 0.04087 =
0.04419 -0.02529 0.00193 -0.01434
F8 3 0.244250 0.450164 0.401052 11.00000 0.03912 0.02264 =
0.03589 -0.00517 -0.00765 0.00029
F9 3 0.073499 0.560584 0.415542 11.00000 0.03160 0.02244 =
0.02740 -0.00812 0.01368 -0.01281
F10 3 0.145978 0.519249 0.259371 11.00000 0.03057 0.03482 =
0.02204 -0.01024 0.00403 -0.01443
F11 3 0.288723 0.585931 0.271545 11.00000 0.03487 0.03382 =
0.05311 -0.02205 0.02445 -0.02107
F12 3 0.116464 0.692355 0.285050 11.00000 0.04319 0.01779 =
0.03988 0.00505 0.00490 -0.00442
SB3 6 0.223237 0.055650 0.409448 11.00000 0.02345 0.01699 =
0.03231 -0.00073 -0.00231 -0.00472
PART 3
F13C 3 0.266431 0.094503 0.278326 10.25000 0.07515
F14C 3 0.219756 -0.049495 0.367727 10.25000 0.08389
F15C 3 0.194804 0.007023 0.525720 10.25000 0.07847
F16C 3 0.248220 0.162142 0.428880 10.25000 0.08213
F17C 3 0.103465 0.116236 0.379367 10.25000 0.07464
F18C 3 0.355325 -0.000484 0.413380 10.25000 0.06128
PART 0
P1 5 0.086686 0.610585 0.739492 11.00000 0.01853 0.01655 =
0.01486 -0.00366 0.00032 -0.00571
N1 4 0.116886 0.751384 0.593960 11.00000 0.02041 0.01965 =
0.02196 -0.00333 0.00239 -0.00846
N2 4 0.004420 0.696698 0.569596 11.00000 0.02142 0.01515 =
0.01247 -0.00126 0.00006 -0.00509
C1 1 0.065907 0.689368 0.625931 11.00000 0.01528 0.01325 =
0.01682 -0.00594 0.00418 -0.00363
C2 1 0.089930 0.807297 0.504657 11.00000 0.03017 0.01690 =
0.02171 0.00059 0.00333 -0.00797
AFIX 23
H2A 2 0.142390 0.797909 0.459487 11.00000 -1.20000
H2B 2 0.067580 0.875486 0.504568 11.00000 -1.20000
AFIX 0
C3 1 0.012146 0.768103 0.486790 11.00000 0.02780 0.01333 =
0.01615 0.00024 0.00166 -0.00327
AFIX 23
H3A 2 -0.046388 0.818147 0.477092 11.00000 -1.20000
H3B 2 0.028672 0.738999 0.434085 11.00000 -1.20000
AFIX 0
C4 1 0.196204 0.762071 0.631295 11.00000 0.02604 0.03374 =
0.03627 -0.00174 -0.00215 -0.01861
AFIX 137
H4A 2 0.198822 0.728472 0.694234 11.00000 -1.50000
H4B 2 0.190468 0.829310 0.627085 11.00000 -1.50000
H4C 2 0.253009 0.735666 0.597835 11.00000 -1.50000
AFIX 0
C5 1 -0.063124 0.641698 0.577100 11.00000 0.02122 0.02208 =
0.01835 -0.00508 -0.00246 -0.00938
AFIX 137
H5A 2 -0.125585 0.684087 0.573436 11.00000 -1.50000
H5B 2 -0.058671 0.595935 0.634658 11.00000 -1.50000
H5C 2 -0.050633 0.608010 0.528261 11.00000 -1.50000
AFIX 0
C6 1 0.098417 0.489847 0.720738 11.00000 0.02081 0.01692 =
0.01094 -0.00313 0.00163 -0.00383
AFIX 13
H6 2 0.035506 0.479771 0.719774 11.00000 -1.20000
AFIX 0
C7 1 0.154638 0.474649 0.633204 11.00000 0.02687 0.01862 =
0.01496 -0.00234 0.00267 -0.00160
AFIX 23
H7A 2 0.120461 0.517503 0.581764 11.00000 -1.20000
H7B 2 0.214674 0.490346 0.631888 11.00000 -1.20000
AFIX 0
C8 1 0.172069 0.372422 0.624653 11.00000 0.02807 0.02374 =
0.01839 -0.00902 0.00448 -0.00350
AFIX 23
H8A 2 0.112179 0.358806 0.620138 11.00000 -1.20000
H8B 2 0.210616 0.363919 0.569029 11.00000 -1.20000
AFIX 0
C9 1 0.220652 0.303017 0.704139 11.00000 0.02624 0.01866 =
0.02619 -0.00539 0.00165 -0.00175
AFIX 23
H9A 2 0.283100 0.312408 0.705528 11.00000 -1.20000
H9B 2 0.228135 0.237560 0.697716 11.00000 -1.20000
AFIX 0
C10 1 0.165151 0.317051 0.791142 11.00000 0.03706 0.01810 =
0.01889 -0.00035 0.00387 -0.00039
AFIX 23
H10A 2 0.199135 0.273469 0.842372 11.00000 -1.20000
H10B 2 0.104784 0.302144 0.792095 11.00000 -1.20000
AFIX 0
C11 1 0.149007 0.419107 0.800171 11.00000 0.03384 0.02001 =
0.01551 -0.00320 -0.00207 -0.00160
AFIX 23
H11A 2 0.209388 0.432305 0.803442 11.00000 -1.20000
H11B 2 0.111745 0.427428 0.856486 11.00000 -1.20000
AFIX 0
C12 1 -0.031154 0.647108 0.794452 11.00000 0.01954 0.01728 =
0.01776 -0.00503 0.00252 -0.00723
AFIX 13
H12 2 -0.078870 0.651778 0.752583 11.00000 -1.20000
AFIX 0
C13 1 -0.042481 0.573564 0.880123 11.00000 0.02599 0.01687 =
0.01712 -0.00317 0.00257 -0.00754
AFIX 23
H13A 2 0.009610 0.562386 0.918276 11.00000 -1.20000
H13B 2 -0.040628 0.513080 0.864588 11.00000 -1.20000
AFIX 0
C14 1 -0.134290 0.606807 0.932177 11.00000 0.02537 0.02549 =
0.01275 -0.00506 0.00642 -0.01217
AFIX 23
H14A 2 -0.186489 0.612036 0.896249 11.00000 -1.20000
H14B 2 -0.138566 0.559467 0.988584 11.00000 -1.20000
AFIX 0
C15 1 -0.141989 0.702093 0.953606 11.00000 0.02202 0.02422 =
0.02226 -0.01089 0.00647 -0.00706
AFIX 23
H15A 2 -0.092068 0.696175 0.992585 11.00000 -1.20000
H15B 2 -0.202243 0.722515 0.986247 11.00000 -1.20000
AFIX 0
C16 1 -0.134204 0.775721 0.867681 11.00000 0.03010 0.02000 =
0.02693 -0.00572 0.00936 -0.00612
AFIX 23
H16A 2 -0.137920 0.836969 0.882579 11.00000 -1.20000
H16B 2 -0.186579 0.784594 0.830600 11.00000 -1.20000
AFIX 0
C17 1 -0.042421 0.744948 0.814332 11.00000 0.02557 0.01742 =
0.02497 -0.00666 0.00907 -0.00996
AFIX 23
H17A 2 0.009785 0.742727 0.848888 11.00000 -1.20000
H17B 2 -0.040551 0.791994 0.757267 11.00000 -1.20000
AFIX 0
P2 5 0.448994 0.740287 0.663689 11.00000 0.01845 0.01699 =
0.02338 -0.00642 0.00208 -0.00719
N3 4 0.491251 0.579230 0.798940 11.00000 0.02515 0.01451 =
0.02629 -0.00306 0.00882 -0.00796
N4 4 0.608741 0.643422 0.768371 11.00000 0.01829 0.01543 =
0.02276 -0.00405 0.00324 -0.00365
C21 1 0.523871 0.649945 0.747298 11.00000 0.01980 0.01453 =
0.02055 -0.00837 0.00712 -0.00600
C22 1 0.561034 0.513365 0.858544 11.00000 0.03547 0.01814 =
0.02325 -0.00240 0.00980 -0.00516
AFIX 23
H22A 2 0.583340 0.451772 0.840826 11.00000 -1.20000
H22B 2 0.536051 0.502912 0.921571 11.00000 -1.20000
AFIX 0
C23 1 0.638293 0.564722 0.845214 11.00000 0.02983 0.01787 =
0.01842 -0.00245 0.00446 -0.00121
AFIX 23
H23A 2 0.642153 0.588207 0.898889 11.00000 -1.20000
H23B 2 0.699107 0.522972 0.831419 11.00000 -1.20000
AFIX 0
C24 1 0.408847 0.551875 0.787581 11.00000 0.03181 0.02103 =
0.04601 -0.00938 0.01179 -0.01470
AFIX 137
H24A 2 0.366225 0.605643 0.751564 11.00000 -1.50000
H24B 2 0.378398 0.532412 0.846356 11.00000 -1.50000
H24C 2 0.426206 0.499077 0.757144 11.00000 -1.50000
AFIX 0
C25 1 0.669332 0.705518 0.730208 11.00000 0.01933 0.01682 =
0.02550 -0.00510 0.00242 -0.00568
AFIX 137
H25A 2 0.649649 0.741834 0.670832 11.00000 -1.50000
H25B 2 0.733246 0.667540 0.724867 11.00000 -1.50000
H25C 2 0.665902 0.748992 0.769230 11.00000 -1.50000
AFIX 0
C26 1 0.465530 0.852040 0.681715 11.00000 0.01740 0.01193 =
0.02178 -0.00410 0.00093 -0.00399
AFIX 13
H26 2 0.529822 0.857030 0.659953 11.00000 -1.20000
AFIX 0
C27 1 0.451038 0.854232 0.780377 11.00000 0.03377 0.01492 =
0.02150 -0.00380 0.00001 -0.00448
AFIX 23
H27A 2 0.498219 0.802112 0.814276 11.00000 -1.20000
H27B 2 0.389153 0.844469 0.803207 11.00000 -1.20000
AFIX 0
C28 1 0.458386 0.949157 0.795331 11.00000 0.03624 0.01758 =
0.02940 -0.00987 -0.00480 -0.00290
AFIX 23
H28A 2 0.446643 0.949486 0.859813 11.00000 -1.20000
H28B 2 0.522019 0.956270 0.777227 11.00000 -1.20000
AFIX 0
C29 1 0.389788 1.031709 0.742274 11.00000 0.03225 0.01935 =
0.03553 -0.01179 -0.00119 -0.00008
AFIX 23
H29A 2 0.398728 1.091702 0.750675 11.00000 -1.20000
H29B 2 0.325880 1.028386 0.764533 11.00000 -1.20000
AFIX 0
C30 1 0.402767 1.030208 0.643312 11.00000 0.05535 0.01577 =
0.03215 -0.00536 -0.01454 0.00744
AFIX 23
H30A 2 0.464238 1.040596 0.619622 11.00000 -1.20000
H30B 2 0.354872 1.082244 0.610269 11.00000 -1.20000
AFIX 0
C31 1 0.395588 0.935222 0.628016 11.00000 0.04988 0.02138 =
0.03353 -0.01225 -0.01621 0.00630
AFIX 23
H31A 2 0.332077 0.927774 0.646221 11.00000 -1.20000
H31B 2 0.407315 0.935021 0.563508 11.00000 -1.20000
AFIX 0
C32 1 0.517745 0.713836 0.560314 11.00000 0.02207 0.01985 =
0.02466 -0.00966 0.00151 -0.00750
AFIX 13
H32 2 0.579118 0.728635 0.557477 11.00000 -1.20000
AFIX 0
C33 1 0.464062 0.774403 0.478396 11.00000 0.03793 0.02882 =
0.02645 -0.00344 0.00577 -0.00180
AFIX 23
H33A 2 0.400930 0.764440 0.484789 11.00000 -1.20000
H33B 2 0.458082 0.842072 0.475664 11.00000 -1.20000
AFIX 0
C34 1 0.513372 0.748955 0.391143 11.00000 0.04540 0.02958 =
0.01857 -0.00173 0.00561 -0.00354
AFIX 23
H34A 2 0.476286 0.787708 0.339998 11.00000 -1.20000
H34B 2 0.574536 0.763786 0.382277 11.00000 -1.20000
AFIX 0
C35 1 0.526664 0.644831 0.393273 11.00000 0.03528 0.03858 =
0.02228 -0.01228 0.00140 -0.01262
AFIX 23
H35A 2 0.560762 0.629770 0.337436 11.00000 -1.20000
H35B 2 0.465499 0.630771 0.397159 11.00000 -1.20000
AFIX 0
C36 1 0.580650 0.584384 0.473484 11.00000 0.03589 0.02462 =
0.02782 -0.01467 0.00232 -0.00934
AFIX 23
H36A 2 0.643693 0.594633 0.466661 11.00000 -1.20000
H36B 2 0.586821 0.516804 0.475617 11.00000 -1.20000
AFIX 0
C37 1 0.532323 0.608552 0.561351 11.00000 0.02960 0.02180 =
0.02768 -0.01170 0.00043 -0.00688
AFIX 23
H37A 2 0.570319 0.569695 0.611839 11.00000 -1.20000
H37B 2 0.471538 0.592870 0.570832 11.00000 -1.20000
AFIX 0
P3 5 0.136252 0.908255 0.074596 11.00000 0.01772 0.01555 =
0.02310 -0.00197 -0.00060 -0.00798
N5 4 0.293540 0.887010 0.176242 11.00000 0.01797 0.01611 =
0.02241 -0.00479 0.00144 -0.00828
N6 4 0.275738 1.000525 0.057070 11.00000 0.01847 0.01606 =
0.02521 -0.00442 0.00096 -0.00721
C41 1 0.242383 0.931112 0.107290 11.00000 0.01898 0.01216 =
0.02388 -0.00842 0.00389 -0.00504
C42 1 0.371906 0.928240 0.176293 11.00000 0.01674 0.02065 =
0.02916 -0.01137 0.00049 -0.00816
AFIX 23
H42A 2 0.431986 0.881559 0.170972 11.00000 -1.20000
H42B 2 0.369026 0.951852 0.231359 11.00000 -1.20000
AFIX 0
C43 1 0.357976 1.009189 0.093747 11.00000 0.01803 0.02024 =
0.03682 -0.01229 0.00320 -0.01083
AFIX 23
H43A 2 0.346652 1.071027 0.110203 11.00000 -1.20000
H43B 2 0.412365 1.001601 0.050453 11.00000 -1.20000
AFIX 0
C44 1 0.281960 0.808536 0.248870 11.00000 0.02846 0.02341 =
0.02788 0.00228 -0.00700 -0.01286
AFIX 137
H44A 2 0.227266 0.788798 0.240336 11.00000 -1.50000
H44B 2 0.273790 0.828287 0.305946 11.00000 -1.50000
H44C 2 0.337002 0.755522 0.249382 11.00000 -1.50000
AFIX 0
C45 1 0.244649 1.061382 -0.028370 11.00000 0.03097 0.02030 =
0.02739 -0.00195 0.00239 -0.01068
AFIX 137
H45A 2 0.291864 1.046681 -0.076082 11.00000 -1.50000
H45B 2 0.234712 1.127684 -0.025616 11.00000 -1.50000
H45C 2 0.186474 1.050683 -0.040835 11.00000 -1.50000
AFIX 0
C46 1 0.059583 0.909948 0.178649 11.00000 0.01996 0.01839 =
0.02154 0.00126 0.00090 -0.00733
AFIX 13
H46 2 0.086018 0.854304 0.226780 11.00000 -1.20000
AFIX 0
C47 1 0.049740 1.001316 0.209302 11.00000 0.02767 0.02509 =
0.03482 -0.01151 0.00488 -0.01138
AFIX 23
H47A 2 0.029259 1.056004 0.159275 11.00000 -1.20000
H47B 2 0.110842 1.003025 0.225651 11.00000 -1.20000
AFIX 0
C48 1 -0.019970 1.009682 0.289614 11.00000 0.03063 0.03672 =
0.03785 -0.01403 0.00830 -0.01363
AFIX 23
H48A 2 0.003823 0.958968 0.341693 11.00000 -1.20000
H48B 2 -0.027091 1.071214 0.305389 11.00000 -1.20000
AFIX 0
C49 1 -0.113945 1.002068 0.269587 11.00000 0.02321 0.03191 =
0.03393 -0.00619 0.00820 -0.00574
AFIX 23
H49A 2 -0.156311 1.003579 0.323938 11.00000 -1.20000
H49B 2 -0.141046 1.056779 0.222007 11.00000 -1.20000
AFIX 0
C50 1 -0.104671 0.911512 0.239710 11.00000 0.02129 0.03359 =
0.04493 -0.00615 0.00665 -0.01478
AFIX 23
H50A 2 -0.166002 0.909214 0.224487 11.00000 -1.20000
H50B 2 -0.082825 0.856765 0.289275 11.00000 -1.20000
AFIX 0
C51 1 -0.036011 0.905043 0.157821 11.00000 0.02319 0.03242 =
0.04889 -0.01821 0.00566 -0.01370
AFIX 23
H51A 2 -0.030234 0.844850 0.139910 11.00000 -1.20000
H51B 2 -0.059806 0.957638 0.107129 11.00000 -1.20000
AFIX 0
C52 1 0.184551 0.783507 0.063160 11.00000 0.02206 0.01698 =
0.02252 -0.00471 -0.00228 -0.00914
AFIX 13
H52 2 0.216790 0.745147 0.118241 11.00000 -1.20000
AFIX 0
C53 1 0.107281 0.740999 0.049010 11.00000 0.02266 0.02691 =
0.03608 -0.01460 0.00668 -0.01252
AFIX 23
H53A 2 0.065854 0.735168 0.104015 11.00000 -1.20000
H53B 2 0.070029 0.784088 -0.000338 11.00000 -1.20000
AFIX 0
C54 1 0.145446 0.644571 0.026748 11.00000 0.02967 0.02921 =
0.03804 -0.01595 0.00900 -0.01866
AFIX 23
H54A 2 0.175071 0.599382 0.079597 11.00000 -1.20000
H54B 2 0.093533 0.622087 0.013682 11.00000 -1.20000
AFIX 0
C55 1 0.215570 0.645387 -0.052606 11.00000 0.02690 0.03512 =
0.03310 -0.01865 0.00325 -0.01325
AFIX 23
H55A 2 0.184446 0.683637 -0.107477 11.00000 -1.20000
H55B 2 0.242093 0.580085 -0.061051 11.00000 -1.20000
AFIX 0
C56 1 0.292722 0.686500 -0.037837 11.00000 0.02525 0.03802 =
0.04689 -0.02355 0.01128 -0.01299
AFIX 23
H56A 2 0.335671 0.690204 -0.091860 11.00000 -1.20000
H56B 2 0.328184 0.644102 0.013001 11.00000 -1.20000
AFIX 0
C57 1 0.254685 0.784770 -0.018321 11.00000 0.02308 0.03366 =
0.03899 -0.01497 0.01207 -0.01972
AFIX 23
H57A 2 0.224155 0.828625 -0.071353 11.00000 -1.20000
H57B 2 0.306512 0.808309 -0.006741 11.00000 -1.20000
AFIX 0
PART 1
F16A 3 0.227347 0.019005 0.304723 10.50000 0.03589
F15A 3 0.248736 -0.068832 0.477230 10.50000 0.03408
PART 0
PART 2
F14B 3 0.248233 -0.076864 0.444525 10.25000 0.01192
PART 0
PART 1
F17A 3 0.095528 0.055568 0.433765 10.50000 0.02751
PART 0
PART 2
F15B 3 0.214119 0.071089 0.523949 10.25000 0.01592
PART 0
PART 1
F18A 3 0.196128 0.185420 0.357632 10.50000 0.02342
PART 0
PART 2
F16B 3 0.181423 0.180830 0.352891 10.25000 0.03282
PART 0
PART 1
F13A 3 0.211821 0.098768 0.521031 10.50000 0.03219
PART 0
PART 2
F17B 3 0.093176 0.066809 0.410220 10.25000 0.01055
F13B 3 0.346166 0.051352 0.383853 10.25000 0.01737
PART 0
PART 1
F14A 3 0.348272 0.054287 0.404897 10.50000 0.02502
PART 0
PART 2
F18B 3 0.228456 0.042244 0.287539 10.25000 0.02049
HKLF 4
REM
REM R1 = 0.0376 for 11965 Fo > 4sig(Fo) and 0.0674 for all 16429 data
REM 754 parameters refined using 171 restraints
END
WGHT 0.0465 3.9758
REM Highest difference peak 1.100, deepest hole -1.660, 1-sigma level 0.188
Q1 1 0.2631 0.0579 0.3830 11.00000 0.05 1.10
Q2 1 0.2789 -0.0803 0.4588 11.00000 0.05 0.77
Q3 1 0.5221 0.2435 0.9827 11.00000 0.05 0.71
Q4 1 0.0392 0.6405 0.1981 11.00000 0.05 0.69
Q5 1 0.2397 -0.0623 0.5184 11.00000 0.05 0.69
Q6 1 0.0421 0.8236 -0.0581 11.00000 0.05 0.64
Q7 1 0.4555 0.2835 0.8737 11.00000 0.05 0.62
Q8 1 0.0973 0.8619 -0.0951 11.00000 0.05 0.61
Q9 1 0.2021 0.0253 0.5034 11.00000 0.05 0.61
Q10 1 0.1929 0.2967 0.7421 11.00000 0.05 0.58
Q11 1 0.2190 0.9576 -0.1205 11.00000 0.05 0.58
Q12 1 0.2573 0.0237 0.3131 11.00000 0.05 0.58
Q13 1 0.0621 1.1210 0.1369 11.00000 0.05 0.57
Q14 1 -0.0643 0.7790 0.0790 11.00000 0.05 0.56
Q15 1 0.5394 0.6249 0.4423 11.00000 0.05 0.56
Q16 1 0.2004 0.0417 0.3805 11.00000 0.05 0.56
Q17 1 0.2193 0.8414 -0.1412 11.00000 0.05 0.56
Q18 1 0.5579 0.5833 0.5179 11.00000 0.05 0.55
Q19 1 0.1359 0.6415 0.3155 11.00000 0.05 0.55
Q20 1 0.0013 0.7965 -0.0596 11.00000 0.05 0.54
;
_shelx_res_checksum 96040
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_8726sadabs
_database_code_depnum_ccdc_archive 'CCDC 1407667'
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_audit_block_code HAI-HA-128-01
_audit_creation_date 2014-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4813)
;
_chemical_name_common ?
_chemical_name_systematic
;
Title
;
_chemical_formula_moiety '2(C17 H20 Au Cl N2 P), 2(F6 Sb), C H2 Cl2'
_chemical_formula_sum 'C35 H42 Au2 Cl4 F12 N4 P2 Sb2'
_chemical_formula_weight 1587.90
_chemical_compound_source dichloromethane
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_symmetry_cell_setting TRICLINIC
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-p 1'
_symmetry_Int_Tables_number 2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.9015(15)
_cell_length_b 13.6615(18)
_cell_length_c 16.414(2)
_cell_angle_alpha 88.305(2)
_cell_angle_beta 69.996(2)
_cell_angle_gamma 88.438(2)
_cell_volume 2506.2(6)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9973
_cell_measurement_temperature 100
_cell_measurement_theta_max 31.3138
_cell_measurement_theta_min 2.4142
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 7.254
_exptl_absorpt_correction_T_max 0.77058
_exptl_absorpt_correction_T_min 0.37125
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details 'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.104
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.0200
0.00 -1.00 0.00 0.0200
1.00 0.00 1.00 0.0800
-1.00 0.00 -1.00 0.0700
0.00 0.00 1.00 0.0250
0.00 0.00 -1.00 0.0180
1.00 0.00 -1.00 0.0600
-1.00 0.00 1.00 0.0500
_exptl_crystal_description needle
_exptl_crystal_F_000 1492
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.04
_exptl_special_details
;
Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0334
_diffrn_reflns_av_unetI/netI 0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 74031
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 31.428
_diffrn_reflns_theta_min 1.321
_diffrn_radiation_monochromator 'Incoatec Helios mirrors'
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type 'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method 'CCD \f- and \w-scans'
_diffrn_radiation_type Mo-K\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 1\mS
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 13532
_reflns_number_total 16397
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT software (Bruker AXS, 2004)'
_computing_data_collection 'APEX2 (Bruker AXS, 2005-2013)'
_computing_data_reduction 'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 1997-2012)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL (G. M. Sheldrick, 2013)'
_computing_structure_solution 'SHELXS (G. M. Sheldrick, 2013)'
_refine_diff_density_max 6.374
_refine_diff_density_min -2.335
_refine_diff_density_rms 0.257
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 567
_refine_ls_number_reflns 16397
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0607
_refine_ls_R_factor_gt 0.0474
_refine_ls_restrained_S_all 1.035
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+20.9605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1233
_refine_ls_wR_factor_ref 0.1321
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The minimum and maximum estimated transmissions from the multi-scan
scaling are 0.3874 and 0.7855 (SADABS).
Highest peak ?
Deepest hole ?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Fixed Sof: F7A(0.5) F7B(0.5) F8A(0.5) F8B(0.5) F10A(0.5) F10B(0.5) F11A(0.5)
F11B(0.5) Cl3(0.5) Cl4(0.5) C98(0.5) H98A(0.5) H98B(0.5) Cl5(0.5) Cl6(0.5)
C99(0.5) H99A(0.5) H99B(0.5)
3.a Secondary CH2 refined with riding coordinates:
C2(H2A,H2B), C3(H3A,H3B), C22(H22A,H22B), C23(H23A,H23B), C98(H98A,H98B),
C99(H99A,H99B)
3.b Aromatic/amide H refined with riding coordinates:
C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
C16(H16), C17(H17), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
C34(H34), C35(H35), C36(H36), C37(H37)
3.c Idealised Me refined as rotating group:
C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.66278(2) 0.70376(2) 0.23987(2) 0.02094(6) Uani 1 1 d . . . . .
Cl1 Cl 0.56908(13) 0.66717(14) 0.38291(10) 0.0339(3) Uani 1 1 d . . . . .
P1 P 0.75945(12) 0.74707(10) 0.10250(9) 0.0174(2) Uani 1 1 d . . . . .
N1 N 0.6902(4) 0.6805(3) -0.0383(3) 0.0193(8) Uani 1 1 d . . . . .
N2 N 0.7330(4) 0.5658(3) 0.0435(3) 0.0190(8) Uani 1 1 d . . . . .
C1 C 0.7261(4) 0.6612(4) 0.0285(3) 0.0168(9) Uani 1 1 d . . . . .
C2 C 0.6563(5) 0.5896(5) -0.0696(4) 0.0240(11) Uani 1 1 d . . . . .
H2A H 0.6965 0.5836 -0.1330 0.029 Uiso 1 1 calc R . . . .
H2B H 0.5687 0.5870 -0.0558 0.029 Uiso 1 1 calc R . . . .
C3 C 0.6997(5) 0.5098(4) -0.0200(4) 0.0241(11) Uani 1 1 d . . . . .
H3A H 0.6354 0.4631 0.0093 0.029 Uiso 1 1 calc R . . . .
H3B H 0.7695 0.4733 -0.0590 0.029 Uiso 1 1 calc R . . . .
C4 C 0.6624(6) 0.7737(5) -0.0733(5) 0.0309(13) Uani 1 1 d . . . . .
H4A H 0.5796 0.7933 -0.0410 0.046 Uiso 1 1 calc GR . . . .
H4B H 0.6721 0.7665 -0.1346 0.046 Uiso 1 1 calc GR . . . .
H4C H 0.7166 0.8237 -0.0679 0.046 Uiso 1 1 calc GR . . . .
C5 C 0.7905(6) 0.5147(4) 0.0978(4) 0.0244(11) Uani 1 1 d . . . . .
H5A H 0.8695 0.4904 0.0616 0.037 Uiso 1 1 calc GR . . . .
H5B H 0.7414 0.4594 0.1280 0.037 Uiso 1 1 calc GR . . . .
H5C H 0.7994 0.5598 0.1405 0.037 Uiso 1 1 calc GR . . . .
C6 C 0.9215(5) 0.7379(4) 0.0656(4) 0.0188(9) Uani 1 1 d . . . . .
C7 C 0.9874(5) 0.7384(4) -0.0225(4) 0.0216(10) Uani 1 1 d . . . . .
H7 H 0.9481 0.7432 -0.0641 0.026 Uiso 1 1 calc R . . . .
C8 C 1.1118(5) 0.7319(4) -0.0492(4) 0.0257(12) Uani 1 1 d . . . . .
H8 H 1.1576 0.7325 -0.1093 0.031 Uiso 1 1 calc R . . . .
C9 C 1.1687(5) 0.7246(4) 0.0109(4) 0.0249(11) Uani 1 1 d . . . . .
H9 H 1.2535 0.7209 -0.0077 0.030 Uiso 1 1 calc R . . . .
C10 C 1.1023(5) 0.7226(5) 0.0984(4) 0.0286(12) Uani 1 1 d . . . . .
H10 H 1.1420 0.7159 0.1397 0.034 Uiso 1 1 calc R . . . .
C11 C 0.9783(5) 0.7303(5) 0.1267(4) 0.0249(11) Uani 1 1 d . . . . .
H11 H 0.9331 0.7305 0.1869 0.030 Uiso 1 1 calc R . . . .
C12 C 0.7186(5) 0.8703(4) 0.0785(4) 0.0244(11) Uani 1 1 d . . . . .
C13 C 0.8018(6) 0.9338(5) 0.0259(5) 0.0335(14) Uani 1 1 d . . . . .
H13 H 0.8832 0.9135 0.0013 0.040 Uiso 1 1 calc R . . . .
C14 C 0.7661(7) 1.0281(5) 0.0087(6) 0.0438(18) Uani 1 1 d . . . . .
H14 H 0.8229 1.0715 -0.0288 0.053 Uiso 1 1 calc R . . . .
C15 C 0.6487(8) 1.0582(5) 0.0459(7) 0.047(2) Uani 1 1 d . . . . .
H15 H 0.6249 1.1227 0.0347 0.056 Uiso 1 1 calc R . . . .
C16 C 0.5650(7) 0.9948(6) 0.0998(7) 0.0452(19) Uani 1 1 d . . . . .
H16 H 0.4840 1.0159 0.1250 0.054 Uiso 1 1 calc R . . . .
C17 C 0.5992(6) 0.9008(5) 0.1170(5) 0.0329(14) Uani 1 1 d . . . . .
H17 H 0.5423 0.8575 0.1545 0.039 Uiso 1 1 calc R . . . .
Au2 Au 0.33143(2) 0.70873(2) 0.25318(2) 0.02262(6) Uani 1 1 d . . . . .
Cl2 Cl 0.42382(13) 0.67494(15) 0.11050(10) 0.0354(4) Uani 1 1 d . . . . .
P2 P 0.23275(12) 0.74944(10) 0.38978(9) 0.0181(2) Uani 1 1 d . . . . .
N3 N 0.2621(4) 0.5657(3) 0.4529(3) 0.0193(8) Uani 1 1 d . . . . .
N4 N 0.3013(4) 0.6768(3) 0.5329(3) 0.0190(8) Uani 1 1 d . . . . .
C21 C 0.2670(4) 0.6605(4) 0.4659(3) 0.0167(9) Uani 1 1 d . . . . .
C22 C 0.2953(5) 0.5072(4) 0.5182(4) 0.0231(10) Uani 1 1 d . . . . .
H22A H 0.3600 0.4593 0.4903 0.028 Uiso 1 1 calc R . . . .
H22B H 0.2256 0.4716 0.5578 0.028 Uiso 1 1 calc R . . . .
C23 C 0.3375(5) 0.5832(4) 0.5665(4) 0.0226(10) Uani 1 1 d . . . . .
H23A H 0.2974 0.5758 0.6300 0.027 Uiso 1 1 calc R . . . .
H23B H 0.4252 0.5788 0.5527 0.027 Uiso 1 1 calc R . . . .
C24 C 0.2067(6) 0.5178(4) 0.3986(4) 0.0277(12) Uani 1 1 d . . . . .
H24A H 0.2593 0.4645 0.3674 0.042 Uiso 1 1 calc GR . . . .
H24B H 0.1938 0.5655 0.3567 0.042 Uiso 1 1 calc GR . . . .
H24C H 0.1298 0.4910 0.4350 0.042 Uiso 1 1 calc GR . . . .
C25 C 0.3237(6) 0.7675(5) 0.5687(4) 0.0294(12) Uani 1 1 d . . . . .
H25A H 0.3114 0.7573 0.6304 0.044 Uiso 1 1 calc GR . . . .
H25B H 0.2684 0.8189 0.5616 0.044 Uiso 1 1 calc GR . . . .
H25C H 0.4062 0.7874 0.5380 0.044 Uiso 1 1 calc GR . . . .
C26 C 0.0717(5) 0.7424(4) 0.4240(4) 0.0206(10) Uani 1 1 d . . . . .
C27 C 0.0036(5) 0.7354(4) 0.5126(4) 0.0232(11) Uani 1 1 d . . . . .
H27 H 0.0415 0.7357 0.5549 0.028 Uiso 1 1 calc R . . . .
C28 C -0.1200(5) 0.7280(4) 0.5377(4) 0.0259(12) Uani 1 1 d . . . . .
H28 H -0.1667 0.7241 0.5976 0.031 Uiso 1 1 calc R . . . .
C29 C -0.1752(5) 0.7263(4) 0.4764(5) 0.0281(13) Uani 1 1 d . . . . .
H29 H -0.2597 0.7212 0.4939 0.034 Uiso 1 1 calc R . . . .
C30 C -0.1076(6) 0.7319(6) 0.3901(5) 0.0353(15) Uani 1 1 d . . . . .
H30 H -0.1460 0.7292 0.3481 0.042 Uiso 1 1 calc R . . . .
C31 C 0.0163(6) 0.7415(6) 0.3625(4) 0.0325(14) Uani 1 1 d . . . . .
H31 H 0.0618 0.7473 0.3025 0.039 Uiso 1 1 calc R . . . .
C32 C 0.2703(5) 0.8702(4) 0.4131(4) 0.0241(11) Uani 1 1 d . . . . .
C33 C 0.3892(6) 0.8982(5) 0.3786(5) 0.0317(13) Uani 1 1 d . . . . .
H33 H 0.4479 0.8551 0.3424 0.038 Uiso 1 1 calc R . . . .
C34 C 0.4217(7) 0.9903(5) 0.3977(6) 0.0443(19) Uani 1 1 d . . . . .
H34 H 0.5030 1.0093 0.3758 0.053 Uiso 1 1 calc R . . . .
C35 C 0.3355(7) 1.0531(5) 0.4481(7) 0.051(2) Uani 1 1 d . . . . .
H35 H 0.3571 1.1158 0.4607 0.061 Uiso 1 1 calc R . . . .
C36 C 0.2181(7) 1.0251(5) 0.4805(7) 0.047(2) Uani 1 1 d . . . . .
H36 H 0.1590 1.0687 0.5156 0.057 Uiso 1 1 calc R . . . .
C37 C 0.1850(6) 0.9342(5) 0.4625(5) 0.0344(15) Uani 1 1 d . . . . .
H37 H 0.1034 0.9160 0.4843 0.041 Uiso 1 1 calc R . . . .
Sb2 Sb 0.50228(3) 0.28968(3) 0.25489(2) 0.02185(8) Uani 1 1 d . . . . .
F7A F 0.5901(12) 0.3940(10) 0.2615(8) 0.062(3) Uiso 0.5 1 d . . P A 1
F7B F 0.6410(8) 0.3567(6) 0.2481(5) 0.0322(16) Uiso 0.5 1 d . . P A 2
F8A F 0.3712(11) 0.3639(9) 0.2567(8) 0.057(3) Uiso 0.5 1 d . . P A 1
F8B F 0.4264(9) 0.4072(8) 0.2415(7) 0.046(2) Uiso 0.5 1 d . . P A 2
F9 F 0.4444(5) 0.2944(4) 0.3763(4) 0.0528(12) Uiso 1 1 d . . . . .
F10A F 0.4199(11) 0.1753(9) 0.2425(8) 0.061(3) Uiso 0.5 1 d . . P A 1
F10B F 0.3606(9) 0.2226(7) 0.2666(6) 0.042(2) Uiso 0.5 1 d . . P A 2
F11A F 0.6410(13) 0.2112(10) 0.2447(9) 0.070(3) Uiso 0.5 1 d . . P A 1
F11B F 0.5789(8) 0.1734(6) 0.2712(6) 0.0349(17) Uiso 0.5 1 d . . P A 2
F12 F 0.5584(5) 0.2889(4) 0.1341(3) 0.0485(11) Uiso 1 1 d . . . . .
Sb1 Sb 0.99806(3) 0.56740(3) -0.24926(3) 0.02657(9) Uani 1 1 d . . . . .
F1 F 0.8817(4) 0.6639(4) -0.2398(4) 0.0584(15) Uani 1 1 d . . . . .
F2 F 1.1116(4) 0.6630(4) -0.2608(4) 0.0545(14) Uani 1 1 d . . . . .
F3 F 1.0360(4) 0.5678(4) -0.3704(3) 0.0427(11) Uani 1 1 d . . . . .
F4 F 1.1157(4) 0.4698(4) -0.2604(3) 0.0385(10) Uani 1 1 d . . . . .
F5 F 0.8836(4) 0.4715(4) -0.2364(3) 0.0388(10) Uani 1 1 d . . . . .
F6 F 0.9611(4) 0.5648(4) -0.1282(3) 0.0402(10) Uani 1 1 d . . . . .
Cl3 Cl 0.7530(3) 0.9482(3) 0.2950(2) 0.0416(9) Uani 0.5 1 d . . P . .
Cl4 Cl 0.9564(2) 1.0132(3) 0.15175(17) 0.0313(7) Uani 0.5 1 d . . P . .
C98 C 0.8132(10) 1.0448(8) 0.2225(7) 0.022(2) Uani 0.5 1 d . . P . .
H98A H 0.8179 1.1034 0.2552 0.026 Uiso 0.5 1 calc R . P . .
H98B H 0.7603 1.0612 0.1887 0.026 Uiso 0.5 1 calc R . P . .
Cl5 Cl 0.7681(3) 1.0285(3) -0.2114(2) 0.0407(9) Uani 0.5 1 d . . P . .
Cl6 Cl 0.9777(2) 0.9495(3) -0.34331(17) 0.0323(7) Uani 0.5 1 d . . P . .
C99 C 0.8331(14) 0.9285(13) -0.2737(10) 0.045(4) Uani 0.5 1 d . . P . .
H99A H 0.7832 0.9109 -0.3084 0.054 Uiso 0.5 1 calc R . P . .
H99B H 0.8344 0.8721 -0.2348 0.054 Uiso 0.5 1 calc R . P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.01607(9) 0.02769(11) 0.01784(9) -0.00185(7) -0.00434(7) 0.00255(7)
Cl1 0.0216(6) 0.0530(10) 0.0214(6) 0.0044(6) -0.0013(5) 0.0089(6)
P1 0.0159(5) 0.0170(6) 0.0198(6) -0.0012(5) -0.0066(5) 0.0007(4)
N1 0.019(2) 0.021(2) 0.019(2) 0.0016(16) -0.0074(16) -0.0010(16)
N2 0.020(2) 0.018(2) 0.020(2) -0.0009(16) -0.0075(17) -0.0037(16)
C1 0.0118(19) 0.020(2) 0.018(2) 0.0015(17) -0.0041(17) -0.0013(16)
C2 0.021(2) 0.033(3) 0.021(2) -0.005(2) -0.011(2) -0.002(2)
C3 0.023(2) 0.024(3) 0.025(3) -0.006(2) -0.008(2) -0.005(2)
C4 0.036(3) 0.029(3) 0.034(3) 0.011(2) -0.021(3) -0.001(2)
C5 0.031(3) 0.017(2) 0.028(3) 0.002(2) -0.014(2) 0.000(2)
C6 0.018(2) 0.015(2) 0.024(2) -0.0021(18) -0.0068(19) 0.0015(17)
C7 0.022(2) 0.017(2) 0.025(3) -0.0001(19) -0.006(2) -0.0012(18)
C8 0.024(3) 0.017(2) 0.030(3) -0.001(2) -0.001(2) -0.0011(19)
C9 0.017(2) 0.017(2) 0.037(3) 0.000(2) -0.005(2) -0.0012(18)
C10 0.019(2) 0.039(3) 0.032(3) -0.002(3) -0.014(2) -0.002(2)
C11 0.021(2) 0.030(3) 0.025(3) 0.000(2) -0.009(2) -0.001(2)
C12 0.025(3) 0.018(2) 0.032(3) -0.004(2) -0.012(2) 0.004(2)
C13 0.030(3) 0.019(3) 0.052(4) 0.001(3) -0.015(3) 0.000(2)
C14 0.039(4) 0.023(3) 0.069(5) 0.004(3) -0.018(4) -0.002(3)
C15 0.042(4) 0.025(3) 0.076(6) -0.001(3) -0.023(4) 0.009(3)
C16 0.032(3) 0.030(3) 0.076(6) -0.007(4) -0.021(4) 0.011(3)
C17 0.025(3) 0.026(3) 0.048(4) -0.005(3) -0.012(3) 0.006(2)
Au2 0.01732(9) 0.03179(12) 0.01767(10) -0.00207(8) -0.00447(7) -0.00014(7)
Cl2 0.0206(6) 0.0594(11) 0.0221(6) -0.0103(7) -0.0010(5) -0.0066(6)
P2 0.0173(6) 0.0183(6) 0.0182(6) -0.0007(5) -0.0055(5) 0.0018(5)
N3 0.020(2) 0.018(2) 0.022(2) -0.0034(16) -0.0087(17) 0.0031(16)
N4 0.018(2) 0.023(2) 0.0166(19) -0.0020(16) -0.0069(16) -0.0006(16)
C21 0.0107(19) 0.020(2) 0.018(2) -0.0029(18) -0.0038(17) 0.0007(16)
C22 0.026(3) 0.020(2) 0.023(3) 0.001(2) -0.010(2) 0.003(2)
C23 0.022(2) 0.027(3) 0.021(2) 0.002(2) -0.009(2) 0.001(2)
C24 0.035(3) 0.022(3) 0.031(3) -0.007(2) -0.017(3) 0.000(2)
C25 0.036(3) 0.028(3) 0.028(3) -0.010(2) -0.016(3) -0.001(2)
C26 0.020(2) 0.018(2) 0.023(2) -0.0015(19) -0.008(2) 0.0047(18)
C27 0.021(2) 0.020(2) 0.028(3) 0.000(2) -0.008(2) -0.0009(19)
C28 0.021(2) 0.017(2) 0.033(3) -0.001(2) -0.002(2) 0.0028(19)
C29 0.022(3) 0.017(2) 0.043(3) -0.009(2) -0.007(2) 0.0022(19)
C30 0.024(3) 0.049(4) 0.036(3) -0.008(3) -0.015(3) 0.003(3)
C31 0.022(3) 0.049(4) 0.028(3) -0.008(3) -0.011(2) 0.006(3)
C32 0.025(3) 0.017(2) 0.030(3) 0.004(2) -0.010(2) -0.0005(19)
C33 0.026(3) 0.024(3) 0.043(4) 0.001(3) -0.009(3) -0.003(2)
C34 0.036(4) 0.027(3) 0.068(5) 0.004(3) -0.016(4) -0.011(3)
C35 0.039(4) 0.019(3) 0.090(7) -0.004(4) -0.017(4) -0.006(3)
C36 0.036(4) 0.016(3) 0.082(6) -0.011(3) -0.011(4) 0.003(3)
C37 0.026(3) 0.021(3) 0.055(4) -0.004(3) -0.012(3) 0.002(2)
Sb2 0.01443(15) 0.0354(2) 0.01542(15) -0.00114(13) -0.00475(12) 0.00095(13)
Sb1 0.01577(16) 0.0372(2) 0.02456(18) 0.00208(15) -0.00438(13) -0.00019(14)
F1 0.033(2) 0.053(3) 0.070(4) 0.014(3) 0.004(2) 0.019(2)
F2 0.029(2) 0.046(3) 0.071(3) -0.012(2) 0.007(2) -0.0148(19)
F3 0.029(2) 0.069(3) 0.0270(19) 0.016(2) -0.0074(16) 0.002(2)
F4 0.035(2) 0.053(3) 0.0263(19) -0.0028(18) -0.0094(16) 0.0150(19)
F5 0.031(2) 0.059(3) 0.0265(19) 0.0053(18) -0.0100(16) -0.0188(19)
F6 0.031(2) 0.060(3) 0.0268(19) -0.0133(19) -0.0047(16) -0.0054(19)
Cl3 0.0231(13) 0.066(2) 0.0333(16) 0.0235(16) -0.0073(12) -0.0148(14)
Cl4 0.0115(10) 0.065(2) 0.0147(11) -0.0043(12) -0.0009(8) 0.0048(11)
C98 0.021(5) 0.024(5) 0.015(4) -0.002(4) 0.000(4) 0.010(4)
Cl5 0.0207(13) 0.082(3) 0.0187(12) -0.0084(14) -0.0056(10) 0.0128(15)
Cl6 0.0171(11) 0.064(2) 0.0126(10) -0.0098(12) 0.0004(9) -0.0099(12)
C99 0.036(7) 0.053(9) 0.030(7) -0.002(6) 0.012(6) -0.025(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Cl1 2.2748(15) . ?
Au1 P1 2.2229(14) . ?
P1 C1 1.856(6) . ?
P1 C6 1.815(5) . ?
P1 C12 1.810(6) . ?
N1 C1 1.324(7) . ?
N1 C2 1.476(8) . ?
N1 C4 1.457(7) . ?
N2 C1 1.326(7) . ?
N2 C3 1.474(7) . ?
N2 C5 1.450(7) . ?
C2 C3 1.525(9) . ?
C6 C7 1.389(8) . ?
C6 C11 1.388(8) . ?
C7 C8 1.394(8) . ?
C8 C9 1.374(9) . ?
C9 C10 1.382(9) . ?
C10 C11 1.390(8) . ?
C12 C13 1.377(9) . ?
C12 C17 1.400(8) . ?
C13 C14 1.397(9) . ?
C14 C15 1.376(11) . ?
C15 C16 1.387(12) . ?
C16 C17 1.387(10) . ?
Au2 Cl2 2.2762(15) . ?
Au2 P2 2.2253(14) . ?
P2 C21 1.853(5) . ?
P2 C26 1.808(6) . ?
P2 C32 1.807(6) . ?
N3 C21 1.324(7) . ?
N3 C22 1.472(7) . ?
N3 C24 1.456(8) . ?
N4 C21 1.325(7) . ?
N4 C23 1.489(7) . ?
N4 C25 1.455(7) . ?
C22 C23 1.520(8) . ?
C26 C27 1.403(8) . ?
C26 C31 1.382(9) . ?
C27 C28 1.391(8) . ?
C28 C29 1.378(10) . ?
C29 C30 1.370(10) . ?
C30 C31 1.396(9) . ?
C32 C33 1.392(9) . ?
C32 C37 1.372(9) . ?
C33 C34 1.402(10) . ?
C34 C35 1.373(12) . ?
C35 C36 1.375(11) . ?
C36 C37 1.383(10) . ?
Sb2 F7A 1.818(13) . ?
Sb2 F7B 1.878(8) . ?
Sb2 F8A 1.829(12) . ?
Sb2 F8B 1.865(10) . ?
Sb2 F9 1.874(6) . ?
Sb2 F10A 1.919(13) . ?
Sb2 F10B 1.890(10) . ?
Sb2 F11A 1.904(14) . ?
Sb2 F11B 1.868(9) . ?
Sb2 F12 1.864(5) . ?
Sb1 F1 1.857(5) . ?
Sb1 F2 1.864(5) . ?
Sb1 F3 1.882(4) . ?
Sb1 F4 1.873(4) . ?
Sb1 F5 1.871(4) . ?
Sb1 F6 1.882(4) . ?
Cl3 C98 1.745(12) . ?
Cl4 C98 1.754(10) . ?
Cl5 C99 1.731(17) . ?
Cl6 C99 1.735(13) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Au1 Cl1 176.53(6) . . ?
C1 P1 Au1 110.26(16) . . ?
C6 P1 Au1 116.63(19) . . ?
C6 P1 C1 100.9(2) . . ?
C12 P1 Au1 111.5(2) . . ?
C12 P1 C1 109.1(3) . . ?
C12 P1 C6 107.9(3) . . ?
C1 N1 C2 110.5(5) . . ?
C1 N1 C4 130.5(5) . . ?
C4 N1 C2 118.1(5) . . ?
C1 N2 C3 110.8(5) . . ?
C1 N2 C5 128.7(5) . . ?
C5 N2 C3 119.0(5) . . ?
N1 C1 P1 129.3(4) . . ?
N1 C1 N2 111.9(5) . . ?
N2 C1 P1 118.7(4) . . ?
N1 C2 C3 102.9(4) . . ?
N2 C3 C2 102.8(5) . . ?
C7 C6 P1 120.3(4) . . ?
C11 C6 P1 119.0(4) . . ?
C11 C6 C7 120.6(5) . . ?
C6 C7 C8 119.2(6) . . ?
C9 C8 C7 120.4(6) . . ?
C8 C9 C10 119.9(5) . . ?
C9 C10 C11 120.7(6) . . ?
C6 C11 C10 119.0(6) . . ?
C13 C12 P1 121.7(5) . . ?
C13 C12 C17 120.4(6) . . ?
C17 C12 P1 117.9(5) . . ?
C12 C13 C14 119.7(7) . . ?
C15 C14 C13 120.1(7) . . ?
C14 C15 C16 120.3(7) . . ?
C15 C16 C17 120.2(7) . . ?
C16 C17 C12 119.3(7) . . ?
P2 Au2 Cl2 175.88(6) . . ?
C21 P2 Au2 110.46(17) . . ?
C26 P2 Au2 115.6(2) . . ?
C26 P2 C21 101.5(2) . . ?
C32 P2 Au2 112.1(2) . . ?
C32 P2 C21 108.3(3) . . ?
C32 P2 C26 108.3(3) . . ?
C21 N3 C22 110.6(5) . . ?
C21 N3 C24 128.7(5) . . ?
C24 N3 C22 119.2(5) . . ?
C21 N4 C23 110.4(5) . . ?
C21 N4 C25 131.3(5) . . ?
C25 N4 C23 117.7(5) . . ?
N3 C21 P2 118.7(4) . . ?
N3 C21 N4 112.0(5) . . ?
N4 C21 P2 129.3(4) . . ?
N3 C22 C23 103.5(4) . . ?
N4 C23 C22 102.3(4) . . ?
C27 C26 P2 120.1(4) . . ?
C31 C26 P2 119.7(5) . . ?
C31 C26 C27 120.2(5) . . ?
C28 C27 C26 119.3(6) . . ?
C29 C28 C27 120.5(6) . . ?
C30 C29 C28 119.6(6) . . ?
C29 C30 C31 121.5(7) . . ?
C26 C31 C30 118.8(6) . . ?
C33 C32 P2 118.2(5) . . ?
C37 C32 P2 121.7(5) . . ?
C37 C32 C33 120.1(6) . . ?
C32 C33 C34 119.6(7) . . ?
C35 C34 C33 119.7(7) . . ?
C34 C35 C36 120.0(7) . . ?
C35 C36 C37 120.8(7) . . ?
C32 C37 C36 119.8(6) . . ?
F7A Sb2 F8A 94.4(6) . . ?
F7A Sb2 F9 84.4(4) . . ?
F7A Sb2 F10A 175.9(6) . . ?
F7A Sb2 F11A 86.6(6) . . ?
F7A Sb2 F12 94.6(4) . . ?
F7B Sb2 F10B 177.7(4) . . ?
F8A Sb2 F9 87.2(4) . . ?
F8A Sb2 F10A 88.9(6) . . ?
F8A Sb2 F11A 176.0(5) . . ?
F8A Sb2 F12 91.5(4) . . ?
F8B Sb2 F7B 90.8(4) . . ?
F8B Sb2 F9 93.5(4) . . ?
F8B Sb2 F10B 89.3(4) . . ?
F8B Sb2 F11B 178.4(4) . . ?
F9 Sb2 F7B 91.8(3) . . ?
F9 Sb2 F10A 98.2(4) . . ?
F9 Sb2 F10B 85.9(3) . . ?
F9 Sb2 F11A 96.7(4) . . ?
F11A Sb2 F10A 89.9(6) . . ?
F11B Sb2 F7B 88.4(4) . . ?
F11B Sb2 F9 85.1(3) . . ?
F11B Sb2 F10B 91.5(4) . . ?
F12 Sb2 F7B 87.8(3) . . ?
F12 Sb2 F8B 84.8(4) . . ?
F12 Sb2 F9 178.3(2) . . ?
F12 Sb2 F10A 82.8(4) . . ?
F12 Sb2 F10B 94.5(3) . . ?
F12 Sb2 F11A 84.6(4) . . ?
F12 Sb2 F11B 96.6(3) . . ?
F1 Sb1 F2 90.3(3) . . ?
F1 Sb1 F3 90.4(2) . . ?
F1 Sb1 F4 179.2(2) . . ?
F1 Sb1 F5 89.6(2) . . ?
F1 Sb1 F6 90.5(2) . . ?
F2 Sb1 F3 90.3(2) . . ?
F2 Sb1 F4 89.8(2) . . ?
F2 Sb1 F5 179.4(2) . . ?
F2 Sb1 F6 90.2(2) . . ?
F4 Sb1 F3 88.85(19) . . ?
F4 Sb1 F6 90.26(19) . . ?
F5 Sb1 F3 90.3(2) . . ?
F5 Sb1 F4 90.3(2) . . ?
F5 Sb1 F6 89.22(19) . . ?
F6 Sb1 F3 179.0(2) . . ?
Cl3 C98 Cl4 110.6(6) . . ?
Cl5 C99 Cl6 113.2(8) . . ?
_shelx_res_file
;
TITL 8726sadabs in P-1 #2
CELL 0.71073 11.9015 13.6615 16.4136 88.3053 69.9958 88.4379
ZERR 2 0.0015 0.0018 0.0021 0.0023 0.0021 0.0023
LATT 1
SFAC C H Au Cl F N P Sb
UNIT 70 84 4 8 24 8 4 4
L.S. 10 0 0
PLAN 20
TEMP -173
REM reset to P-1 #2
BOND
fmap 2 53
acta
OMIT 0 1 0
OMIT 0 -1 1
OMIT 0 1 1
OMIT 1 0 0
OMIT -1 1 0
OMIT 1 1 0
OMIT 0 4 2
OMIT -4 1 2
OMIT -1 1 2
OMIT -1 -5 1
OMIT -1 -4 3
OMIT 1 1 2
OMIT -1 4 1
OMIT 1 -1 2
OMIT -4 2 2
REM V:/8726/8726sadabs.hkl
WGHT 0.068100 20.960499
FVAR 0.05961
AU1 3 0.662777 0.703758 0.239872 11.00000 0.01607 0.02769 =
0.01784 -0.00185 -0.00434 0.00255
CL1 4 0.569080 0.667167 0.382905 11.00000 0.02163 0.05303 =
0.02137 0.00443 -0.00133 0.00892
P1 7 0.759450 0.747072 0.102502 11.00000 0.01593 0.01696 =
0.01984 -0.00117 -0.00664 0.00067
N1 6 0.690239 0.680531 -0.038279 11.00000 0.01853 0.02088 =
0.01918 0.00165 -0.00742 -0.00101
N2 6 0.732960 0.565753 0.043522 11.00000 0.02008 0.01803 =
0.01977 -0.00092 -0.00751 -0.00367
C1 1 0.726140 0.661220 0.028546 11.00000 0.01184 0.01997 =
0.01767 0.00147 -0.00411 -0.00128
C2 1 0.656306 0.589576 -0.069630 11.00000 0.02116 0.03322 =
0.02095 -0.00495 -0.01105 -0.00176
AFIX 23
H2A 2 0.696492 0.583563 -0.133007 11.00000 -1.20000
H2B 2 0.568677 0.587044 -0.055840 11.00000 -1.20000
AFIX 0
C3 1 0.699745 0.509761 -0.019982 11.00000 0.02278 0.02432 =
0.02546 -0.00609 -0.00770 -0.00470
AFIX 23
H3A 2 0.635432 0.463108 0.009339 11.00000 -1.20000
H3B 2 0.769537 0.473314 -0.058977 11.00000 -1.20000
AFIX 0
C4 1 0.662351 0.773652 -0.073287 11.00000 0.03593 0.02908 =
0.03363 0.01103 -0.02057 -0.00118
AFIX 137
H4A 2 0.579585 0.793315 -0.040960 11.00000 -1.50000
H4B 2 0.672089 0.766529 -0.134580 11.00000 -1.50000
H4C 2 0.716620 0.823744 -0.067869 11.00000 -1.50000
AFIX 0
C5 1 0.790486 0.514708 0.097807 11.00000 0.03117 0.01727 =
0.02792 0.00165 -0.01443 0.00004
AFIX 137
H5A 2 0.869524 0.490378 0.061630 11.00000 -1.50000
H5B 2 0.741442 0.459446 0.128018 11.00000 -1.50000
H5C 2 0.799362 0.559808 0.140454 11.00000 -1.50000
AFIX 0
C6 1 0.921473 0.737854 0.065631 11.00000 0.01758 0.01509 =
0.02354 -0.00209 -0.00680 0.00154
C7 1 0.987399 0.738429 -0.022479 11.00000 0.02169 0.01702 =
0.02489 -0.00011 -0.00625 -0.00123
AFIX 43
H7 2 0.948143 0.743201 -0.064072 11.00000 -1.20000
AFIX 0
C8 1 1.111835 0.731921 -0.049163 11.00000 0.02364 0.01742 =
0.02999 -0.00054 -0.00124 -0.00110
AFIX 43
H8 2 1.157596 0.732550 -0.109283 11.00000 -1.20000
AFIX 0
C9 1 1.168681 0.724606 0.010904 11.00000 0.01669 0.01716 =
0.03741 -0.00039 -0.00489 -0.00117
AFIX 43
H9 2 1.253520 0.720928 -0.007681 11.00000 -1.20000
AFIX 0
C10 1 1.102330 0.722603 0.098412 11.00000 0.01891 0.03854 =
0.03240 -0.00200 -0.01364 -0.00170
AFIX 43
H10 2 1.141950 0.715862 0.139694 11.00000 -1.20000
AFIX 0
C11 1 0.978307 0.730340 0.126682 11.00000 0.02054 0.02988 =
0.02532 -0.00006 -0.00904 -0.00148
AFIX 43
H11 2 0.933103 0.730484 0.186896 11.00000 -1.20000
AFIX 0
C12 1 0.718555 0.870349 0.078469 11.00000 0.02528 0.01766 =
0.03201 -0.00399 -0.01220 0.00382
C13 1 0.801783 0.933766 0.025855 11.00000 0.03025 0.01886 =
0.05228 0.00110 -0.01540 -0.00002
AFIX 43
H13 2 0.883175 0.913464 0.001327 11.00000 -1.20000
AFIX 0
C14 1 0.766082 1.028105 0.008669 11.00000 0.03894 0.02285 =
0.06892 0.00368 -0.01776 -0.00188
AFIX 43
H14 2 0.822890 1.071521 -0.028763 11.00000 -1.20000
AFIX 0
C15 1 0.648712 1.058187 0.045913 11.00000 0.04216 0.02454 =
0.07601 -0.00148 -0.02306 0.00934
AFIX 43
H15 2 0.624919 1.122652 0.034656 11.00000 -1.20000
AFIX 0
C16 1 0.565000 0.994841 0.099800 11.00000 0.03210 0.02958 =
0.07564 -0.00663 -0.02115 0.01073
AFIX 43
H16 2 0.483993 1.015894 0.125032 11.00000 -1.20000
AFIX 0
C17 1 0.599231 0.900811 0.116963 11.00000 0.02453 0.02612 =
0.04768 -0.00513 -0.01208 0.00612
AFIX 43
H17 2 0.542274 0.857545 0.154454 11.00000 -1.20000
AFIX 0
AU2 3 0.331432 0.708729 0.253185 11.00000 0.01732 0.03179 =
0.01767 -0.00207 -0.00447 -0.00014
CL2 4 0.423818 0.674944 0.110503 11.00000 0.02062 0.05942 =
0.02208 -0.01034 -0.00096 -0.00664
P2 7 0.232751 0.749444 0.389782 11.00000 0.01732 0.01832 =
0.01823 -0.00072 -0.00549 0.00184
N3 6 0.262140 0.565744 0.452880 11.00000 0.01977 0.01779 =
0.02169 -0.00344 -0.00873 0.00305
N4 6 0.301332 0.676818 0.532887 11.00000 0.01848 0.02267 =
0.01656 -0.00197 -0.00690 -0.00056
C21 1 0.266972 0.660497 0.465862 11.00000 0.01065 0.02039 =
0.01831 -0.00290 -0.00382 0.00070
C22 1 0.295257 0.507156 0.518228 11.00000 0.02619 0.02034 =
0.02344 0.00147 -0.00975 0.00311
AFIX 23
H22A 2 0.360025 0.459290 0.490348 11.00000 -1.20000
H22B 2 0.225567 0.471640 0.557815 11.00000 -1.20000
AFIX 0
C23 1 0.337492 0.583176 0.566512 11.00000 0.02151 0.02658 =
0.02116 0.00184 -0.00936 0.00122
AFIX 23
H23A 2 0.297397 0.575845 0.630009 11.00000 -1.20000
H23B 2 0.425196 0.578750 0.552708 11.00000 -1.20000
AFIX 0
C24 1 0.206706 0.517781 0.398568 11.00000 0.03471 0.02171 =
0.03125 -0.00675 -0.01682 0.00038
AFIX 137
H24A 2 0.259268 0.464536 0.367402 11.00000 -1.50000
H24B 2 0.193771 0.565494 0.356736 11.00000 -1.50000
H24C 2 0.129766 0.491031 0.435009 11.00000 -1.50000
AFIX 0
C25 1 0.323655 0.767498 0.568655 11.00000 0.03639 0.02800 =
0.02812 -0.01005 -0.01585 -0.00059
AFIX 137
H25A 2 0.311398 0.757287 0.630431 11.00000 -1.50000
H25B 2 0.268405 0.818878 0.561622 11.00000 -1.50000
H25C 2 0.406197 0.787397 0.538001 11.00000 -1.50000
AFIX 0
C26 1 0.071682 0.742440 0.423995 11.00000 0.01999 0.01834 =
0.02336 -0.00146 -0.00763 0.00467
C27 1 0.003583 0.735422 0.512559 11.00000 0.02119 0.01951 =
0.02844 0.00033 -0.00779 -0.00094
AFIX 43
H27 2 0.041513 0.735746 0.554929 11.00000 -1.20000
AFIX 0
C28 1 -0.119972 0.727988 0.537680 11.00000 0.02140 0.01728 =
0.03333 -0.00095 -0.00232 0.00276
AFIX 43
H28 2 -0.166668 0.724074 0.597560 11.00000 -1.20000
AFIX 0
C29 1 -0.175236 0.726252 0.476403 11.00000 0.02180 0.01657 =
0.04319 -0.00920 -0.00695 0.00219
AFIX 43
H29 2 -0.259679 0.721159 0.493902 11.00000 -1.20000
AFIX 0
C30 1 -0.107649 0.731916 0.390110 11.00000 0.02374 0.04938 =
0.03635 -0.00848 -0.01466 0.00290
AFIX 43
H30 2 -0.145997 0.729245 0.348111 11.00000 -1.20000
AFIX 0
C31 1 0.016323 0.741526 0.362499 11.00000 0.02190 0.04942 =
0.02816 -0.00849 -0.01111 0.00633
AFIX 43
H31 2 0.061818 0.747334 0.302488 11.00000 -1.20000
AFIX 0
C32 1 0.270274 0.870229 0.413137 11.00000 0.02513 0.01703 =
0.03047 0.00379 -0.01041 -0.00051
C33 1 0.389200 0.898161 0.378635 11.00000 0.02617 0.02408 =
0.04269 0.00143 -0.00894 -0.00320
AFIX 43
H33 2 0.447929 0.855058 0.342430 11.00000 -1.20000
AFIX 0
C34 1 0.421704 0.990298 0.397672 11.00000 0.03625 0.02707 =
0.06837 0.00367 -0.01601 -0.01095
AFIX 43
H34 2 0.502994 1.009255 0.375765 11.00000 -1.20000
AFIX 0
C35 1 0.335532 1.053051 0.448128 11.00000 0.03937 0.01867 =
0.09038 -0.00435 -0.01686 -0.00608
AFIX 43
H35 2 0.357057 1.115843 0.460682 11.00000 -1.20000
AFIX 0
C36 1 0.218116 1.025063 0.480493 11.00000 0.03643 0.01632 =
0.08241 -0.01059 -0.01078 0.00289
AFIX 43
H36 2 0.159033 1.068706 0.515622 11.00000 -1.20000
AFIX 0
C37 1 0.184957 0.934152 0.462537 11.00000 0.02635 0.02070 =
0.05492 -0.00423 -0.01221 0.00185
AFIX 43
H37 2 0.103357 0.916044 0.484347 11.00000 -1.20000
AFIX 0
SB2 8 0.502283 0.289676 0.254886 11.00000 0.01443 0.03537 =
0.01542 -0.00114 -0.00475 0.00095
PART 1
F7A 5 0.590120 0.394026 0.261509 10.50000 0.06172
PART 0
PART 2
F7B 5 0.641048 0.356722 0.248053 10.50000 0.03223
PART 0
PART 1
F8A 5 0.371246 0.363915 0.256703 10.50000 0.05685
PART 0
PART 2
F8B 5 0.426433 0.407201 0.241461 10.50000 0.04592
PART 0
F9 5 0.444378 0.294365 0.376252 11.00000 0.05278
PART 1
F10A 5 0.419874 0.175308 0.242511 10.50000 0.06142
PART 0
PART 2
F10B 5 0.360566 0.222631 0.266618 10.50000 0.04209
PART 0
PART 1
F11A 5 0.640964 0.211216 0.244664 10.50000 0.06951
PART 0
PART 2
F11B 5 0.578915 0.173350 0.271154 10.50000 0.03485
PART 0
F12 5 0.558443 0.288950 0.134060 11.00000 0.04845
SB1 8 0.998061 0.567398 -0.249255 11.00000 0.01577 0.03724 =
0.02456 0.00208 -0.00438 -0.00019
F1 5 0.881667 0.663907 -0.239836 11.00000 0.03286 0.05302 =
0.07048 0.01391 0.00391 0.01904
F2 5 1.111599 0.662955 -0.260758 11.00000 0.02894 0.04616 =
0.07095 -0.01218 0.00742 -0.01482
F3 5 1.036017 0.567775 -0.370413 11.00000 0.02908 0.06908 =
0.02703 0.01648 -0.00737 0.00160
F4 5 1.115690 0.469826 -0.260392 11.00000 0.03450 0.05308 =
0.02628 -0.00279 -0.00943 0.01498
F5 5 0.883564 0.471518 -0.236407 11.00000 0.03125 0.05944 =
0.02651 0.00528 -0.01004 -0.01883
F6 5 0.961084 0.564767 -0.128218 11.00000 0.03051 0.06041 =
0.02679 -0.01331 -0.00474 -0.00544
CL3 4 0.752975 0.948201 0.295001 10.50000 0.02308 0.06582 =
0.03334 0.02348 -0.00725 -0.01478
CL4 4 0.956356 1.013208 0.151747 10.50000 0.01147 0.06499 =
0.01466 -0.00427 -0.00094 0.00482
C98 1 0.813173 1.044807 0.222537 10.50000 0.02072 0.02449 =
0.01523 -0.00238 0.00038 0.01047
AFIX 23
H98A 2 0.817917 1.103384 0.255229 10.50000 -1.20000
H98B 2 0.760265 1.061176 0.188665 10.50000 -1.20000
AFIX 0
CL5 4 0.768081 1.028532 -0.211388 10.50000 0.02074 0.08156 =
0.01869 -0.00835 -0.00563 0.01283
CL6 4 0.977682 0.949547 -0.343312 10.50000 0.01713 0.06414 =
0.01264 -0.00982 0.00037 -0.00992
C99 1 0.833065 0.928530 -0.273742 10.50000 0.03566 0.05304 =
0.02988 -0.00160 0.01164 -0.02500
AFIX 23
H99A 2 0.783171 0.910893 -0.308353 10.50000 -1.20000
H99B 2 0.834428 0.872089 -0.234825 10.50000 -1.20000
AFIX 0
HKLF 4
REM 8726sadabs in P-1 #2
REM R1 = 0.0474 for 13532 Fo > 4sig(Fo) and 0.0607 for all 16397 data
REM 567 parameters refined using 0 restraints
END
WGHT 0.0683 20.9719
REM Highest difference peak 6.374, deepest hole -2.335, 1-sigma level 0.257
Q1 1 0.6974 0.7135 0.2778 11.00000 0.05 6.37
Q2 1 0.3655 0.7036 0.2961 11.00000 0.05 5.81
Q3 1 0.2904 0.7018 0.2148 11.00000 0.05 4.40
Q4 1 0.6233 0.7048 0.2005 11.00000 0.05 4.30
Q5 1 0.4653 0.2869 0.2192 11.00000 0.05 3.85
Q6 1 1.0426 0.5651 -0.2156 11.00000 0.05 3.15
Q7 1 0.7526 0.9845 0.3187 11.00000 0.05 3.04
Q8 1 0.4469 0.2554 0.3753 11.00000 0.05 2.69
Q9 1 0.9621 0.5617 -0.2925 11.00000 0.05 2.52
Q10 1 0.6753 0.7402 0.2129 11.00000 0.05 2.51
Q11 1 0.4387 0.3275 0.3781 11.00000 0.05 2.50
Q12 1 0.7859 1.0647 -0.2159 11.00000 0.05 2.42
Q13 1 0.7580 0.9218 0.2951 11.00000 0.05 2.38
Q14 1 0.7786 0.9991 -0.2139 11.00000 0.05 2.33
Q15 1 0.5587 0.2536 0.1384 11.00000 0.05 2.32
Q16 1 0.5479 0.2876 0.2881 11.00000 0.05 2.29
Q17 1 0.9781 0.9805 -0.3383 11.00000 0.05 2.22
Q18 1 0.7390 1.0179 -0.2141 11.00000 0.05 2.22
Q19 1 0.9515 0.9786 0.1601 11.00000 0.05 2.18
Q20 1 0.5603 0.3286 0.1318 11.00000 0.05 2.12
;
_shelx_res_checksum 80562
_shelxl_version_number 2013-4
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_8866sadabs
_database_code_depnum_ccdc_archive 'CCDC 1407668'
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_audit_block_code HAI-HA-155-01
_audit_creation_date 2014-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_chemical_name_common ?
_chemical_name_systematic
;
Title
;
_chemical_formula_moiety 'C23 H30 Au Cl N2 P, F6 Sb'
_chemical_formula_sum 'C23 H30 Au Cl F6 N2 P Sb'
_chemical_formula_weight 833.62
_chemical_compound_source dichloromethane
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
_symmetry_cell_setting MONOCLINIC
_symmetry_space_group_name_H-M P21/n
_symmetry_space_group_name_Hall '-p 2yn'
_symmetry_Int_Tables_number 14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 15.8215(7)
_cell_length_b 10.3524(7)
_cell_length_c 18.0617(5)
_cell_angle_alpha 90
_cell_angle_beta 115.205(3)
_cell_angle_gamma 90
_cell_volume 2676.7(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 81778
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 33.0987
_cell_measurement_theta_min 2.8453
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 6.701
_exptl_absorpt_correction_T_max 0.70509
_exptl_absorpt_correction_T_min 0.50095
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details 'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.069
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.0300
0.00 0.00 -1.00 0.0300
-1.00 -2.00 0.00 0.0350
1.00 2.00 0.00 0.0450
2.00 -1.00 0.00 0.0550
-2.00 1.00 0.00 0.0550
_exptl_crystal_description prism
_exptl_crystal_F_000 1592
_exptl_crystal_size_max 0.11
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.06
_exptl_special_details
;
Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0246
_diffrn_reflns_av_unetI/netI 0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 76143
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 33.132
_diffrn_reflns_theta_min 3.015
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method 'CCD \f- and \w-scans'
_diffrn_radiation_monochromator 'Incoatec Helios focusing multilayer optics'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source '0.2 x 2mm^2^ focus rotating anode'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 9620
_reflns_number_total 10154
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'REVALCCD V. 1.6, 2008'
_computing_data_collection 'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction 'REVALCCD V. 1.6, 2008'
_computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 1997-2013)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL (Sheldrick, 2013)'
_computing_structure_solution 'SHELXS (Sheldrick, 2013)'
_refine_diff_density_max 0.529
_refine_diff_density_min -1.018
_refine_diff_density_rms 0.083
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.079
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 316
_refine_ls_number_reflns 10154
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0159
_refine_ls_R_factor_gt 0.0138
_refine_ls_restrained_S_all 1.079
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0131P)^2^+1.7217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0321
_refine_ls_wR_factor_ref 0.0333
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The minimum and maximum estimated transmissions from the multi-scan
scaling are 0.5017 and 0.7166 (SADABS).
Highest peak ?
Deepest hole ?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
C21(H21), C22(H22), C23(H23)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.56275(2) 0.64562(2) 0.53571(2) 0.01329(1) Uani 1 1 d . . . . .
Cl1 Cl 0.56217(2) 0.56097(3) 0.65249(2) 0.01795(6) Uani 1 1 d . . . . .
P1 P 0.57855(2) 0.74105(3) 0.43132(2) 0.01276(5) Uani 1 1 d . . . . .
N1 N 0.58184(8) 0.63885(11) 0.28666(7) 0.01449(19) Uani 1 1 d . . . . .
N2 N 0.67738(7) 0.53744(10) 0.40842(7) 0.01364(18) Uani 1 1 d . . . . .
C1 C 0.61329(9) 0.62509(12) 0.36790(8) 0.0128(2) Uani 1 1 d . . . . .
C2 C 0.48232(9) 0.65497(13) 0.22940(8) 0.0167(2) Uani 1 1 d . . . . .
H2A H 0.4457 0.6744 0.2609 0.020 Uiso 1 1 calc R . . . .
H2B H 0.4585 0.5730 0.1995 0.020 Uiso 1 1 calc R . . . .
C3 C 0.46847(11) 0.76297(15) 0.16820(9) 0.0217(3) Uani 1 1 d . . . . .
H3A H 0.4842 0.8468 0.1973 0.026 Uiso 1 1 calc R . . . .
H3B H 0.4021 0.7659 0.1281 0.026 Uiso 1 1 calc R . . . .
C4 C 0.53004(12) 0.74222(15) 0.12305(9) 0.0238(3) Uani 1 1 d . . . . .
H4A H 0.5089 0.6646 0.0879 0.029 Uiso 1 1 calc R . . . .
H4B H 0.5248 0.8176 0.0876 0.029 Uiso 1 1 calc R . . . .
C5 C 0.63145(11) 0.72497(15) 0.18486(9) 0.0220(3) Uani 1 1 d . . . . .
H5A H 0.6539 0.8060 0.2162 0.026 Uiso 1 1 calc R . . . .
H5B H 0.6705 0.7077 0.1553 0.026 Uiso 1 1 calc R . . . .
C6 C 0.64274(10) 0.61376(14) 0.24429(8) 0.0184(2) Uani 1 1 d . . . . .
H6A H 0.6249 0.5311 0.2139 0.022 Uiso 1 1 calc R . . . .
H6B H 0.7087 0.6073 0.2849 0.022 Uiso 1 1 calc R . . . .
C7 C 0.68580(10) 0.41488(13) 0.36911(9) 0.0179(2) Uani 1 1 d . . . . .
H7A H 0.7463 0.4130 0.3652 0.022 Uiso 1 1 calc R . . . .
H7B H 0.6352 0.4097 0.3130 0.022 Uiso 1 1 calc R . . . .
C8 C 0.67948(10) 0.29978(13) 0.41944(10) 0.0210(3) Uani 1 1 d . . . . .
H8A H 0.6158 0.2960 0.4170 0.025 Uiso 1 1 calc R . . . .
H8B H 0.6899 0.2192 0.3950 0.025 Uiso 1 1 calc R . . . .
C9 C 0.75023(11) 0.30728(14) 0.50840(10) 0.0234(3) Uani 1 1 d . . . . .
H9A H 0.8142 0.3001 0.5119 0.028 Uiso 1 1 calc R . . . .
H9B H 0.7403 0.2346 0.5394 0.028 Uiso 1 1 calc R . . . .
C10 C 0.73999(11) 0.43468(14) 0.54568(9) 0.0211(3) Uani 1 1 d . . . . .
H10A H 0.7897 0.4419 0.6021 0.025 Uiso 1 1 calc R . . . .
H10B H 0.6789 0.4368 0.5485 0.025 Uiso 1 1 calc R . . . .
C11 C 0.74665(9) 0.54829(13) 0.49498(8) 0.0157(2) Uani 1 1 d . . . . .
H11A H 0.7358 0.6296 0.5185 0.019 Uiso 1 1 calc R . . . .
H11B H 0.8103 0.5517 0.4974 0.019 Uiso 1 1 calc R . . . .
C12 C 0.67828(9) 0.84911(12) 0.46557(8) 0.0145(2) Uani 1 1 d . . . . .
C13 C 0.70743(9) 0.90620(13) 0.54293(8) 0.0173(2) Uani 1 1 d . . . . .
H13 H 0.6733 0.8918 0.5745 0.021 Uiso 1 1 calc R . . . .
C14 C 0.78666(10) 0.98400(13) 0.57312(9) 0.0204(2) Uani 1 1 d . . . . .
H14 H 0.8064 1.0232 0.6254 0.024 Uiso 1 1 calc R . . . .
C15 C 0.83725(10) 1.00488(13) 0.52721(10) 0.0208(3) Uani 1 1 d . . . . .
H15 H 0.8919 1.0570 0.5486 0.025 Uiso 1 1 calc R . . . .
C16 C 0.80782(10) 0.94943(14) 0.45015(10) 0.0211(3) Uani 1 1 d . . . . .
H16 H 0.8420 0.9644 0.4186 0.025 Uiso 1 1 calc R . . . .
C17 C 0.72824(10) 0.87184(13) 0.41899(9) 0.0186(2) Uani 1 1 d . . . . .
H17 H 0.7080 0.8345 0.3662 0.022 Uiso 1 1 calc R . . . .
C18 C 0.47830(9) 0.83774(13) 0.36760(8) 0.0158(2) Uani 1 1 d . . . . .
C19 C 0.38856(10) 0.79087(14) 0.35104(9) 0.0188(2) Uani 1 1 d . . . . .
H19 H 0.3814 0.7099 0.3725 0.023 Uiso 1 1 calc R . . . .
C20 C 0.31042(10) 0.86348(15) 0.30317(10) 0.0222(3) Uani 1 1 d . . . . .
H20 H 0.2496 0.8306 0.2899 0.027 Uiso 1 1 calc R . . . .
C21 C 0.32124(11) 0.98436(16) 0.27474(9) 0.0243(3) Uani 1 1 d . . . . .
H21 H 0.2676 1.0340 0.2425 0.029 Uiso 1 1 calc R . . . .
C22 C 0.40983(11) 1.03310(15) 0.29317(10) 0.0239(3) Uani 1 1 d . . . . .
H22 H 0.4166 1.1166 0.2746 0.029 Uiso 1 1 calc R . . . .
C23 C 0.48888(10) 0.95922(14) 0.33901(9) 0.0191(2) Uani 1 1 d . . . . .
H23 H 0.5495 0.9915 0.3507 0.023 Uiso 1 1 calc R . . . .
Sb1 Sb 0.43900(2) 0.82326(2) 0.84457(2) 0.01552(2) Uani 1 1 d . . . . .
F1 F 0.33848(7) 0.70616(10) 0.80300(6) 0.02672(19) Uani 1 1 d . . . . .
F2 F 0.53901(7) 0.93956(10) 0.88562(7) 0.0337(2) Uani 1 1 d . . . . .
F3 F 0.49604(7) 0.71940(10) 0.93768(6) 0.0294(2) Uani 1 1 d . . . . .
F4 F 0.37556(7) 0.91597(10) 0.89470(7) 0.0310(2) Uani 1 1 d . . . . .
F5 F 0.38021(8) 0.92449(12) 0.75010(7) 0.0370(2) Uani 1 1 d . . . . .
F6 F 0.50037(8) 0.72770(12) 0.79349(7) 0.0354(2) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.01298(2) 0.01543(2) 0.01307(2) 0.00109(1) 0.00710(2) 0.00071(1)
Cl1 0.01723(13) 0.02269(14) 0.01557(13) 0.00273(11) 0.00857(11) -0.00180(11)
P1 0.01244(13) 0.01409(13) 0.01254(13) 0.00034(10) 0.00607(11) 0.00011(10)
N1 0.0142(5) 0.0175(5) 0.0127(4) 0.0001(4) 0.0066(4) -0.0014(4)
N2 0.0137(4) 0.0137(4) 0.0137(4) -0.0006(4) 0.0060(4) -0.0004(3)
C1 0.0121(5) 0.0137(5) 0.0130(5) -0.0002(4) 0.0057(4) -0.0015(4)
C2 0.0151(5) 0.0198(6) 0.0129(5) 0.0007(4) 0.0037(4) -0.0012(4)
C3 0.0249(7) 0.0226(6) 0.0151(6) 0.0039(5) 0.0060(5) 0.0012(5)
C4 0.0330(8) 0.0248(7) 0.0139(6) 0.0014(5) 0.0101(6) -0.0043(6)
C5 0.0276(7) 0.0240(6) 0.0185(6) -0.0003(5) 0.0138(5) -0.0059(5)
C6 0.0201(6) 0.0222(6) 0.0172(6) -0.0014(5) 0.0122(5) -0.0022(5)
C7 0.0197(6) 0.0142(5) 0.0202(6) -0.0031(4) 0.0088(5) 0.0004(4)
C8 0.0203(6) 0.0139(5) 0.0300(7) 0.0013(5) 0.0119(6) 0.0009(4)
C9 0.0262(7) 0.0182(6) 0.0271(7) 0.0062(5) 0.0126(6) 0.0069(5)
C10 0.0247(7) 0.0217(6) 0.0194(6) 0.0061(5) 0.0117(5) 0.0076(5)
C11 0.0142(5) 0.0178(5) 0.0138(5) 0.0003(4) 0.0046(4) 0.0017(4)
C12 0.0141(5) 0.0133(5) 0.0163(5) -0.0004(4) 0.0067(4) -0.0002(4)
C13 0.0171(6) 0.0170(5) 0.0172(6) -0.0020(4) 0.0067(5) 0.0014(4)
C14 0.0189(6) 0.0169(6) 0.0215(6) -0.0047(5) 0.0049(5) 0.0001(5)
C15 0.0154(6) 0.0146(5) 0.0293(7) -0.0022(5) 0.0065(5) -0.0009(4)
C16 0.0193(6) 0.0177(6) 0.0290(7) -0.0009(5) 0.0131(5) -0.0029(5)
C17 0.0200(6) 0.0181(6) 0.0203(6) -0.0018(5) 0.0111(5) -0.0031(5)
C18 0.0146(5) 0.0188(5) 0.0150(5) 0.0014(4) 0.0073(4) 0.0026(4)
C19 0.0164(6) 0.0203(6) 0.0215(6) 0.0003(5) 0.0098(5) 0.0012(4)
C20 0.0155(6) 0.0296(7) 0.0218(6) 0.0001(5) 0.0082(5) 0.0040(5)
C21 0.0214(6) 0.0311(7) 0.0201(6) 0.0053(5) 0.0087(5) 0.0103(6)
C22 0.0263(7) 0.0238(6) 0.0241(7) 0.0085(5) 0.0132(6) 0.0080(5)
C23 0.0196(6) 0.0199(6) 0.0196(6) 0.0045(5) 0.0102(5) 0.0027(5)
Sb1 0.01532(4) 0.01643(4) 0.01586(4) -0.00002(3) 0.00764(3) 0.00114(3)
F1 0.0229(4) 0.0250(4) 0.0327(5) -0.0063(4) 0.0123(4) -0.0067(3)
F2 0.0218(5) 0.0278(5) 0.0447(6) -0.0012(4) 0.0077(4) -0.0071(4)
F3 0.0308(5) 0.0329(5) 0.0244(5) 0.0109(4) 0.0116(4) 0.0108(4)
F4 0.0264(5) 0.0338(5) 0.0343(5) -0.0104(4) 0.0145(4) 0.0087(4)
F5 0.0368(6) 0.0401(6) 0.0269(5) 0.0161(4) 0.0067(4) 0.0008(5)
F6 0.0352(6) 0.0452(6) 0.0375(6) -0.0111(5) 0.0268(5) 0.0018(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Cl1 2.2878(3) . ?
Au1 P1 2.2350(3) . ?
P1 C1 1.8951(13) . ?
P1 C12 1.8146(13) . ?
P1 C18 1.8131(14) . ?
N1 C1 1.3413(16) . ?
N1 C2 1.4798(18) . ?
N1 C6 1.4864(17) . ?
N2 C1 1.3249(16) . ?
N2 C7 1.4874(17) . ?
N2 C11 1.4827(17) . ?
C2 C3 1.5211(19) . ?
C3 C4 1.529(2) . ?
C4 C5 1.525(2) . ?
C5 C6 1.532(2) . ?
C7 C8 1.528(2) . ?
C8 C9 1.519(2) . ?
C9 C10 1.521(2) . ?
C10 C11 1.5215(19) . ?
C12 C13 1.4019(18) . ?
C12 C17 1.3979(18) . ?
C13 C14 1.3911(19) . ?
C14 C15 1.393(2) . ?
C15 C16 1.390(2) . ?
C16 C17 1.3942(19) . ?
C18 C19 1.4068(19) . ?
C18 C23 1.3964(19) . ?
C19 C20 1.389(2) . ?
C20 C21 1.391(2) . ?
C21 C22 1.390(2) . ?
C22 C23 1.397(2) . ?
Sb1 F1 1.8829(9) . ?
Sb1 F2 1.8719(10) . ?
Sb1 F3 1.8724(9) . ?
Sb1 F4 1.8767(9) . ?
Sb1 F5 1.8770(10) . ?
Sb1 F6 1.8803(9) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Au1 Cl1 173.205(12) . . ?
C1 P1 Au1 113.28(4) . . ?
C12 P1 Au1 112.23(5) . . ?
C12 P1 C1 99.36(6) . . ?
C18 P1 Au1 113.43(4) . . ?
C18 P1 C1 111.50(6) . . ?
C18 P1 C12 105.95(6) . . ?
C1 N1 C2 124.42(11) . . ?
C1 N1 C6 121.66(11) . . ?
C2 N1 C6 112.95(11) . . ?
C1 N2 C7 121.57(11) . . ?
C1 N2 C11 125.36(11) . . ?
C11 N2 C7 113.07(10) . . ?
N1 C1 P1 121.73(9) . . ?
N2 C1 P1 116.79(9) . . ?
N2 C1 N1 121.14(11) . . ?
N1 C2 C3 111.84(11) . . ?
C2 C3 C4 110.91(12) . . ?
C5 C4 C3 109.68(12) . . ?
C4 C5 C6 111.91(12) . . ?
N1 C6 C5 108.78(12) . . ?
N2 C7 C8 109.84(11) . . ?
C9 C8 C7 112.58(12) . . ?
C8 C9 C10 110.07(12) . . ?
C9 C10 C11 110.87(12) . . ?
N2 C11 C10 111.50(11) . . ?
C13 C12 P1 117.97(10) . . ?
C17 C12 P1 122.07(10) . . ?
C17 C12 C13 119.90(12) . . ?
C14 C13 C12 119.60(13) . . ?
C13 C14 C15 120.44(13) . . ?
C16 C15 C14 119.98(13) . . ?
C15 C16 C17 120.13(13) . . ?
C16 C17 C12 119.93(13) . . ?
C19 C18 P1 118.39(10) . . ?
C23 C18 P1 121.44(10) . . ?
C23 C18 C19 120.07(13) . . ?
C20 C19 C18 119.72(13) . . ?
C19 C20 C21 119.98(14) . . ?
C22 C21 C20 120.56(14) . . ?
C21 C22 C23 119.99(14) . . ?
C18 C23 C22 119.60(13) . . ?
F2 Sb1 F1 179.82(5) . . ?
F2 Sb1 F3 90.62(5) . . ?
F2 Sb1 F4 90.89(5) . . ?
F2 Sb1 F5 90.51(5) . . ?
F2 Sb1 F6 90.38(5) . . ?
F3 Sb1 F1 89.46(5) . . ?
F3 Sb1 F4 90.73(5) . . ?
F3 Sb1 F5 178.81(5) . . ?
F3 Sb1 F6 89.22(5) . . ?
F4 Sb1 F1 89.27(5) . . ?
F4 Sb1 F5 89.61(5) . . ?
F4 Sb1 F6 178.73(5) . . ?
F5 Sb1 F1 89.40(5) . . ?
F5 Sb1 F6 90.42(6) . . ?
F6 Sb1 F1 89.46(5) . . ?
_shelx_res_file
;
TITL 8866sadabs in P21/n #14
CELL 0.71073 15.8215 10.3524 18.0617 90 115.2046 90
ZERR 4 0.00065 0.00066 0.00054 0 0.0032 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Au Cl F N P Sb
UNIT 92 120 4 4 24 8 4 4
L.S. 10
PLAN 20
TEMP -173
REM reset to P21/n #14
BOND
fmap 2 53
acta
REM Z:/8866/8866sadabs.hkl
WGHT 0.013100 1.721700
FVAR 0.07822
AU1 3 0.562750 0.645617 0.535710 11.00000 0.01298 0.01543 =
0.01307 0.00109 0.00710 0.00071
CL1 4 0.562167 0.560965 0.652493 11.00000 0.01723 0.02269 =
0.01557 0.00273 0.00857 -0.00180
P1 7 0.578548 0.741055 0.431317 11.00000 0.01244 0.01409 =
0.01254 0.00034 0.00607 0.00011
N1 6 0.581841 0.638845 0.286665 11.00000 0.01416 0.01751 =
0.01273 0.00005 0.00664 -0.00145
N2 6 0.677385 0.537442 0.408425 11.00000 0.01366 0.01369 =
0.01371 -0.00064 0.00596 -0.00037
C1 1 0.613286 0.625087 0.367902 11.00000 0.01207 0.01369 =
0.01302 -0.00015 0.00568 -0.00149
C2 1 0.482320 0.654972 0.229397 11.00000 0.01506 0.01979 =
0.01289 0.00068 0.00367 -0.00117
AFIX 23
H2A 2 0.445738 0.674429 0.260910 11.00000 -1.20000
H2B 2 0.458468 0.573042 0.199482 11.00000 -1.20000
AFIX 0
C3 1 0.468466 0.762975 0.168196 11.00000 0.02491 0.02264 =
0.01506 0.00391 0.00598 0.00116
AFIX 23
H3A 2 0.484185 0.846831 0.197276 11.00000 -1.20000
H3B 2 0.402089 0.765873 0.128138 11.00000 -1.20000
AFIX 0
C4 1 0.530038 0.742218 0.123053 11.00000 0.03305 0.02476 =
0.01387 0.00145 0.01015 -0.00427
AFIX 23
H4A 2 0.508853 0.664589 0.087898 11.00000 -1.20000
H4B 2 0.524812 0.817557 0.087599 11.00000 -1.20000
AFIX 0
C5 1 0.631454 0.724970 0.184856 11.00000 0.02757 0.02398 =
0.01848 -0.00034 0.01378 -0.00587
AFIX 23
H5A 2 0.653943 0.806012 0.216246 11.00000 -1.20000
H5B 2 0.670471 0.707700 0.155251 11.00000 -1.20000
AFIX 0
C6 1 0.642737 0.613763 0.244290 11.00000 0.02013 0.02218 =
0.01717 -0.00141 0.01218 -0.00216
AFIX 23
H6A 2 0.624856 0.531132 0.213947 11.00000 -1.20000
H6B 2 0.708729 0.607330 0.284879 11.00000 -1.20000
AFIX 0
C7 1 0.685801 0.414883 0.369108 11.00000 0.01971 0.01417 =
0.02020 -0.00309 0.00882 0.00035
AFIX 23
H7A 2 0.746340 0.412962 0.365216 11.00000 -1.20000
H7B 2 0.635155 0.409678 0.313010 11.00000 -1.20000
AFIX 0
C8 1 0.679484 0.299781 0.419442 11.00000 0.02030 0.01392 =
0.03001 0.00133 0.01189 0.00085
AFIX 23
H8A 2 0.615811 0.296046 0.416974 11.00000 -1.20000
H8B 2 0.689892 0.219167 0.395016 11.00000 -1.20000
AFIX 0
C9 1 0.750229 0.307282 0.508396 11.00000 0.02616 0.01820 =
0.02708 0.00621 0.01260 0.00688
AFIX 23
H9A 2 0.814213 0.300061 0.511878 11.00000 -1.20000
H9B 2 0.740257 0.234586 0.539400 11.00000 -1.20000
AFIX 0
C10 1 0.739995 0.434681 0.545677 11.00000 0.02469 0.02174 =
0.01941 0.00610 0.01174 0.00760
AFIX 23
H10A 2 0.789707 0.441860 0.602103 11.00000 -1.20000
H10B 2 0.678899 0.436847 0.548539 11.00000 -1.20000
AFIX 0
C11 1 0.746650 0.548294 0.494981 11.00000 0.01419 0.01779 =
0.01380 0.00029 0.00459 0.00169
AFIX 23
H11A 2 0.735819 0.629641 0.518450 11.00000 -1.20000
H11B 2 0.810320 0.551749 0.497428 11.00000 -1.20000
AFIX 0
C12 1 0.678281 0.849113 0.465571 11.00000 0.01407 0.01332 =
0.01629 -0.00038 0.00667 -0.00019
C13 1 0.707430 0.906199 0.542926 11.00000 0.01714 0.01700 =
0.01719 -0.00199 0.00667 0.00144
AFIX 43
H13 2 0.673286 0.891838 0.574533 11.00000 -1.20000
AFIX 0
C14 1 0.786659 0.984004 0.573124 11.00000 0.01885 0.01688 =
0.02150 -0.00471 0.00492 0.00015
AFIX 43
H14 2 0.806393 1.023163 0.625409 11.00000 -1.20000
AFIX 0
C15 1 0.837253 1.004880 0.527211 11.00000 0.01535 0.01461 =
0.02928 -0.00216 0.00651 -0.00088
AFIX 43
H15 2 0.891858 1.057003 0.548568 11.00000 -1.20000
AFIX 0
C16 1 0.807821 0.949433 0.450151 11.00000 0.01932 0.01773 =
0.02904 -0.00094 0.01305 -0.00292
AFIX 43
H16 2 0.842001 0.964431 0.418643 11.00000 -1.20000
AFIX 0
C17 1 0.728236 0.871842 0.418991 11.00000 0.01999 0.01813 =
0.02027 -0.00180 0.01113 -0.00306
AFIX 43
H17 2 0.707978 0.834458 0.366162 11.00000 -1.20000
AFIX 0
C18 1 0.478298 0.837736 0.367600 11.00000 0.01458 0.01884 =
0.01496 0.00144 0.00732 0.00263
C19 1 0.388560 0.790874 0.351041 11.00000 0.01641 0.02030 =
0.02149 0.00029 0.00981 0.00118
AFIX 43
H19 2 0.381416 0.709927 0.372497 11.00000 -1.20000
AFIX 0
C20 1 0.310418 0.863479 0.303173 11.00000 0.01549 0.02957 =
0.02177 0.00006 0.00820 0.00400
AFIX 43
H20 2 0.249614 0.830553 0.289868 11.00000 -1.20000
AFIX 0
C21 1 0.321244 0.984358 0.274745 11.00000 0.02143 0.03111 =
0.02011 0.00531 0.00871 0.01031
AFIX 43
H21 2 0.267649 1.034043 0.242458 11.00000 -1.20000
AFIX 0
C22 1 0.409831 1.033104 0.293173 11.00000 0.02626 0.02383 =
0.02406 0.00853 0.01319 0.00802
AFIX 43
H22 2 0.416627 1.116633 0.274604 11.00000 -1.20000
AFIX 0
C23 1 0.488885 0.959223 0.339014 11.00000 0.01964 0.01990 =
0.01960 0.00453 0.01024 0.00269
AFIX 43
H23 2 0.549465 0.991452 0.350661 11.00000 -1.20000
AFIX 0
SB1 8 0.438996 0.823260 0.844568 11.00000 0.01532 0.01643 =
0.01586 -0.00002 0.00764 0.00114
F1 5 0.338481 0.706160 0.803002 11.00000 0.02289 0.02502 =
0.03270 -0.00634 0.01227 -0.00669
F2 5 0.539006 0.939563 0.885616 11.00000 0.02181 0.02776 =
0.04473 -0.00118 0.00768 -0.00712
F3 5 0.496044 0.719400 0.937675 11.00000 0.03080 0.03293 =
0.02438 0.01086 0.01164 0.01083
F4 5 0.375564 0.915973 0.894696 11.00000 0.02643 0.03375 =
0.03434 -0.01041 0.01445 0.00873
F5 5 0.380209 0.924490 0.750095 11.00000 0.03679 0.04008 =
0.02690 0.01609 0.00671 0.00084
F6 5 0.500369 0.727697 0.793494 11.00000 0.03518 0.04520 =
0.03751 -0.01106 0.02678 0.00185
HKLF 4
REM 8866sadabs in P21/n #14
REM R1 = 0.0138 for 9620 Fo > 4sig(Fo) and 0.0159 for all 10154 data
REM 316 parameters refined using 0 restraints
END
WGHT 0.0131 1.7219
REM Highest difference peak 0.529, deepest hole -1.018, 1-sigma level 0.083
Q1 1 0.5743 0.6823 0.4788 11.00000 0.05 0.53
Q2 1 0.6004 0.6644 0.3927 11.00000 0.05 0.51
Q3 1 0.4350 0.8204 0.0860 11.00000 0.05 0.47
Q4 1 0.7481 0.9432 0.5589 11.00000 0.05 0.45
Q5 1 0.3198 0.9181 0.2856 11.00000 0.05 0.44
Q6 1 0.6472 0.5819 0.3891 11.00000 0.05 0.44
Q7 1 0.6029 0.6227 0.4948 11.00000 0.05 0.44
Q8 1 0.5247 0.6400 0.4615 11.00000 0.05 0.41
Q9 1 0.4870 0.6566 0.5038 11.00000 0.05 0.41
Q10 1 0.6805 0.8804 0.4985 11.00000 0.05 0.41
Q11 1 0.7718 0.9070 0.4391 11.00000 0.05 0.40
Q12 1 0.7207 0.3039 0.4605 11.00000 0.05 0.40
Q13 1 0.4485 1.0011 0.3157 11.00000 0.05 0.40
Q14 1 0.5627 0.5352 0.1545 11.00000 0.05 0.39
Q15 1 0.6832 0.3542 0.3952 11.00000 0.05 0.39
Q16 1 0.4796 0.7131 0.2028 11.00000 0.05 0.39
Q17 1 0.8202 0.9843 0.5583 11.00000 0.05 0.39
Q18 1 0.5224 0.5639 0.4995 11.00000 0.05 0.39
Q19 1 0.4371 0.9360 0.4625 11.00000 0.05 0.37
Q20 1 0.3654 1.0179 0.2965 11.00000 0.05 0.37
;
_shelx_res_checksum 77048
_olex2_submission_special_instructions 'No special instructions were received'
_iucr_refine_instructions_details
;
TITL 8866sadabs in P21/n #14
CELL 0.71073 15.8215 10.3524 18.0617 90 115.2046 90
ZERR 4 0.00065 0.00066 0.00054 0 0.0032 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Au Cl F N P Sb
UNIT 92 120 4 4 24 8 4 4
L.S. 10
PLAN 20
TEMP -173
REM reset to P21/n #14
BOND
fmap 2 53
acta
REM Z:/8866/8866sadabs.hkl
WGHT 0.013100 1.721700
FVAR 0.07822
AU1 3 0.562750 0.645617 0.535710 11.00000 0.01298 0.01543 =
0.01307 0.00109 0.00710 0.00071
CL1 4 0.562167 0.560965 0.652493 11.00000 0.01723 0.02269 =
0.01557 0.00273 0.00857 -0.00180
P1 7 0.578548 0.741055 0.431317 11.00000 0.01244 0.01409 =
0.01254 0.00034 0.00607 0.00011
N1 6 0.581841 0.638845 0.286665 11.00000 0.01416 0.01751 =
0.01273 0.00005 0.00664 -0.00145
N2 6 0.677385 0.537442 0.408425 11.00000 0.01366 0.01369 =
0.01371 -0.00064 0.00596 -0.00037
C1 1 0.613286 0.625087 0.367902 11.00000 0.01207 0.01369 =
0.01302 -0.00015 0.00568 -0.00149
C2 1 0.482320 0.654972 0.229397 11.00000 0.01506 0.01979 =
0.01289 0.00068 0.00367 -0.00117
AFIX 23
H2A 2 0.445738 0.674429 0.260910 11.00000 -1.20000
H2B 2 0.458468 0.573042 0.199482 11.00000 -1.20000
AFIX 0
C3 1 0.468466 0.762975 0.168196 11.00000 0.02491 0.02264 =
0.01506 0.00391 0.00598 0.00116
AFIX 23
H3A 2 0.484185 0.846831 0.197276 11.00000 -1.20000
H3B 2 0.402089 0.765873 0.128138 11.00000 -1.20000
AFIX 0
C4 1 0.530038 0.742218 0.123053 11.00000 0.03305 0.02476 =
0.01387 0.00145 0.01015 -0.00427
AFIX 23
H4A 2 0.508853 0.664589 0.087898 11.00000 -1.20000
H4B 2 0.524812 0.817557 0.087599 11.00000 -1.20000
AFIX 0
C5 1 0.631454 0.724970 0.184856 11.00000 0.02757 0.02398 =
0.01848 -0.00034 0.01378 -0.00587
AFIX 23
H5A 2 0.653943 0.806012 0.216246 11.00000 -1.20000
H5B 2 0.670471 0.707700 0.155251 11.00000 -1.20000
AFIX 0
C6 1 0.642737 0.613763 0.244290 11.00000 0.02013 0.02218 =
0.01717 -0.00141 0.01218 -0.00216
AFIX 23
H6A 2 0.624856 0.531132 0.213947 11.00000 -1.20000
H6B 2 0.708729 0.607330 0.284879 11.00000 -1.20000
AFIX 0
C7 1 0.685801 0.414883 0.369108 11.00000 0.01971 0.01417 =
0.02020 -0.00309 0.00882 0.00035
AFIX 23
H7A 2 0.746340 0.412962 0.365216 11.00000 -1.20000
H7B 2 0.635155 0.409678 0.313010 11.00000 -1.20000
AFIX 0
C8 1 0.679484 0.299781 0.419442 11.00000 0.02030 0.01392 =
0.03001 0.00133 0.01189 0.00085
AFIX 23
H8A 2 0.615811 0.296046 0.416974 11.00000 -1.20000
H8B 2 0.689892 0.219167 0.395016 11.00000 -1.20000
AFIX 0
C9 1 0.750229 0.307282 0.508396 11.00000 0.02616 0.01820 =
0.02708 0.00621 0.01260 0.00688
AFIX 23
H9A 2 0.814213 0.300061 0.511878 11.00000 -1.20000
H9B 2 0.740257 0.234586 0.539400 11.00000 -1.20000
AFIX 0
C10 1 0.739995 0.434681 0.545677 11.00000 0.02469 0.02174 =
0.01941 0.00610 0.01174 0.00760
AFIX 23
H10A 2 0.789707 0.441860 0.602103 11.00000 -1.20000
H10B 2 0.678899 0.436847 0.548539 11.00000 -1.20000
AFIX 0
C11 1 0.746650 0.548294 0.494981 11.00000 0.01419 0.01779 =
0.01380 0.00029 0.00459 0.00169
AFIX 23
H11A 2 0.735819 0.629641 0.518450 11.00000 -1.20000
H11B 2 0.810320 0.551749 0.497428 11.00000 -1.20000
AFIX 0
C12 1 0.678281 0.849113 0.465571 11.00000 0.01407 0.01332 =
0.01629 -0.00038 0.00667 -0.00019
C13 1 0.707430 0.906199 0.542926 11.00000 0.01714 0.01700 =
0.01719 -0.00199 0.00667 0.00144
AFIX 43
H13 2 0.673286 0.891838 0.574533 11.00000 -1.20000
AFIX 0
C14 1 0.786659 0.984004 0.573124 11.00000 0.01885 0.01688 =
0.02150 -0.00471 0.00492 0.00015
AFIX 43
H14 2 0.806393 1.023163 0.625409 11.00000 -1.20000
AFIX 0
C15 1 0.837253 1.004880 0.527211 11.00000 0.01535 0.01461 =
0.02928 -0.00216 0.00651 -0.00088
AFIX 43
H15 2 0.891858 1.057003 0.548568 11.00000 -1.20000
AFIX 0
C16 1 0.807821 0.949433 0.450151 11.00000 0.01932 0.01773 =
0.02904 -0.00094 0.01305 -0.00292
AFIX 43
H16 2 0.842001 0.964431 0.418643 11.00000 -1.20000
AFIX 0
C17 1 0.728236 0.871842 0.418991 11.00000 0.01999 0.01813 =
0.02027 -0.00180 0.01113 -0.00306
AFIX 43
H17 2 0.707978 0.834458 0.366162 11.00000 -1.20000
AFIX 0
C18 1 0.478298 0.837736 0.367600 11.00000 0.01458 0.01884 =
0.01496 0.00144 0.00732 0.00263
C19 1 0.388560 0.790874 0.351041 11.00000 0.01641 0.02030 =
0.02149 0.00029 0.00981 0.00118
AFIX 43
H19 2 0.381416 0.709927 0.372497 11.00000 -1.20000
AFIX 0
C20 1 0.310418 0.863479 0.303173 11.00000 0.01549 0.02957 =
0.02177 0.00006 0.00820 0.00400
AFIX 43
H20 2 0.249614 0.830553 0.289868 11.00000 -1.20000
AFIX 0
C21 1 0.321244 0.984358 0.274745 11.00000 0.02143 0.03111 =
0.02011 0.00531 0.00871 0.01031
AFIX 43
H21 2 0.267649 1.034043 0.242458 11.00000 -1.20000
AFIX 0
C22 1 0.409831 1.033104 0.293173 11.00000 0.02626 0.02383 =
0.02406 0.00853 0.01319 0.00802
AFIX 43
H22 2 0.416627 1.116633 0.274604 11.00000 -1.20000
AFIX 0
C23 1 0.488885 0.959223 0.339014 11.00000 0.01964 0.01990 =
0.01960 0.00453 0.01024 0.00269
AFIX 43
H23 2 0.549465 0.991452 0.350661 11.00000 -1.20000
AFIX 0
SB1 8 0.438996 0.823260 0.844568 11.00000 0.01532 0.01643 =
0.01586 -0.00002 0.00764 0.00114
F1 5 0.338481 0.706160 0.803002 11.00000 0.02289 0.02502 =
0.03270 -0.00634 0.01227 -0.00669
F2 5 0.539006 0.939563 0.885616 11.00000 0.02181 0.02776 =
0.04473 -0.00118 0.00768 -0.00712
F3 5 0.496044 0.719400 0.937675 11.00000 0.03080 0.03293 =
0.02438 0.01086 0.01164 0.01083
F4 5 0.375564 0.915973 0.894696 11.00000 0.02643 0.03375 =
0.03434 -0.01041 0.01445 0.00873
F5 5 0.380209 0.924490 0.750095 11.00000 0.03679 0.04008 =
0.02690 0.01609 0.00671 0.00084
F6 5 0.500369 0.727697 0.793494 11.00000 0.03518 0.04520 =
0.03751 -0.01106 0.02678 0.00185
HKLF 4
REM 8866sadabs in P21/n #14
REM R1 = 0.0138 for 9620 Fo > 4sig(Fo) and 0.0159 for all 10154 data
REM 316 parameters refined using 0 restraints
END
WGHT 0.0131 1.7219
REM Highest difference peak 0.529, deepest hole -1.018, 1-sigma level 0.083
Q1 1 0.5743 0.6823 0.4788 11.00000 0.05 0.53
Q2 1 0.6004 0.6644 0.3927 11.00000 0.05 0.51
Q3 1 0.4350 0.8204 0.0860 11.00000 0.05 0.47
Q4 1 0.7481 0.9432 0.5589 11.00000 0.05 0.45
Q5 1 0.3198 0.9181 0.2856 11.00000 0.05 0.44
Q6 1 0.6472 0.5819 0.3891 11.00000 0.05 0.44
Q7 1 0.6029 0.6227 0.4948 11.00000 0.05 0.44
Q8 1 0.5247 0.6400 0.4615 11.00000 0.05 0.41
Q9 1 0.4870 0.6566 0.5038 11.00000 0.05 0.41
Q10 1 0.6805 0.8804 0.4985 11.00000 0.05 0.41
Q11 1 0.7718 0.9070 0.4391 11.00000 0.05 0.40
Q12 1 0.7207 0.3039 0.4605 11.00000 0.05 0.40
Q13 1 0.4485 1.0011 0.3157 11.00000 0.05 0.40
Q14 1 0.5627 0.5352 0.1545 11.00000 0.05 0.39
Q15 1 0.6832 0.3542 0.3952 11.00000 0.05 0.39
Q16 1 0.4796 0.7131 0.2028 11.00000 0.05 0.39
Q17 1 0.8202 0.9843 0.5583 11.00000 0.05 0.39
Q18 1 0.5224 0.5639 0.4995 11.00000 0.05 0.39
Q19 1 0.4371 0.9360 0.4625 11.00000 0.05 0.37
Q20 1 0.3654 1.0179 0.2965 11.00000 0.05 0.37
REM The information below was added by Olex2.
REM
REM R1 = 0.0138 for 9620 Fo > 4sig(Fo) and 0.0159 for all 78128 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.53, deepest hole -1.02
REM Mean Shift 0, Max Shift 0.006.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0159
REM R1_gt = 0.0138
REM wR_ref = 0.0333
REM GOOF = 1.079
REM Shift_max = 0.006
REM Shift_mean = 0
REM Reflections_all = 78128
REM Reflections_gt = 9620
REM Parameters = n/a
REM Hole = -1.02
REM Peak = 0.53
REM Flack = n/a
;
_shelxl_version_number 2014-3
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_8888
_database_code_depnum_ccdc_archive 'CCDC 1407669'
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_audit_creation_date 2014-07-23
_audit_block_code HAI-HA-156-01
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic
;
Title
;
_chemical_name_common ?
_chemical_compound_source dichloromethane
_chemical_melting_point ?
_chemical_formula_moiety 'C23 H30 Cl3 N2 P Pt, 2(C H2 Cl2)'
_chemical_formula_sum 'C25 H34 Cl7 N2 P Pt'
_chemical_formula_weight 836.75
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M 'P 21 21 21'
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_Int_Tables_number 19
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 8.878(4)
_cell_length_b 15.409(6)
_cell_length_c 22.384(9)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3062(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 100
_cell_measurement_reflns_used 9600
_cell_measurement_theta_min 2.4739
_cell_measurement_theta_max 35.9443
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 -1.00 0.0750
-1.00 0.00 1.00 0.0750
0.00 1.00 0.00 0.0770
0.00 -1.00 0.00 0.0780
0.00 0.00 -1.00 0.0410
0.00 0.00 1.00 0.0080
_exptl_crystal_description plate
_exptl_crystal_colour yellow
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.815
_exptl_crystal_F_000 1640
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.05
_exptl_absorpt_coefficient_mu 5.265
_shelx_estimated_absorpt_T_min 0.428
_shelx_estimated_absorpt_T_max 0.669
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_correction_T_min 0.44340
_exptl_absorpt_correction_T_max 0.78215
_exptl_absorpt_process_details 'SADABS (Bruker AXS, 2012/1)'
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type Mo-K\a
_diffrn_source 1\mS
_diffrn_measurement_device_type 'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method 'CCD \f- and \w-scans'
_diffrn_detector_area_resol_mean 66.67
_diffrn_reflns_number 109357
_diffrn_reflns_av_unetI/netI 0.0521
_diffrn_reflns_av_R_equivalents 0.0883
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_l_min -37
_diffrn_reflns_limit_l_max 37
_diffrn_reflns_theta_min 2.249
_diffrn_reflns_theta_max 37.246
_diffrn_reflns_theta_full 25.242
_diffrn_radiation_monochromator 'Incoatec Helios mirrors'
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total 15230
_reflns_number_gt 14276
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.827
_reflns_Friedel_fraction_max 0.973
_reflns_Friedel_fraction_full 1.000
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'APEX2 (Bruker AXS, 2005-2013)'
_computing_cell_refinement 'SAINT software (Bruker AXS, 2004)'
_computing_data_reduction 'SAINT software (Bruker AXS, 2004)'
_computing_structure_solution 'SHELXs (G. M. Sheldrick, 2013)'
_computing_structure_refinement 'SHELXL (G. M. Sheldrick, 2014/7)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 1997-2012)'
_computing_publication_material ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The minimum and maximum estimated transmissions from the multi-scan
scaling are 0.4129 and 0.9153 (SADABS).
INTENSITY STATISTICS FOR DATASET
Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma
Inf - 2.68 127 128 99.2 12.04 114.8 37.24 0.0819 0.0251
2.68 - 1.69 302 302 100.0 16.02 90.7 44.21 0.0731 0.0234
1.69 - 1.32 433 433 100.0 17.53 55.0 43.57 0.0791 0.0218
1.32 - 1.14 439 439 100.0 17.38 36.6 39.65 0.0883 0.0226
1.14 - 1.03 429 429 100.0 17.12 32.0 37.38 0.0907 0.0240
1.03 - 0.96 394 394 100.0 15.85 27.5 34.08 0.0965 0.0263
0.96 - 0.90 423 423 100.0 15.65 21.8 30.88 0.1089 0.0288
0.90 - 0.85 456 456 100.0 14.76 17.9 26.41 0.1248 0.0333
0.85 - 0.81 430 430 100.0 14.27 15.3 23.96 0.1309 0.0369
0.81 - 0.78 411 411 100.0 13.72 14.0 21.82 0.1371 0.0404
0.78 - 0.75 456 456 100.0 13.15 12.8 19.91 0.1405 0.0439
0.75 - 0.72 554 554 100.0 12.64 11.6 17.86 0.1517 0.0489
0.72 - 0.70 393 393 100.0 12.38 10.4 16.12 0.1619 0.0541
0.70 - 0.68 446 446 100.0 11.75 9.2 14.47 0.1779 0.0605
0.68 - 0.67 265 265 100.0 11.81 8.3 13.23 0.1868 0.0666
0.67 - 0.65 544 544 100.0 11.09 7.7 12.10 0.1999 0.0745
0.65 - 0.64 300 301 99.7 10.75 6.7 10.27 0.2179 0.0869
0.64 - 0.62 659 659 100.0 10.49 6.3 9.69 0.2240 0.0927
0.62 - 0.61 359 365 98.4 9.98 5.3 8.19 0.2439 0.1124
0.61 - 0.60 373 377 98.9 6.66 4.9 6.02 0.2698 0.1670
0.60 - 0.59 280 528 53.0 1.29 4.6 3.29 0.2496 0.3253
#------------------------------------------------------------------------------
0.69 - 0.59 3008 3267 92.1 8.83 6.5 9.63 0.2120 0.1058
Inf - 0.59 8473 8733 97.0 12.55 20.5 21.91 0.1046 0.0374
Merged [A], lowest resolution = 22.42 Angstroms
#------------------------------------------------------------------------------
The crystal diffracted poorly at high angles, presumably due to loss of solute
from the crystal. The high second parameter in the WGHT card is a result of
downweighting the less-accurate high-angle reflections.
There is a high residual peak on each side of the Pt atom. We attribute it to
anharmonic displacement of the Pt atom. The peaks point along the c axis of the
unit cell and may be a result of partial loss of solute dichloromethane from
the crystal, extinction or an inadequate absorption correction due to difficulty
in determining the true thickness of the thin plate-like crystal.
Highest peak 11.26 at 0.1387 0.5599 0.2414 [ 0.71 A from PT1 ]
Deepest hole -9.45 at 0.1415 0.3306 0.2110 [ 1.77 A from H7B ]
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+125.8489P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens constr
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.080(18)
_chemical_absolute_configuration ad
_refine_ls_number_reflns 15230
_refine_ls_number_parameters 326
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0892
_refine_ls_R_factor_gt 0.0856
_refine_ls_wR_factor_ref 0.2478
_refine_ls_wR_factor_gt 0.2464
_refine_ls_goodness_of_fit_ref 1.151
_refine_ls_restrained_S_all 1.151
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0943(16) 0.7111(9) 0.2636(6) 0.015(2) Uani 1 1 d . . . . .
C2 C -0.1725(16) 0.5812(9) 0.3257(7) 0.017(2) Uani 1 1 d . . . . .
H2A H -0.2451 0.5418 0.3059 0.020 Uiso 1 1 calc R U . . .
H2B H -0.0697 0.5604 0.3163 0.020 Uiso 1 1 calc R U . . .
C3 C -0.196(2) 0.5775(11) 0.3911(7) 0.023(3) Uani 1 1 d . . . . .
H3A H -0.1126 0.6081 0.4115 0.027 Uiso 1 1 calc R U . . .
H3B H -0.1952 0.5162 0.4044 0.027 Uiso 1 1 calc R U . . .
C4 C -0.345(2) 0.6189(12) 0.4088(8) 0.025(3) Uani 1 1 d . . . . .
H4A H -0.4295 0.5854 0.3917 0.030 Uiso 1 1 calc R U . . .
H4B H -0.3551 0.6188 0.4529 0.030 Uiso 1 1 calc R U . . .
C5 C -0.349(2) 0.7106(10) 0.3859(7) 0.022(3) Uani 1 1 d . . . . .
H5A H -0.2649 0.7439 0.4039 0.027 Uiso 1 1 calc R U . . .
H5B H -0.4444 0.7383 0.3982 0.027 Uiso 1 1 calc R U . . .
C6 C -0.3355(17) 0.7139(11) 0.3178(7) 0.020(3) Uani 1 1 d . . . . .
H6A H -0.4210 0.6827 0.2993 0.024 Uiso 1 1 calc R U . . .
H6B H -0.3373 0.7749 0.3039 0.024 Uiso 1 1 calc R U . . .
C7 C -0.0882(15) 0.8515(9) 0.2069(8) 0.017(2) Uani 1 1 d . . . . .
H7A H 0.0122 0.8572 0.2258 0.020 Uiso 1 1 calc R U . . .
H7B H -0.1545 0.8967 0.2242 0.020 Uiso 1 1 calc R U . . .
C8 C -0.0735(19) 0.8663(10) 0.1404(7) 0.019(3) Uani 1 1 d . . . . .
H8A H 0.0058 0.8278 0.1242 0.023 Uiso 1 1 calc R U . . .
H8B H -0.0429 0.9271 0.1330 0.023 Uiso 1 1 calc R U . . .
C9 C -0.2229(19) 0.8480(11) 0.1083(8) 0.021(3) Uani 1 1 d . . . . .
H9A H -0.2084 0.8519 0.0645 0.026 Uiso 1 1 calc R U . . .
H9B H -0.2992 0.8916 0.1202 0.026 Uiso 1 1 calc R U . . .
C10 C -0.2776(17) 0.7561(11) 0.1253(8) 0.020(3) Uani 1 1 d . . . . .
H10A H -0.3752 0.7444 0.1054 0.024 Uiso 1 1 calc R U . . .
H10B H -0.2039 0.7127 0.1109 0.024 Uiso 1 1 calc R U . . .
C11 C -0.2962(17) 0.7472(10) 0.1916(7) 0.019(2) Uani 1 1 d . . . . .
H11A H -0.3732 0.7886 0.2061 0.023 Uiso 1 1 calc R U . . .
H11B H -0.3302 0.6877 0.2015 0.023 Uiso 1 1 calc R U . . .
C12 C 0.1451(19) 0.6704(11) 0.3445(6) 0.020(2) Uani 1 1 d . . . . .
C13 C 0.091(2) 0.7384(11) 0.3813(8) 0.022(3) Uani 1 1 d . . . . .
H13 H 0.0391 0.7867 0.3649 0.027 Uiso 1 1 calc R U . . .
C14 C 0.119(2) 0.7313(15) 0.4444(9) 0.031(4) Uani 1 1 d . . . . .
H14 H 0.0867 0.7762 0.4705 0.037 Uiso 1 1 calc R U . . .
C15 C 0.193(2) 0.6594(14) 0.4675(8) 0.030(4) Uani 1 1 d . . . . .
H15 H 0.2054 0.6544 0.5095 0.035 Uiso 1 1 calc R U . . .
C16 C 0.248(2) 0.5942(13) 0.4303(8) 0.026(3) Uani 1 1 d . . . . .
H16 H 0.3036 0.5470 0.4465 0.031 Uiso 1 1 calc R U . . .
C17 C 0.222(2) 0.5993(13) 0.3691(8) 0.025(3) Uani 1 1 d . . . . .
H17 H 0.2557 0.5540 0.3437 0.030 Uiso 1 1 calc R U . . .
C18 C 0.2236(16) 0.7638(9) 0.2358(7) 0.016(2) Uani 1 1 d . . . . .
C19 C 0.2846(16) 0.8262(9) 0.2737(8) 0.020(3) Uani 1 1 d . . . . .
H19 H 0.2669 0.8243 0.3156 0.024 Uiso 1 1 calc R U . . .
C20 C 0.3737(15) 0.8927(10) 0.2482(10) 0.027(4) Uani 1 1 d . . . . .
H20 H 0.4186 0.9352 0.2732 0.032 Uiso 1 1 calc R U . . .
C21 C 0.3959(18) 0.8961(10) 0.1873(10) 0.026(4) Uani 1 1 d . . . . .
H21 H 0.4532 0.9422 0.1706 0.031 Uiso 1 1 calc R U . . .
C22 C 0.3364(17) 0.8339(11) 0.1507(8) 0.023(3) Uani 1 1 d . . . . .
H22 H 0.3522 0.8374 0.1088 0.028 Uiso 1 1 calc R U . . .
C23 C 0.2519(19) 0.7647(11) 0.1744(7) 0.020(3) Uani 1 1 d . . . . .
H23 H 0.2150 0.7198 0.1492 0.024 Uiso 1 1 calc R U . . .
C24 C 0.431(3) 0.3934(17) 0.5438(9) 0.034(4) Uani 1 1 d . . . . .
H24A H 0.3322 0.4224 0.5378 0.041 Uiso 1 1 calc R U . . .
H24B H 0.4580 0.3990 0.5865 0.041 Uiso 1 1 calc R U . . .
C25 C 0.938(2) 0.4911(13) 0.5868(9) 0.028(3) Uani 1 1 d . . . . .
H25A H 0.8539 0.4594 0.6061 0.033 Uiso 1 1 calc R U . . .
H25B H 1.0203 0.4966 0.6163 0.033 Uiso 1 1 calc R U . . .
N1 N -0.1921(14) 0.6725(8) 0.3009(5) 0.015(2) Uani 1 1 d . . . . .
N2 N -0.1509(16) 0.7649(8) 0.2209(5) 0.018(2) Uani 1 1 d . . . . .
P1 P 0.1076(4) 0.6755(2) 0.26458(17) 0.0136(6) Uani 1 1 d . . . . .
Cl1 Cl -0.1048(4) 0.5432(2) 0.18272(17) 0.0195(6) Uani 1 1 d . . . . .
Cl2 Cl 0.2012(5) 0.4358(3) 0.14888(18) 0.0228(6) Uani 1 1 d . . . . .
Cl3 Cl 0.3972(4) 0.5707(3) 0.23298(19) 0.0222(7) Uani 1 1 d . . . . .
Cl4 Cl 0.5667(9) 0.4454(6) 0.5003(3) 0.0519(16) Uani 1 1 d . . . . .
Cl5 Cl 0.4131(9) 0.2828(4) 0.5256(2) 0.0430(14) Uani 1 1 d . . . . .
Cl6 Cl 1.0025(7) 0.4310(4) 0.5243(3) 0.0405(12) Uani 1 1 d . . . . .
Cl7 Cl 0.8755(7) 0.5954(3) 0.5660(2) 0.0347(10) Uani 1 1 d . . . . .
Pt1 Pt 0.14506(6) 0.55712(3) 0.20970(2) 0.01394(10) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.014(5) 0.016(5) 0.015(5) -0.004(4) 0.002(4) -0.007(4)
C2 0.014(6) 0.011(5) 0.024(6) -0.001(4) 0.002(4) 0.000(4)
C3 0.034(8) 0.016(6) 0.019(6) 0.000(5) 0.000(6) -0.006(5)
C4 0.021(7) 0.031(8) 0.022(6) -0.001(5) 0.010(6) -0.001(6)
C5 0.027(7) 0.017(6) 0.023(6) 0.000(5) 0.010(6) 0.003(6)
C6 0.013(6) 0.025(7) 0.022(6) -0.003(5) 0.003(5) -0.003(5)
C7 0.012(5) 0.014(5) 0.024(6) 0.001(5) 0.001(5) -0.002(4)
C8 0.023(7) 0.015(6) 0.020(6) 0.002(5) 0.001(5) 0.001(5)
C9 0.020(6) 0.016(6) 0.027(7) 0.006(5) 0.000(5) 0.000(5)
C10 0.013(5) 0.021(6) 0.026(7) 0.001(5) -0.003(5) 0.001(5)
C11 0.016(6) 0.017(6) 0.024(6) 0.002(5) 0.000(5) -0.001(5)
C12 0.012(5) 0.026(6) 0.021(6) -0.006(5) 0.002(5) -0.010(6)
C13 0.020(6) 0.018(6) 0.028(8) -0.006(5) 0.001(6) -0.001(5)
C14 0.027(9) 0.039(10) 0.026(8) -0.013(7) 0.000(6) -0.009(7)
C15 0.030(8) 0.037(10) 0.021(7) -0.002(6) -0.003(6) -0.014(7)
C16 0.022(7) 0.029(8) 0.027(8) 0.008(6) -0.003(6) 0.000(6)
C17 0.030(8) 0.028(8) 0.018(6) -0.002(6) -0.002(6) 0.000(6)
C18 0.012(5) 0.012(5) 0.023(6) 0.002(4) -0.002(4) 0.001(4)
C19 0.013(5) 0.009(5) 0.038(8) -0.001(5) 0.001(5) -0.004(4)
C20 0.005(5) 0.010(5) 0.065(12) -0.002(6) 0.003(6) 0.001(4)
C21 0.012(5) 0.012(5) 0.054(11) 0.008(6) 0.001(6) -0.002(4)
C22 0.014(6) 0.023(7) 0.033(8) 0.008(6) 0.010(5) 0.002(5)
C23 0.021(7) 0.020(6) 0.020(6) -0.001(5) 0.001(5) 0.002(5)
C24 0.029(9) 0.049(12) 0.024(8) -0.013(8) 0.001(7) 0.005(8)
C25 0.023(7) 0.026(8) 0.035(9) 0.000(7) 0.004(7) 0.002(6)
N1 0.014(4) 0.015(5) 0.016(5) -0.002(4) 0.002(3) -0.003(4)
N2 0.016(4) 0.016(4) 0.021(5) 0.000(4) -0.003(4) -0.002(4)
P1 0.0112(12) 0.0130(13) 0.0166(14) -0.0021(11) 0.0005(10) -0.0014(10)
Cl1 0.0147(12) 0.0210(16) 0.0228(14) -0.0041(11) -0.0004(10) -0.0042(11)
Cl2 0.0293(17) 0.0124(13) 0.0266(16) -0.0049(12) 0.0020(13) 0.0032(13)
Cl3 0.0167(13) 0.0202(17) 0.0298(17) -0.0054(12) -0.0042(12) 0.0067(11)
Cl4 0.058(4) 0.053(4) 0.045(3) 0.000(3) 0.014(3) -0.020(4)
Cl5 0.077(4) 0.024(2) 0.028(2) 0.0033(16) -0.015(2) 0.004(2)
Cl6 0.035(2) 0.035(3) 0.051(3) -0.015(2) 0.009(2) -0.001(2)
Cl7 0.037(3) 0.028(2) 0.040(2) -0.0024(17) 0.000(2) -0.0003(18)
Pt1 0.01444(16) 0.01043(15) 0.01694(17) -0.00016(16) -0.00047(17) -0.00041(16)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.343(18) . ?
C1 N2 1.36(2) . ?
C1 P1 1.875(15) . ?
C2 C3 1.48(2) . ?
C2 N1 1.52(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.52(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.50(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.53(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N1 1.47(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N2 1.479(18) . ?
C7 C8 1.51(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.53(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.54(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.50(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N2 1.47(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C17 1.40(3) . ?
C12 C13 1.41(2) . ?
C12 P1 1.822(15) . ?
C13 C14 1.44(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.39(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.40(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.39(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.39(2) . ?
C18 C23 1.40(2) . ?
C18 P1 1.823(15) . ?
C19 C20 1.41(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.38(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.37(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.41(2) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 Cl4 1.75(2) . ?
C24 Cl5 1.76(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 Cl7 1.76(2) . ?
C25 Cl6 1.77(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
P1 Pt1 2.224(4) . ?
Cl1 Pt1 2.309(4) . ?
Cl2 Pt1 2.366(4) . ?
Cl3 Pt1 2.308(4) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 117.8(13) . . ?
N1 C1 P1 118.8(12) . . ?
N2 C1 P1 122.6(11) . . ?
C3 C2 N1 112.3(12) . . ?
C3 C2 H2A 109.1 . . ?
N1 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
N1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
C2 C3 C4 111.4(15) . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C5 C4 C3 109.1(14) . . ?
C5 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C5 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
C4 C5 C6 111.7(13) . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
N1 C6 C5 108.0(14) . . ?
N1 C6 H6A 110.1 . . ?
C5 C6 H6A 110.1 . . ?
N1 C6 H6B 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
N2 C7 C8 112.1(12) . . ?
N2 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 C9 111.1(13) . . ?
C7 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C8 C9 C10 109.0(13) . . ?
C8 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
C8 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C11 C10 C9 111.2(14) . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N2 C11 C10 109.1(13) . . ?
N2 C11 H11A 109.9 . . ?
C10 C11 H11A 109.9 . . ?
N2 C11 H11B 109.9 . . ?
C10 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
C17 C12 C13 121.0(15) . . ?
C17 C12 P1 120.5(12) . . ?
C13 C12 P1 118.5(14) . . ?
C12 C13 C14 117.2(17) . . ?
C12 C13 H13 121.4 . . ?
C14 C13 H13 121.4 . . ?
C15 C14 C13 120.5(17) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 121.3(17) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C17 C16 C15 119.1(18) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C16 C17 C12 120.8(17) . . ?
C16 C17 H17 119.6 . . ?
C12 C17 H17 119.6 . . ?
C19 C18 C23 121.5(15) . . ?
C19 C18 P1 121.4(12) . . ?
C23 C18 P1 117.2(12) . . ?
C18 C19 C20 118.1(17) . . ?
C18 C19 H19 120.9 . . ?
C20 C19 H19 120.9 . . ?
C21 C20 C19 120.5(17) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C20 120.6(15) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 120.8(17) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C18 C23 C22 118.3(16) . . ?
C18 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
Cl4 C24 Cl5 112.2(11) . . ?
Cl4 C24 H24A 109.2 . . ?
Cl5 C24 H24A 109.2 . . ?
Cl4 C24 H24B 109.2 . . ?
Cl5 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
Cl7 C25 Cl6 111.7(12) . . ?
Cl7 C25 H25A 109.3 . . ?
Cl6 C25 H25A 109.3 . . ?
Cl7 C25 H25B 109.3 . . ?
Cl6 C25 H25B 109.3 . . ?
H25A C25 H25B 107.9 . . ?
C1 N1 C6 121.8(13) . . ?
C1 N1 C2 124.2(12) . . ?
C6 N1 C2 113.9(11) . . ?
C1 N2 C11 121.5(12) . . ?
C1 N2 C7 124.0(12) . . ?
C11 N2 C7 113.8(12) . . ?
C12 P1 C18 106.0(7) . . ?
C12 P1 C1 101.4(7) . . ?
C18 P1 C1 108.5(7) . . ?
C12 P1 Pt1 118.7(6) . . ?
C18 P1 Pt1 109.4(5) . . ?
C1 P1 Pt1 112.1(4) . . ?
P1 Pt1 Cl3 86.89(13) . . ?
P1 Pt1 Cl1 94.41(13) . . ?
Cl3 Pt1 Cl1 177.88(15) . . ?
P1 Pt1 Cl2 175.88(15) . . ?
Cl3 Pt1 Cl2 89.85(14) . . ?
Cl1 Pt1 Cl2 88.78(14) . . ?
_refine_diff_density_max 11.547
_refine_diff_density_min -9.938
_refine_diff_density_rms 0.483
_shelx_res_file
;
8888.res created by SHELXL-2014/7
TITL 8888 in P2(1)2(1)2(1)
CELL 0.71073 8.8778 15.4089 22.3839 90.000 90.000 90.000
ZERR 4.000 0.0036 0.0060 0.0090 0.000 0.000 0.000
LATT -1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC C H N P CL PT
UNIT 100 136 8 4 28 4
TEMP -173.000
SIZE 0.083 0.156 0.194
L.S. 10
BOND $H
SHEL 11.0 0.5
LIST 4
ACTA
TWIN
FMAP 2
PLAN 20
WGHT 0.075500 125.848930
BASF 0.08014
FVAR 0.06943
C1 1 -0.094308 0.711117 0.263632 11.00000 0.01364 0.01633 =
0.01524 -0.00378 0.00219 -0.00661
C2 1 -0.172479 0.581189 0.325689 11.00000 0.01441 0.01138 =
0.02412 -0.00092 0.00202 -0.00019
AFIX 23
H2A 2 -0.245051 0.541829 0.305852 11.00000 -1.20000
H2B 2 -0.069651 0.560366 0.316341 11.00000 -1.20000
AFIX 0
C3 1 -0.196196 0.577531 0.391138 11.00000 0.03388 0.01625 =
0.01862 -0.00036 0.00018 -0.00557
AFIX 23
H3A 2 -0.112619 0.608073 0.411517 11.00000 -1.20000
H3B 2 -0.195163 0.516233 0.404380 11.00000 -1.20000
AFIX 0
C4 1 -0.344722 0.618943 0.408827 11.00000 0.02118 0.03128 =
0.02191 -0.00073 0.01036 -0.00140
AFIX 23
H4A 2 -0.429474 0.585404 0.391704 11.00000 -1.20000
H4B 2 -0.355096 0.618827 0.452863 11.00000 -1.20000
AFIX 0
C5 1 -0.348766 0.710595 0.385866 11.00000 0.02719 0.01720 =
0.02294 0.00032 0.00999 0.00250
AFIX 23
H5A 2 -0.264892 0.743908 0.403856 11.00000 -1.20000
H5B 2 -0.444434 0.738300 0.398223 11.00000 -1.20000
AFIX 0
C6 1 -0.335512 0.713908 0.317849 11.00000 0.01304 0.02499 =
0.02217 -0.00327 0.00258 -0.00291
AFIX 23
H6A 2 -0.421018 0.682743 0.299254 11.00000 -1.20000
H6B 2 -0.337279 0.774893 0.303948 11.00000 -1.20000
AFIX 0
C7 1 -0.088194 0.851503 0.206939 11.00000 0.01229 0.01383 =
0.02361 0.00068 0.00054 -0.00222
AFIX 23
H7A 2 0.012221 0.857176 0.225774 11.00000 -1.20000
H7B 2 -0.154461 0.896719 0.224159 11.00000 -1.20000
AFIX 0
C8 1 -0.073533 0.866282 0.140430 11.00000 0.02286 0.01529 =
0.01997 0.00248 0.00060 0.00074
AFIX 23
H8A 2 0.005809 0.827785 0.124196 11.00000 -1.20000
H8B 2 -0.042851 0.927092 0.132966 11.00000 -1.20000
AFIX 0
C9 1 -0.222903 0.847979 0.108275 11.00000 0.02047 0.01614 =
0.02728 0.00597 -0.00038 -0.00005
AFIX 23
H9A 2 -0.208362 0.851872 0.064506 11.00000 -1.20000
H9B 2 -0.299174 0.891553 0.120161 11.00000 -1.20000
AFIX 0
C10 1 -0.277642 0.756130 0.125259 11.00000 0.01308 0.02104 =
0.02615 0.00125 -0.00314 0.00129
AFIX 23
H10A 2 -0.375174 0.744413 0.105391 11.00000 -1.20000
H10B 2 -0.203910 0.712680 0.110895 11.00000 -1.20000
AFIX 0
C11 1 -0.296198 0.747183 0.191634 11.00000 0.01602 0.01667 =
0.02363 0.00152 -0.00029 -0.00117
AFIX 23
H11A 2 -0.373212 0.788644 0.206075 11.00000 -1.20000
H11B 2 -0.330222 0.687707 0.201518 11.00000 -1.20000
AFIX 0
C12 1 0.145131 0.670445 0.344549 11.00000 0.01242 0.02568 =
0.02145 -0.00559 0.00246 -0.01008
C13 1 0.091323 0.738370 0.381258 11.00000 0.01970 0.01846 =
0.02823 -0.00650 0.00142 -0.00066
AFIX 43
H13 2 0.039069 0.786657 0.364923 11.00000 -1.20000
AFIX 0
C14 1 0.119052 0.731273 0.444414 11.00000 0.02747 0.03895 =
0.02620 -0.01318 -0.00001 -0.00871
AFIX 43
H14 2 0.086659 0.776206 0.470480 11.00000 -1.20000
AFIX 0
C15 1 0.192620 0.659420 0.467493 11.00000 0.03031 0.03703 =
0.02121 -0.00191 -0.00332 -0.01376
AFIX 43
H15 2 0.205436 0.654442 0.509489 11.00000 -1.20000
AFIX 0
C16 1 0.248290 0.594193 0.430279 11.00000 0.02178 0.02907 =
0.02696 0.00801 -0.00291 -0.00020
AFIX 43
H16 2 0.303624 0.546965 0.446486 11.00000 -1.20000
AFIX 0
C17 1 0.221635 0.599284 0.369122 11.00000 0.03014 0.02837 =
0.01751 -0.00188 -0.00157 0.00036
AFIX 43
H17 2 0.255693 0.553983 0.343699 11.00000 -1.20000
AFIX 0
C18 1 0.223644 0.763754 0.235841 11.00000 0.01223 0.01229 =
0.02289 0.00175 -0.00235 0.00119
C19 1 0.284631 0.826246 0.273733 11.00000 0.01287 0.00924 =
0.03754 -0.00126 0.00100 -0.00431
AFIX 43
H19 2 0.266886 0.824300 0.315565 11.00000 -1.20000
AFIX 0
C20 1 0.373678 0.892657 0.248206 11.00000 0.00520 0.01014 =
0.06514 -0.00176 0.00350 0.00140
AFIX 43
H20 2 0.418556 0.935221 0.273225 11.00000 -1.20000
AFIX 0
C21 1 0.395919 0.896146 0.187271 11.00000 0.01172 0.01179 =
0.05440 0.00751 0.00131 -0.00210
AFIX 43
H21 2 0.453157 0.942231 0.170555 11.00000 -1.20000
AFIX 0
C22 1 0.336385 0.833922 0.150702 11.00000 0.01356 0.02330 =
0.03312 0.00772 0.01026 0.00209
AFIX 43
H22 2 0.352247 0.837432 0.108800 11.00000 -1.20000
AFIX 0
C23 1 0.251898 0.764740 0.174375 11.00000 0.02110 0.01974 =
0.02020 -0.00093 0.00081 0.00249
AFIX 43
H23 2 0.214982 0.719839 0.149245 11.00000 -1.20000
AFIX 0
C24 1 0.430599 0.393403 0.543779 11.00000 0.02889 0.04866 =
0.02401 -0.01267 0.00121 0.00499
AFIX 23
H24A 2 0.332224 0.422406 0.537848 11.00000 -1.20000
H24B 2 0.457982 0.398961 0.586482 11.00000 -1.20000
AFIX 0
C25 1 0.937722 0.491109 0.586811 11.00000 0.02255 0.02558 =
0.03514 0.00014 0.00400 0.00235
AFIX 23
H25A 2 0.853897 0.459368 0.606135 11.00000 -1.20000
H25B 2 1.020343 0.496607 0.616273 11.00000 -1.20000
AFIX 0
N1 3 -0.192105 0.672476 0.300861 11.00000 0.01437 0.01534 =
0.01624 -0.00202 0.00228 -0.00319
N2 3 -0.150928 0.764931 0.220923 11.00000 0.01550 0.01596 =
0.02113 -0.00037 -0.00251 -0.00202
P1 4 0.107614 0.675490 0.264578 11.00000 0.01120 0.01298 =
0.01658 -0.00205 0.00047 -0.00141
CL1 5 -0.104806 0.543237 0.182716 11.00000 0.01471 0.02099 =
0.02285 -0.00413 -0.00035 -0.00415
CL2 5 0.201217 0.435754 0.148882 11.00000 0.02933 0.01241 =
0.02656 -0.00485 0.00196 0.00323
CL3 5 0.397238 0.570735 0.232985 11.00000 0.01669 0.02015 =
0.02985 -0.00536 -0.00419 0.00669
CL4 5 0.566705 0.445446 0.500305 11.00000 0.05791 0.05337 =
0.04453 0.00003 0.01377 -0.01973
CL5 5 0.413059 0.282811 0.525649 11.00000 0.07657 0.02418 =
0.02824 0.00329 -0.01455 0.00354
CL6 5 1.002469 0.430984 0.524253 11.00000 0.03543 0.03521 =
0.05096 -0.01457 0.00947 -0.00059
CL7 5 0.875491 0.595389 0.566015 11.00000 0.03669 0.02756 =
0.03985 -0.00240 -0.00045 -0.00033
PT1 6 0.145055 0.557121 0.209698 11.00000 0.01444 0.01043 =
0.01694 -0.00016 -0.00047 -0.00041
HKLF 4
REM 8888 in P2(1)2(1)2(1)
REM R1 = 0.0856 for 14276 Fo > 4sig(Fo) and 0.0892 for all 15230 data
REM 326 parameters refined using 0 restraints
END
WGHT 0.0752 126.7077
REM Highest difference peak 11.547, deepest hole -9.938, 1-sigma level 0.483
Q1 1 0.1382 0.5601 0.2410 11.00000 0.05 11.55
Q2 1 0.1422 0.5599 0.1774 11.00000 0.05 9.69
Q3 1 0.1321 0.5981 0.2099 11.00000 0.05 5.27
Q4 1 -0.1451 0.6238 0.2114 11.00000 0.05 4.93
Q5 1 -0.3999 0.5586 0.3607 11.00000 0.05 4.71
Q6 1 0.1428 0.7845 0.2099 11.00000 0.05 4.54
Q7 1 0.1423 0.7621 0.2890 11.00000 0.05 4.48
Q8 1 -0.1324 0.7941 0.2807 11.00000 0.05 4.45
Q9 1 0.3842 1.0601 0.2779 11.00000 0.05 3.95
Q10 1 0.0976 0.5587 0.3544 11.00000 0.05 3.88
Q11 1 0.4136 0.7933 0.2868 11.00000 0.05 3.34
Q12 1 0.4358 0.8287 0.1260 11.00000 0.05 3.11
Q13 1 -0.1476 0.7953 0.1363 11.00000 0.05 2.89
Q14 1 -0.4147 0.6001 0.2114 11.00000 0.05 2.56
Q15 1 -0.2756 0.5557 0.2086 11.00000 0.05 2.33
Q16 1 0.3805 0.5580 0.2626 11.00000 0.05 2.29
Q17 1 0.3507 0.4431 0.5462 11.00000 0.05 2.20
Q18 1 -0.4771 0.6766 0.2678 11.00000 0.05 2.16
Q19 1 -0.1083 0.5486 0.1518 11.00000 0.05 2.11
Q20 1 0.1467 0.6003 0.3692 11.00000 0.05 2.05
;
_shelx_res_checksum 32946
_iucr_refine_instructions_details
;
;
_exptl_special_details
;
Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_8909sadabs
_database_code_depnum_ccdc_archive 'CCDC 1407670'
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_audit_block_code GUN-GB-260-01
_audit_creation_date 2014-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_common ?
_chemical_name_systematic
;
Title
;
_chemical_formula_moiety 'C28 H45 N4 P, 2(F6 Sb)'
_chemical_formula_sum 'C28 H45 F12 N4 P Sb2'
_chemical_formula_weight 940.15
_chemical_compound_source dichloromethane
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_symmetry_cell_setting TRICLINIC
_symmetry_space_group_name_H-M 'p -1'
_symmetry_space_group_name_Hall '-p 1 (#2:1)'
_symmetry_Int_Tables_number 2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.2341(2)
_cell_length_b 11.9121(3)
_cell_length_c 14.5106(3)
_cell_angle_alpha 82.3872(10)
_cell_angle_beta 82.2212(9)
_cell_angle_gamma 87.2389(10)
_cell_volume 1736.43(7)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9983
_cell_measurement_temperature 100
_cell_measurement_theta_max 67.2688
_cell_measurement_theta_min 3.0990
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 13.602
_exptl_absorpt_correction_T_max 0.60027
_exptl_absorpt_correction_T_min 0.11584
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details 'SADABS (Bruker AXS, 2012)'
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.798
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2.00 0.00 -1.00 0.0200
-2.00 0.00 1.00 0.0200
0.00 2.00 1.00 0.1300
0.00 -2.00 -1.00 0.1300
1.00 0.00 2.00 0.0600
-1.00 0.00 -2.00 0.0600
_exptl_crystal_description plate
_exptl_crystal_F_000 932
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.04
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0676
_diffrn_reflns_av_unetI/netI 0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 41228
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 67.509
_diffrn_reflns_theta_min 3.099
_diffrn_radiation_monochromator 'MONTEL graded multilayer optic'
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type 'Bruker AXS X8 Proteum'
_diffrn_measurement_method 'CCD \f- and \w-scans'
_diffrn_radiation_type Cu-K\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source '0.2 x 2mm^2^ focus rotating anode'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5404
_reflns_number_total 6054
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT software (Bruker AXS, 2004)'
_computing_data_collection 'APEX2 (Bruker AXS, 2005-2013)'
_computing_data_reduction 'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 1997-2012)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL (G. M. Sheldrick, 2013)'
_computing_structure_solution 'SHELXS (G. M. Sheldrick, 2013)'
_refine_diff_density_max 0.661
_refine_diff_density_min -1.106
_refine_diff_density_rms 0.117
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.021
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 424
_refine_ls_number_reflns 6054
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0380
_refine_ls_R_factor_gt 0.0320
_refine_ls_restrained_S_all 1.021
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+3.1831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0778
_refine_ls_wR_factor_ref 0.0815
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The minimum and maximum estimated transmissions from the multi-scan
scaling are 0.1111 and 0.6481 (SADABS).
Highest peak ?
Deepest hole ?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,
H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9515(3) 0.2224(3) 0.7965(2) 0.0135(7) Uani 1 1 d . . . . .
C2 C 0.9095(3) 0.2200(3) 0.8924(2) 0.0170(7) Uani 1 1 d . . . . .
H2 H 0.8281 0.2558 0.9138 0.020 Uiso 1 1 calc R . . . .
C3 C 0.9880(4) 0.1648(3) 0.9562(2) 0.0204(8) Uani 1 1 d . . . . .
H3 H 0.9602 0.1636 1.0215 0.024 Uiso 1 1 calc R . . . .
C4 C 1.1067(4) 0.1114(3) 0.9258(3) 0.0204(8) Uani 1 1 d . . . . .
H4 H 1.1595 0.0738 0.9702 0.024 Uiso 1 1 calc R . . . .
C5 C 1.1482(3) 0.1127(3) 0.8307(3) 0.0187(7) Uani 1 1 d . . . . .
H5 H 1.2285 0.0748 0.8099 0.022 Uiso 1 1 calc R . . . .
C6 C 1.0720(3) 0.1698(3) 0.7659(2) 0.0164(7) Uani 1 1 d . . . . .
H6 H 1.1018 0.1731 0.7007 0.020 Uiso 1 1 calc R . . . .
C7 C 0.7842(3) 0.1890(3) 0.6516(2) 0.0146(7) Uani 1 1 d . . . . .
C8 C 0.7695(3) 0.0229(3) 0.7778(2) 0.0179(7) Uani 1 1 d . . . . .
H8A H 0.6840 -0.0147 0.7839 0.022 Uiso 1 1 calc R . . . .
H8B H 0.7593 0.0820 0.8205 0.022 Uiso 1 1 calc R . . . .
C9 C 0.8742(4) -0.0644(3) 0.8082(2) 0.0194(8) Uani 1 1 d . . . . .
H9A H 0.8391 -0.1090 0.8682 0.023 Uiso 1 1 calc R . . . .
H9B H 0.9525 -0.0247 0.8190 0.023 Uiso 1 1 calc R . . . .
C10 C 0.9156(4) -0.1445(3) 0.7349(3) 0.0245(8) Uani 1 1 d . . . . .
H10A H 0.9922 -0.1925 0.7527 0.029 Uiso 1 1 calc R . . . .
H10B H 0.8422 -0.1948 0.7326 0.029 Uiso 1 1 calc R . . . .
C11 C 0.9521(4) -0.0776(3) 0.6390(3) 0.0241(8) Uani 1 1 d . . . . .
H11A H 1.0280 -0.0297 0.6407 0.029 Uiso 1 1 calc R . . . .
H11B H 0.9785 -0.1304 0.5922 0.029 Uiso 1 1 calc R . . . .
C12 C 0.8361(4) -0.0032(3) 0.6107(2) 0.0206(8) Uani 1 1 d . . . . .
H12A H 0.8595 0.0384 0.5473 0.025 Uiso 1 1 calc R . . . .
H12B H 0.7596 -0.0505 0.6093 0.025 Uiso 1 1 calc R . . . .
C13 C 0.6335(4) 0.1590(3) 0.5379(3) 0.0230(8) Uani 1 1 d . . . . .
H13A H 0.5463 0.1986 0.5468 0.028 Uiso 1 1 calc R . . . .
H13B H 0.6262 0.0832 0.5752 0.028 Uiso 1 1 calc R . . . .
C14 C 0.6696(4) 0.1451(4) 0.4346(3) 0.0272(9) Uani 1 1 d . . . . .
H14A H 0.5971 0.1081 0.4126 0.033 Uiso 1 1 calc R . . . .
H14B H 0.7501 0.0960 0.4265 0.033 Uiso 1 1 calc R . . . .
C15 C 0.6939(4) 0.2601(4) 0.3761(3) 0.0282(9) Uani 1 1 d . . . . .
H15A H 0.7281 0.2489 0.3107 0.034 Uiso 1 1 calc R . . . .
H15B H 0.6094 0.3041 0.3753 0.034 Uiso 1 1 calc R . . . .
C16 C 0.7922(4) 0.3263(3) 0.4155(2) 0.0247(8) Uani 1 1 d . . . . .
H16A H 0.8003 0.4027 0.3792 0.030 Uiso 1 1 calc R . . . .
H16B H 0.8799 0.2872 0.4081 0.030 Uiso 1 1 calc R . . . .
C17 C 0.7508(4) 0.3381(3) 0.5190(2) 0.0236(8) Uani 1 1 d . . . . .
H17A H 0.8193 0.3780 0.5430 0.028 Uiso 1 1 calc R . . . .
H17B H 0.6672 0.3833 0.5264 0.028 Uiso 1 1 calc R . . . .
C18 C 0.7379(3) 0.3895(3) 0.7570(2) 0.0130(7) Uani 1 1 d . . . . .
C19 C 0.5437(3) 0.2697(3) 0.7686(3) 0.0186(7) Uani 1 1 d . . . . .
H19A H 0.6065 0.2083 0.7885 0.022 Uiso 1 1 calc R . . . .
H19B H 0.5156 0.2542 0.7089 0.022 Uiso 1 1 calc R . . . .
C20 C 0.4244(3) 0.2723(3) 0.8430(3) 0.0199(8) Uani 1 1 d . . . . .
H20A H 0.4534 0.2850 0.9031 0.024 Uiso 1 1 calc R . . . .
H20B H 0.3812 0.1983 0.8526 0.024 Uiso 1 1 calc R . . . .
C21 C 0.3258(3) 0.3662(3) 0.8141(2) 0.0194(8) Uani 1 1 d . . . . .
H21A H 0.2928 0.3517 0.7558 0.023 Uiso 1 1 calc R . . . .
H21B H 0.2496 0.3675 0.8639 0.023 Uiso 1 1 calc R . . . .
C22 C 0.3926(3) 0.4798(3) 0.7981(2) 0.0199(8) Uani 1 1 d . . . . .
H22A H 0.4140 0.4988 0.8586 0.024 Uiso 1 1 calc R . . . .
H22B H 0.3311 0.5396 0.7735 0.024 Uiso 1 1 calc R . . . .
C23 C 0.5190(3) 0.4777(3) 0.7290(2) 0.0186(7) Uani 1 1 d . . . . .
H23A H 0.4956 0.4739 0.6655 0.022 Uiso 1 1 calc R . . . .
H23B H 0.5656 0.5490 0.7270 0.022 Uiso 1 1 calc R . . . .
C24 C 0.7021(3) 0.5442(3) 0.8564(2) 0.0191(8) Uani 1 1 d . . . . .
H24A H 0.6165 0.5075 0.8772 0.023 Uiso 1 1 calc R . . . .
H24B H 0.6845 0.6216 0.8256 0.023 Uiso 1 1 calc R . . . .
C25 C 0.7740(4) 0.5505(3) 0.9408(2) 0.0211(8) Uani 1 1 d . . . . .
H25A H 0.7823 0.4736 0.9754 0.025 Uiso 1 1 calc R . . . .
H25B H 0.7211 0.5986 0.9836 0.025 Uiso 1 1 calc R . . . .
C26 C 0.9108(4) 0.5989(3) 0.9126(2) 0.0216(8) Uani 1 1 d . . . . .
H26A H 0.9029 0.6786 0.8837 0.026 Uiso 1 1 calc R . . . .
H26B H 0.9561 0.5976 0.9688 0.026 Uiso 1 1 calc R . . . .
C27 C 0.9912(3) 0.5291(3) 0.8430(2) 0.0199(8) Uani 1 1 d . . . . .
H27A H 1.0775 0.5642 0.8212 0.024 Uiso 1 1 calc R . . . .
H27B H 1.0078 0.4518 0.8744 0.024 Uiso 1 1 calc R . . . .
C28 C 0.9186(3) 0.5221(3) 0.7592(2) 0.0150(7) Uani 1 1 d . . . . .
H28A H 0.9119 0.5984 0.7234 0.018 Uiso 1 1 calc R . . . .
H28B H 0.9698 0.4719 0.7174 0.018 Uiso 1 1 calc R . . . .
N1 N 0.8020(3) 0.0777(2) 0.67982(19) 0.0143(6) Uani 1 1 d . . . . .
N2 N 0.7330(3) 0.2242(2) 0.5732(2) 0.0175(6) Uani 1 1 d . . . . .
N3 N 0.6093(3) 0.3799(2) 0.75415(19) 0.0142(6) Uani 1 1 d . . . . .
N4 N 0.7843(3) 0.4778(2) 0.78865(19) 0.0136(6) Uani 1 1 d . . . . .
P1 P 0.86638(8) 0.29495(7) 0.70356(6) 0.01299(18) Uani 1 1 d . . . . .
F7 F 0.5966(2) 0.82393(19) 0.91997(16) 0.0302(5) Uani 1 1 d . . . . .
F8 F 0.4052(3) 0.6779(2) 0.96946(17) 0.0418(6) Uani 1 1 d . . . . .
F9 F 0.4861(2) 0.7439(2) 0.79026(16) 0.0357(6) Uani 1 1 d . . . . .
F10 F 0.2499(2) 0.8092(2) 0.86629(18) 0.0412(6) Uani 1 1 d . . . . .
F11 F 0.4397(2) 0.9586(2) 0.8185(2) 0.0444(7) Uani 1 1 d . . . . .
F12 F 0.3588(3) 0.8900(3) 0.9987(2) 0.0497(7) Uani 1 1 d . . . . .
Sb2 Sb 0.42268(2) 0.81839(2) 0.89379(2) 0.02210(9) Uani 1 1 d . . . . .
F1 F 0.1712(2) 0.39469(19) 0.60784(16) 0.0298(5) Uani 1 1 d . . . . .
F2 F 0.4045(2) 0.39619(19) 0.50396(16) 0.0337(5) Uani 1 1 d . . . . .
F3 F 0.3170(2) 0.2058(2) 0.60188(18) 0.0388(6) Uani 1 1 d . . . . .
F4 F 0.3313(3) 0.2325(2) 0.4173(2) 0.0570(9) Uani 1 1 d . . . . .
F5 F 0.0964(2) 0.2304(2) 0.52314(16) 0.0353(6) Uani 1 1 d . . . . .
F6 F 0.1868(3) 0.4225(2) 0.42268(18) 0.0499(7) Uani 1 1 d . . . . .
Sb1 Sb 0.25070(2) 0.31362(2) 0.51205(2) 0.02173(9) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0138(16) 0.0121(15) 0.0147(17) -0.0037(14) -0.0004(13) -0.0012(13)
C2 0.0203(17) 0.0143(16) 0.0169(17) -0.0048(15) -0.0005(14) -0.0032(14)
C3 0.029(2) 0.0191(18) 0.0138(17) -0.0022(15) -0.0040(15) -0.0074(16)
C4 0.0224(18) 0.0194(18) 0.0207(18) 0.0004(16) -0.0096(15) -0.0045(15)
C5 0.0158(17) 0.0151(17) 0.0259(19) -0.0020(16) -0.0043(15) -0.0041(14)
C6 0.0164(17) 0.0157(16) 0.0169(17) -0.0033(15) 0.0010(14) -0.0036(14)
C7 0.0178(16) 0.0174(17) 0.0083(16) -0.0032(14) 0.0008(13) 0.0003(14)
C8 0.0194(17) 0.0195(17) 0.0140(17) 0.0013(15) -0.0007(14) -0.0043(15)
C9 0.0255(19) 0.0179(17) 0.0143(17) 0.0033(15) -0.0044(14) -0.0045(15)
C10 0.034(2) 0.0137(17) 0.025(2) 0.0011(16) -0.0064(17) 0.0027(16)
C11 0.038(2) 0.0167(18) 0.0190(19) -0.0086(16) -0.0029(16) 0.0027(17)
C12 0.035(2) 0.0151(17) 0.0136(17) -0.0058(15) -0.0053(15) 0.0006(16)
C13 0.0213(19) 0.029(2) 0.0209(19) -0.0051(17) -0.0086(15) -0.0020(16)
C14 0.028(2) 0.034(2) 0.023(2) -0.0100(18) -0.0107(16) -0.0025(18)
C15 0.033(2) 0.037(2) 0.0161(19) -0.0096(18) -0.0053(16) 0.0046(19)
C16 0.038(2) 0.0219(19) 0.0146(18) -0.0001(16) -0.0064(16) 0.0012(17)
C17 0.037(2) 0.0177(18) 0.0162(18) -0.0019(15) -0.0075(16) 0.0035(16)
C18 0.0169(17) 0.0137(16) 0.0078(15) 0.0001(14) -0.0007(13) 0.0003(14)
C19 0.0169(17) 0.0159(17) 0.0240(19) -0.0071(16) -0.0002(15) -0.0033(14)
C20 0.0194(18) 0.0212(18) 0.0184(18) -0.0026(16) 0.0010(15) -0.0039(15)
C21 0.0157(17) 0.0283(19) 0.0152(17) -0.0067(16) -0.0018(14) -0.0016(15)
C22 0.0193(18) 0.0242(19) 0.0168(18) -0.0050(16) -0.0031(15) 0.0032(15)
C23 0.0176(17) 0.0221(18) 0.0155(17) -0.0023(15) -0.0019(14) 0.0027(15)
C24 0.0203(18) 0.0211(18) 0.0180(18) -0.0128(16) -0.0007(14) 0.0011(15)
C25 0.030(2) 0.0226(19) 0.0119(17) -0.0071(15) -0.0005(15) -0.0040(16)
C26 0.032(2) 0.0195(18) 0.0158(18) -0.0054(16) -0.0087(15) -0.0038(16)
C27 0.0197(18) 0.0210(18) 0.0205(18) -0.0041(16) -0.0065(15) -0.0027(15)
C28 0.0161(17) 0.0162(16) 0.0126(16) -0.0021(14) 0.0010(13) -0.0063(14)
N1 0.0210(15) 0.0129(14) 0.0096(13) -0.0018(12) -0.0032(11) -0.0009(12)
N2 0.0218(15) 0.0182(15) 0.0137(14) -0.0062(13) -0.0035(12) 0.0007(12)
N3 0.0157(14) 0.0157(14) 0.0114(13) -0.0037(12) -0.0010(11) 0.0004(12)
N4 0.0159(14) 0.0144(14) 0.0114(13) -0.0059(12) -0.0010(11) -0.0013(12)
P1 0.0146(4) 0.0136(4) 0.0109(4) -0.0038(3) -0.0002(3) 0.0002(3)
F7 0.0273(12) 0.0323(12) 0.0307(12) 0.0015(10) -0.0055(10) -0.0058(10)
F8 0.0543(16) 0.0407(14) 0.0310(13) 0.0065(12) -0.0105(12) -0.0243(13)
F9 0.0341(13) 0.0481(15) 0.0260(12) -0.0127(11) -0.0046(10) 0.0129(11)
F10 0.0252(12) 0.0577(16) 0.0431(15) -0.0178(13) -0.0016(11) -0.0018(12)
F11 0.0333(13) 0.0332(13) 0.0618(18) 0.0068(13) -0.0037(12) 0.0063(11)
F12 0.0361(14) 0.0662(18) 0.0507(16) -0.0376(15) 0.0145(12) -0.0161(13)
Sb2 0.02106(14) 0.02471(14) 0.01978(14) -0.00494(11) 0.00245(10) -0.00184(10)
F1 0.0299(12) 0.0332(12) 0.0286(12) -0.0118(10) -0.0042(10) -0.0015(10)
F2 0.0363(13) 0.0309(12) 0.0320(13) -0.0014(11) 0.0036(10) -0.0124(11)
F3 0.0269(12) 0.0349(13) 0.0473(15) 0.0096(12) 0.0055(11) 0.0026(10)
F4 0.072(2) 0.0532(17) 0.0458(16) -0.0332(15) 0.0285(15) -0.0295(15)
F5 0.0363(13) 0.0429(14) 0.0291(12) -0.0100(11) -0.0020(10) -0.0156(11)
F6 0.073(2) 0.0467(16) 0.0341(14) 0.0064(13) -0.0278(14) -0.0150(15)
Sb1 0.02891(15) 0.02247(14) 0.01382(13) -0.00357(10) 0.00032(10) -0.00607(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.397(5) . ?
C1 C6 1.401(5) . ?
C1 P1 1.806(3) . ?
C2 C3 1.386(5) . ?
C3 C4 1.390(5) . ?
C4 C5 1.386(5) . ?
C5 C6 1.389(5) . ?
C7 N1 1.346(4) . ?
C7 N2 1.327(4) . ?
C7 P1 1.842(3) . ?
C8 C9 1.523(5) . ?
C8 N1 1.485(4) . ?
C9 C10 1.526(5) . ?
C10 C11 1.518(5) . ?
C11 C12 1.516(5) . ?
C12 N1 1.479(4) . ?
C13 C14 1.524(5) . ?
C13 N2 1.491(5) . ?
C14 C15 1.525(6) . ?
C15 C16 1.521(6) . ?
C16 C17 1.527(5) . ?
C17 N2 1.482(5) . ?
C18 N3 1.333(4) . ?
C18 N4 1.333(4) . ?
C18 P1 1.847(3) . ?
C19 C20 1.519(5) . ?
C19 N3 1.481(4) . ?
C20 C21 1.525(5) . ?
C21 C22 1.522(5) . ?
C22 C23 1.527(5) . ?
C23 N3 1.490(4) . ?
C24 C25 1.524(5) . ?
C24 N4 1.489(4) . ?
C25 C26 1.524(5) . ?
C26 C27 1.523(5) . ?
C27 C28 1.521(5) . ?
C28 N4 1.484(4) . ?
F7 Sb2 1.876(2) . ?
F8 Sb2 1.878(2) . ?
F9 Sb2 1.870(2) . ?
F10 Sb2 1.876(2) . ?
F11 Sb2 1.873(3) . ?
F12 Sb2 1.869(2) . ?
F1 Sb1 1.871(2) . ?
F2 Sb1 1.878(2) . ?
F3 Sb1 1.876(2) . ?
F4 Sb1 1.863(2) . ?
F5 Sb1 1.882(2) . ?
F6 Sb1 1.870(3) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 119.8(3) . . ?
C2 C1 P1 125.5(3) . . ?
C6 C1 P1 114.6(2) . . ?
C3 C2 C1 119.3(3) . . ?
C2 C3 C4 120.8(3) . . ?
C5 C4 C3 120.1(3) . . ?
C4 C5 C6 119.7(3) . . ?
C5 C6 C1 120.2(3) . . ?
N1 C7 P1 120.4(2) . . ?
N2 C7 N1 120.7(3) . . ?
N2 C7 P1 117.2(3) . . ?
N1 C8 C9 113.0(3) . . ?
C8 C9 C10 111.9(3) . . ?
C11 C10 C9 110.4(3) . . ?
C12 C11 C10 110.4(3) . . ?
N1 C12 C11 108.4(3) . . ?
N2 C13 C14 112.2(3) . . ?
C13 C14 C15 110.5(3) . . ?
C16 C15 C14 111.2(3) . . ?
C15 C16 C17 112.1(3) . . ?
N2 C17 C16 109.5(3) . . ?
N3 C18 N4 121.6(3) . . ?
N3 C18 P1 123.5(2) . . ?
N4 C18 P1 114.5(2) . . ?
N3 C19 C20 109.8(3) . . ?
C19 C20 C21 110.9(3) . . ?
C22 C21 C20 109.5(3) . . ?
C21 C22 C23 111.6(3) . . ?
N3 C23 C22 112.7(3) . . ?
N4 C24 C25 109.8(3) . . ?
C24 C25 C26 112.2(3) . . ?
C27 C26 C25 109.8(3) . . ?
C28 C27 C26 110.8(3) . . ?
N4 C28 C27 111.7(3) . . ?
C7 N1 C8 124.6(3) . . ?
C7 N1 C12 120.8(3) . . ?
C12 N1 C8 113.9(3) . . ?
C7 N2 C13 122.8(3) . . ?
C7 N2 C17 124.6(3) . . ?
C17 N2 C13 112.0(3) . . ?
C18 N3 C19 123.2(3) . . ?
C18 N3 C23 123.6(3) . . ?
C19 N3 C23 113.0(3) . . ?
C18 N4 C24 122.1(3) . . ?
C18 N4 C28 124.6(3) . . ?
C28 N4 C24 113.2(3) . . ?
C1 P1 C7 108.55(15) . . ?
C1 P1 C18 107.58(15) . . ?
C7 P1 C18 108.17(15) . . ?
F7 Sb2 F8 89.59(11) . . ?
F7 Sb2 F10 178.47(10) . . ?
F9 Sb2 F7 88.91(10) . . ?
F9 Sb2 F8 89.83(11) . . ?
F9 Sb2 F10 89.78(10) . . ?
F9 Sb2 F11 90.29(12) . . ?
F10 Sb2 F8 89.61(12) . . ?
F11 Sb2 F7 90.51(11) . . ?
F11 Sb2 F8 179.85(13) . . ?
F11 Sb2 F10 90.30(12) . . ?
F12 Sb2 F7 91.13(11) . . ?
F12 Sb2 F8 89.02(13) . . ?
F12 Sb2 F9 178.85(12) . . ?
F12 Sb2 F10 90.16(11) . . ?
F12 Sb2 F11 90.87(13) . . ?
F1 Sb1 F2 89.75(10) . . ?
F1 Sb1 F3 89.75(11) . . ?
F1 Sb1 F5 89.35(10) . . ?
F2 Sb1 F5 178.70(10) . . ?
F3 Sb1 F2 89.30(11) . . ?
F3 Sb1 F5 89.76(11) . . ?
F4 Sb1 F1 179.43(13) . . ?
F4 Sb1 F2 89.92(11) . . ?
F4 Sb1 F3 89.79(13) . . ?
F4 Sb1 F5 90.97(11) . . ?
F4 Sb1 F6 90.37(14) . . ?
F6 Sb1 F1 90.09(12) . . ?
F6 Sb1 F2 89.83(12) . . ?
F6 Sb1 F3 179.11(11) . . ?
F6 Sb1 F5 91.10(12) . . ?
_shelx_res_file
;
TITL 8909sadabs in P-1 #2
CELL 1.54178 10.2341 11.9121 14.5106 82.3872 82.2212 87.2389
ZERR 2 0.0002 0.0003 0.0003 0.001 0.0009 0.001
LATT 1
SFAC C H N F P Sb
UNIT 56 90 8 24 2 4
L.S. 8
PLAN 20
TEMP -173
REM reset to P-1 #2
BOND
fmap 2 53
acta
REM Z:/8909/mondal/8909sadabs.hkl
WGHT 0.035600 3.183100
FVAR 0.11076
C1 1 0.951460 0.222421 0.796509 11.00000 0.01382 0.01209 =
0.01472 -0.00369 -0.00039 -0.00115
C2 1 0.909505 0.219993 0.892449 11.00000 0.02034 0.01433 =
0.01686 -0.00485 -0.00049 -0.00316
AFIX 43
H2 2 0.828080 0.255760 0.913759 11.00000 -1.20000
AFIX 0
C3 1 0.987957 0.164837 0.956215 11.00000 0.02936 0.01910 =
0.01378 -0.00221 -0.00402 -0.00741
AFIX 43
H3 2 0.960239 0.163566 1.021520 11.00000 -1.20000
AFIX 0
C4 1 1.106702 0.111360 0.925754 11.00000 0.02243 0.01941 =
0.02073 0.00036 -0.00965 -0.00452
AFIX 43
H4 2 1.159482 0.073819 0.970210 11.00000 -1.20000
AFIX 0
C5 1 1.148241 0.112698 0.830682 11.00000 0.01577 0.01510 =
0.02593 -0.00205 -0.00429 -0.00414
AFIX 43
H5 2 1.228452 0.074777 0.809860 11.00000 -1.20000
AFIX 0
C6 1 1.072037 0.169759 0.765946 11.00000 0.01643 0.01572 =
0.01692 -0.00329 0.00100 -0.00359
AFIX 43
H6 2 1.101773 0.173083 0.700749 11.00000 -1.20000
AFIX 0
C7 1 0.784208 0.189037 0.651639 11.00000 0.01776 0.01744 =
0.00827 -0.00319 0.00082 0.00032
C8 1 0.769541 0.022888 0.777824 11.00000 0.01936 0.01951 =
0.01400 0.00126 -0.00069 -0.00432
AFIX 23
H8A 2 0.684040 -0.014673 0.783868 11.00000 -1.20000
H8B 2 0.759277 0.081970 0.820477 11.00000 -1.20000
AFIX 0
C9 1 0.874190 -0.064367 0.808195 11.00000 0.02551 0.01794 =
0.01427 0.00332 -0.00437 -0.00448
AFIX 23
H9A 2 0.839131 -0.109034 0.868156 11.00000 -1.20000
H9B 2 0.952491 -0.024681 0.818973 11.00000 -1.20000
AFIX 0
C10 1 0.915632 -0.144477 0.734912 11.00000 0.03438 0.01370 =
0.02471 0.00113 -0.00645 0.00273
AFIX 23
H10A 2 0.992239 -0.192458 0.752654 11.00000 -1.20000
H10B 2 0.842230 -0.194777 0.732577 11.00000 -1.20000
AFIX 0
C11 1 0.952071 -0.077563 0.639043 11.00000 0.03767 0.01670 =
0.01902 -0.00862 -0.00287 0.00265
AFIX 23
H11A 2 1.028001 -0.029741 0.640671 11.00000 -1.20000
H11B 2 0.978512 -0.130432 0.592152 11.00000 -1.20000
AFIX 0
C12 1 0.836062 -0.003234 0.610698 11.00000 0.03456 0.01515 =
0.01361 -0.00578 -0.00534 0.00062
AFIX 23
H12A 2 0.859530 0.038370 0.547315 11.00000 -1.20000
H12B 2 0.759582 -0.050499 0.609250 11.00000 -1.20000
AFIX 0
C13 1 0.633501 0.158977 0.537931 11.00000 0.02131 0.02920 =
0.02086 -0.00511 -0.00858 -0.00199
AFIX 23
H13A 2 0.546319 0.198619 0.546824 11.00000 -1.20000
H13B 2 0.626162 0.083154 0.575207 11.00000 -1.20000
AFIX 0
C14 1 0.669641 0.145092 0.434572 11.00000 0.02804 0.03438 =
0.02303 -0.01001 -0.01068 -0.00248
AFIX 23
H14A 2 0.597144 0.108067 0.412555 11.00000 -1.20000
H14B 2 0.750110 0.095950 0.426544 11.00000 -1.20000
AFIX 0
C15 1 0.693878 0.260086 0.376096 11.00000 0.03305 0.03705 =
0.01612 -0.00956 -0.00526 0.00459
AFIX 23
H15A 2 0.728107 0.248868 0.310702 11.00000 -1.20000
H15B 2 0.609417 0.304145 0.375311 11.00000 -1.20000
AFIX 0
C16 1 0.792236 0.326289 0.415505 11.00000 0.03761 0.02187 =
0.01458 -0.00009 -0.00645 0.00122
AFIX 23
H16A 2 0.800259 0.402668 0.379240 11.00000 -1.20000
H16B 2 0.879922 0.287243 0.408111 11.00000 -1.20000
AFIX 0
C17 1 0.750842 0.338092 0.518999 11.00000 0.03747 0.01768 =
0.01620 -0.00186 -0.00747 0.00353
AFIX 23
H17A 2 0.819335 0.377954 0.543001 11.00000 -1.20000
H17B 2 0.667232 0.383330 0.526376 11.00000 -1.20000
AFIX 0
C18 1 0.737884 0.389508 0.756952 11.00000 0.01690 0.01366 =
0.00783 0.00013 -0.00070 0.00029
C19 1 0.543730 0.269678 0.768558 11.00000 0.01686 0.01595 =
0.02396 -0.00712 -0.00025 -0.00327
AFIX 23
H19A 2 0.606456 0.208280 0.788548 11.00000 -1.20000
H19B 2 0.515606 0.254189 0.708939 11.00000 -1.20000
AFIX 0
C20 1 0.424410 0.272322 0.842979 11.00000 0.01937 0.02118 =
0.01843 -0.00261 0.00100 -0.00394
AFIX 23
H20A 2 0.453361 0.284950 0.903084 11.00000 -1.20000
H20B 2 0.381198 0.198335 0.852578 11.00000 -1.20000
AFIX 0
C21 1 0.325776 0.366199 0.814094 11.00000 0.01568 0.02829 =
0.01519 -0.00667 -0.00179 -0.00164
AFIX 23
H21A 2 0.292821 0.351699 0.755820 11.00000 -1.20000
H21B 2 0.249570 0.367526 0.863902 11.00000 -1.20000
AFIX 0
C22 1 0.392634 0.479824 0.798089 11.00000 0.01927 0.02418 =
0.01680 -0.00499 -0.00308 0.00319
AFIX 23
H22A 2 0.413974 0.498817 0.858635 11.00000 -1.20000
H22B 2 0.331109 0.539555 0.773531 11.00000 -1.20000
AFIX 0
C23 1 0.518964 0.477678 0.728956 11.00000 0.01760 0.02213 =
0.01553 -0.00233 -0.00190 0.00268
AFIX 23
H23A 2 0.495555 0.473901 0.665460 11.00000 -1.20000
H23B 2 0.565635 0.549008 0.727029 11.00000 -1.20000
AFIX 0
C24 1 0.702133 0.544167 0.856406 11.00000 0.02033 0.02109 =
0.01795 -0.01282 -0.00074 0.00110
AFIX 23
H24A 2 0.616496 0.507535 0.877245 11.00000 -1.20000
H24B 2 0.684471 0.621591 0.825558 11.00000 -1.20000
AFIX 0
C25 1 0.773975 0.550539 0.940850 11.00000 0.02978 0.02258 =
0.01186 -0.00711 -0.00051 -0.00400
AFIX 23
H25A 2 0.782334 0.473624 0.975368 11.00000 -1.20000
H25B 2 0.721053 0.598632 0.983624 11.00000 -1.20000
AFIX 0
C26 1 0.910811 0.598947 0.912561 11.00000 0.03218 0.01948 =
0.01575 -0.00544 -0.00875 -0.00385
AFIX 23
H26A 2 0.902864 0.678649 0.883669 11.00000 -1.20000
H26B 2 0.956129 0.597563 0.968825 11.00000 -1.20000
AFIX 0
C27 1 0.991180 0.529139 0.842981 11.00000 0.01973 0.02097 =
0.02053 -0.00408 -0.00649 -0.00274
AFIX 23
H27A 2 1.077484 0.564248 0.821156 11.00000 -1.20000
H27B 2 1.007830 0.451817 0.874418 11.00000 -1.20000
AFIX 0
C28 1 0.918626 0.522086 0.759234 11.00000 0.01615 0.01615 =
0.01256 -0.00211 0.00103 -0.00629
AFIX 23
H28A 2 0.911904 0.598416 0.723412 11.00000 -1.20000
H28B 2 0.969758 0.471910 0.717371 11.00000 -1.20000
AFIX 0
N1 3 0.801994 0.077746 0.679819 11.00000 0.02096 0.01292 =
0.00961 -0.00184 -0.00323 -0.00090
N2 3 0.732951 0.224157 0.573186 11.00000 0.02182 0.01824 =
0.01370 -0.00623 -0.00347 0.00073
N3 3 0.609285 0.379913 0.754151 11.00000 0.01570 0.01566 =
0.01144 -0.00372 -0.00097 0.00041
N4 3 0.784274 0.477780 0.788650 11.00000 0.01589 0.01442 =
0.01139 -0.00586 -0.00100 -0.00134
P1 5 0.866377 0.294950 0.703556 11.00000 0.01460 0.01361 =
0.01093 -0.00381 -0.00023 0.00015
F7 4 0.596636 0.823934 0.919965 11.00000 0.02726 0.03228 =
0.03066 0.00154 -0.00555 -0.00575
F8 4 0.405234 0.677927 0.969463 11.00000 0.05431 0.04069 =
0.03104 0.00652 -0.01050 -0.02435
F9 4 0.486131 0.743931 0.790263 11.00000 0.03405 0.04809 =
0.02601 -0.01272 -0.00457 0.01293
F10 4 0.249860 0.809188 0.866293 11.00000 0.02516 0.05768 =
0.04310 -0.01779 -0.00164 -0.00176
F11 4 0.439687 0.958649 0.818463 11.00000 0.03326 0.03320 =
0.06184 0.00680 -0.00366 0.00634
F12 4 0.358773 0.889965 0.998720 11.00000 0.03614 0.06621 =
0.05069 -0.03757 0.01445 -0.01611
SB2 6 0.422682 0.818390 0.893789 11.00000 0.02106 0.02471 =
0.01978 -0.00494 0.00245 -0.00184
F1 4 0.171195 0.394686 0.607842 11.00000 0.02995 0.03317 =
0.02858 -0.01183 -0.00424 -0.00149
F2 4 0.404549 0.396188 0.503962 11.00000 0.03627 0.03087 =
0.03204 -0.00142 0.00361 -0.01240
F3 4 0.316990 0.205787 0.601876 11.00000 0.02695 0.03487 =
0.04727 0.00956 0.00549 0.00261
F4 4 0.331272 0.232476 0.417329 11.00000 0.07195 0.05320 =
0.04580 -0.03322 0.02852 -0.02952
F5 4 0.096373 0.230408 0.523144 11.00000 0.03625 0.04288 =
0.02914 -0.00995 -0.00198 -0.01556
F6 4 0.186759 0.422548 0.422681 11.00000 0.07291 0.04675 =
0.03412 0.00643 -0.02777 -0.01501
SB1 6 0.250704 0.313620 0.512054 11.00000 0.02891 0.02247 =
0.01382 -0.00357 0.00032 -0.00607
HKLF 4
REM 8909sadabs in P-1 #2
REM R1 = 0.0320 for 5404 Fo > 4sig(Fo) and 0.0380 for all 6054 data
REM 424 parameters refined using 0 restraints
END
WGHT 0.0356 3.1755
REM Highest difference peak 0.661, deepest hole -1.106, 1-sigma level 0.117
Q1 1 0.2875 0.2581 0.4889 11.00000 0.05 0.66
Q2 1 0.1941 0.3232 0.4810 11.00000 0.05 0.63
Q3 1 0.3599 0.9050 0.8415 11.00000 0.05 0.54
Q4 1 0.1843 0.3193 0.5993 11.00000 0.05 0.52
Q5 1 0.2682 0.2655 0.3787 11.00000 0.05 0.50
Q6 1 0.0470 0.3408 0.5857 11.00000 0.05 0.50
Q7 1 0.1827 0.2210 0.5566 11.00000 0.05 0.50
Q8 1 0.4752 0.8062 0.8019 11.00000 0.05 0.47
Q9 1 0.3041 0.2028 0.5388 11.00000 0.05 0.45
Q10 1 0.1578 0.4755 0.5344 11.00000 0.05 0.45
Q11 1 0.6370 0.8065 0.8034 11.00000 0.05 0.44
Q12 1 0.2075 0.3927 0.5516 11.00000 0.05 0.44
Q13 1 1.0755 0.2792 0.6409 11.00000 0.05 0.41
Q14 1 0.3136 0.7556 0.9207 11.00000 0.05 0.40
Q15 1 0.9634 0.3369 0.4376 11.00000 0.05 0.40
Q16 1 0.9415 0.3724 0.6198 11.00000 0.05 0.39
Q17 1 0.3207 0.2801 0.5836 11.00000 0.05 0.39
Q18 1 0.3739 0.8277 1.0014 11.00000 0.05 0.39
Q19 1 0.3210 0.8129 0.9623 11.00000 0.05 0.38
Q20 1 0.4578 0.3068 0.4074 11.00000 0.05 0.38
;
_shelx_res_checksum 67517
_olex2_submission_special_instructions 'No special instructions were received'
_iucr_refine_instructions_details
;
;
_exptl_special_details
;
Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;
_shelxl_version_number 2014/6
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_9314sadabs
_database_code_depnum_ccdc_archive 'CCDC 1407671'
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_audit_block_code HAI-HA-246-01
_chemical_compound_source dichloromethane,pentane
_audit_creation_date 2015-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common ?
_chemical_name_systematic
;
Title
;
_chemical_formula_moiety 'F6 Sb, C17 H20 N2 P'
_chemical_formula_sum 'C17 H20 F6 N2 P Sb'
_chemical_formula_weight 519.07
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_symmetry_cell_setting MONOCLINIC
_symmetry_space_group_name_H-M 'p 21/c'
_symmetry_space_group_name_Hall '-p 2ybc (#14:b1)'
_symmetry_Int_Tables_number 14
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 7.5835(4)
_cell_length_b 11.1050(4)
_cell_length_c 23.5818(10)
_cell_angle_alpha 90
_cell_angle_beta 94.658(5)
_cell_angle_gamma 90
_cell_volume 1979.38(15)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 56706
_cell_measurement_temperature 100
_cell_measurement_theta_max 33.0987
_cell_measurement_theta_min 2.6926
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.533
_exptl_absorpt_correction_T_max 0.86809
_exptl_absorpt_correction_T_min 0.77720
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details 'SADABS (Bruker AXS, 2012)'
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.742
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.0420
0.00 0.00 1.00 0.0530
0.00 -1.00 0.00 0.0800
0.00 1.00 0.00 0.0880
-1.00 0.00 0.00 0.0800
1.00 0.00 0.00 0.1010
_exptl_crystal_description prism
_exptl_crystal_F_000 1024
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.09
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0210
_diffrn_reflns_av_unetI/netI 0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 36
_diffrn_reflns_limit_l_min -36
_diffrn_reflns_number 50691
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 33.140
_diffrn_reflns_theta_min 2.695
_diffrn_radiation_monochromator 'Incoatec Helios focusing multilayer optics'
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type 'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method 'CCD \f- and \w-scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source '0.2 x 2mm^2^ focus rotating anode'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6963
_reflns_number_total 7487
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'REVALCCD V. 1.6, 2008'
_computing_data_collection 'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction 'REVALCCD V. 1.6, 2008'
_computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 1997-2013)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL (Sheldrick, 2013)'
_computing_structure_solution 'SHELXS (Sheldrick, 2013)'
_refine_diff_density_max 1.900
_refine_diff_density_min -1.182
_refine_diff_density_rms 0.195
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.173
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 246
_refine_ls_number_reflns 7487
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0307
_refine_ls_R_factor_gt 0.0280
_refine_ls_restrained_S_all 1.173
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+1.8987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0945
_refine_ls_wR_factor_ref 0.0976
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The minimum and maximum estimated transmissions from the multi-scan
scaling are 0.7428 and 0.8842 (SADABS).
Highest peak ?
Deepest hole ?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C3(H3A,H3B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
C13(H13), C17(H17), C11(H11), C14(H14), C10(H10), C8(H8), C7(H7), C15(H15),
C16(H16), C9(H9)
2.c Idealised Me refined as rotating group:
C5(H5A,H5B,H5C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.29467(2) 0.55033(2) 0.15946(2) 0.01837(5) Uani 1 1 d . . . . .
P1 P 0.98829(6) -0.05246(4) 0.09015(2) 0.01491(8) Uani 1 1 d . . . . .
F1 F 0.3022(2) 0.38238(15) 0.16915(9) 0.0429(4) Uani 1 1 d . . . . .
F6 F 0.0519(2) 0.55095(12) 0.16942(8) 0.0348(3) Uani 1 1 d . . . . .
F5 F 0.53825(19) 0.55087(12) 0.15126(8) 0.0348(3) Uani 1 1 d . . . . .
N2 N 0.94073(18) -0.16649(13) 0.19878(6) 0.0158(2) Uani 1 1 d . . . . .
N1 N 1.1722(2) -0.04957(13) 0.19444(7) 0.0186(3) Uani 1 1 d . . . . .
C13 C 0.7434(2) 0.11793(15) 0.12847(7) 0.0173(3) Uani 1 1 d . . . . .
H13 H 0.6901 0.0539 0.1476 0.021 Uiso 1 1 calc R . . . .
C1 C 1.0259(2) -0.09268(14) 0.16652(7) 0.0141(2) Uani 1 1 d . . . . .
F2 F 0.2457(2) 0.53178(15) 0.08122(6) 0.0361(3) Uani 1 1 d . . . . .
C12 C 0.8898(2) 0.09557(14) 0.09764(6) 0.0144(2) Uani 1 1 d . . . . .
C6 C 0.8130(2) -0.15324(14) 0.06246(6) 0.0160(3) Uani 1 1 d . . . . .
F4 F 0.3403(3) 0.5701(2) 0.23811(7) 0.0609(6) Uani 1 1 d . . . . .
C5 C 0.7683(2) -0.22344(17) 0.18893(8) 0.0209(3) Uani 1 1 d . . . . .
H5A H 0.7027 -0.1859 0.1560 0.031 Uiso 1 1 calc GR . . . .
H5B H 0.7021 -0.2133 0.2226 0.031 Uiso 1 1 calc GR . . . .
H5C H 0.7838 -0.3095 0.1815 0.031 Uiso 1 1 calc GR . . . .
C17 C 0.9715(2) 0.19113(16) 0.07137(7) 0.0189(3) Uani 1 1 d . . . . .
H17 H 1.0721 0.1765 0.0509 0.023 Uiso 1 1 calc R . . . .
F3 F 0.28865(19) 0.71820(13) 0.15081(8) 0.0364(3) Uani 1 1 d . . . . .
C11 C 0.8638(2) -0.27327(15) 0.05507(7) 0.0192(3) Uani 1 1 d . . . . .
H11 H 0.9811 -0.2981 0.0667 0.023 Uiso 1 1 calc R . . . .
C14 C 0.6758(2) 0.23415(16) 0.13111(7) 0.0203(3) Uani 1 1 d . . . . .
H14 H 0.5739 0.2489 0.1510 0.024 Uiso 1 1 calc R . . . .
C10 C 0.7427(3) -0.35601(16) 0.03072(8) 0.0246(3) Uani 1 1 d . . . . .
H10 H 0.7771 -0.4375 0.0262 0.029 Uiso 1 1 calc R . . . .
C3 C 1.2023(2) -0.10330(19) 0.25126(8) 0.0231(3) Uani 1 1 d . . . . .
H3A H 1.2044 -0.0410 0.2813 0.028 Uiso 1 1 calc R . . . .
H3B H 1.3147 -0.1489 0.2552 0.028 Uiso 1 1 calc R . . . .
C8 C 0.5213(3) -0.20059(19) 0.01948(10) 0.0313(4) Uani 1 1 d . . . . .
H8 H 0.4044 -0.1761 0.0072 0.038 Uiso 1 1 calc R . . . .
C4 C 1.0429(2) -0.18713(16) 0.25402(7) 0.0194(3) Uani 1 1 d . . . . .
H4A H 1.0808 -0.2722 0.2581 0.023 Uiso 1 1 calc R . . . .
H4B H 0.9727 -0.1655 0.2861 0.023 Uiso 1 1 calc R . . . .
C7 C 0.6417(3) -0.11699(16) 0.04375(8) 0.0227(3) Uani 1 1 d . . . . .
H7 H 0.6074 -0.0353 0.0476 0.027 Uiso 1 1 calc R . . . .
C15 C 0.7575(3) 0.32913(16) 0.10452(8) 0.0215(3) Uani 1 1 d . . . . .
H15 H 0.7115 0.4084 0.1066 0.026 Uiso 1 1 calc R . . . .
C16 C 0.9055(3) 0.30786(16) 0.07519(8) 0.0224(3) Uani 1 1 d . . . . .
H16 H 0.9621 0.3728 0.0577 0.027 Uiso 1 1 calc R . . . .
C9 C 0.5720(3) -0.32019(18) 0.01310(10) 0.0310(4) Uani 1 1 d . . . . .
H9 H 0.4895 -0.3771 -0.0033 0.037 Uiso 1 1 calc R . . . .
C2 C 1.3070(3) 0.0244(2) 0.17138(11) 0.0322(4) Uani 1 1 d . . . . .
H2A H 1.3610 -0.0201 0.1413 0.048 Uiso 1 1 calc GR . . . .
H2B H 1.3981 0.0448 0.2017 0.048 Uiso 1 1 calc GR . . . .
H2C H 1.2531 0.0985 0.1555 0.048 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.01642(7) 0.01957(7) 0.01909(7) -0.00097(3) 0.00128(4) 0.00463(3)
P1 0.01591(17) 0.01418(18) 0.01477(17) -0.00100(12) 0.00198(13) 0.00046(12)
F1 0.0374(8) 0.0244(7) 0.0706(11) 0.0176(7) 0.0261(7) 0.0116(5)
F6 0.0204(6) 0.0316(7) 0.0542(10) 0.0078(6) 0.0140(6) 0.0064(4)
F5 0.0157(5) 0.0335(7) 0.0553(10) -0.0099(6) 0.0042(6) 0.0024(4)
N2 0.0146(5) 0.0181(6) 0.0144(5) 0.0003(4) -0.0011(4) -0.0004(4)
N1 0.0152(6) 0.0193(6) 0.0204(6) -0.0011(5) -0.0039(5) -0.0022(4)
C13 0.0172(6) 0.0171(6) 0.0180(6) -0.0021(5) 0.0039(5) -0.0007(5)
C1 0.0123(5) 0.0136(6) 0.0160(6) -0.0022(5) -0.0011(4) 0.0014(5)
F2 0.0430(8) 0.0442(8) 0.0204(6) -0.0091(5) -0.0024(5) -0.0026(6)
C12 0.0153(6) 0.0137(6) 0.0142(6) -0.0011(5) 0.0012(5) -0.0003(5)
C6 0.0208(6) 0.0140(6) 0.0128(6) -0.0006(5) -0.0015(5) 0.0005(5)
F4 0.0608(12) 0.1022(17) 0.0180(6) -0.0087(8) -0.0070(7) 0.0370(11)
C5 0.0174(7) 0.0248(8) 0.0205(7) 0.0008(6) 0.0006(5) -0.0059(6)
C17 0.0213(7) 0.0169(7) 0.0190(7) 0.0020(5) 0.0040(5) 0.0000(5)
F3 0.0326(7) 0.0165(6) 0.0610(10) -0.0067(6) 0.0096(6) 0.0023(4)
C11 0.0270(8) 0.0151(6) 0.0153(6) 0.0006(5) -0.0001(5) 0.0025(6)
C14 0.0214(7) 0.0208(7) 0.0189(7) -0.0045(6) 0.0020(5) 0.0045(6)
C10 0.0396(10) 0.0137(7) 0.0194(7) 0.0003(5) -0.0042(7) -0.0018(6)
C3 0.0195(7) 0.0292(9) 0.0195(7) -0.0019(6) -0.0055(6) -0.0005(6)
C8 0.0315(9) 0.0217(8) 0.0374(11) 0.0008(7) -0.0186(8) -0.0026(7)
C4 0.0206(7) 0.0222(7) 0.0150(6) 0.0000(5) -0.0018(5) 0.0031(6)
C7 0.0248(8) 0.0157(7) 0.0257(8) -0.0006(6) -0.0095(6) 0.0009(6)
C15 0.0281(8) 0.0163(7) 0.0193(7) -0.0029(5) -0.0022(6) 0.0045(6)
C16 0.0292(8) 0.0152(7) 0.0229(7) 0.0027(6) 0.0031(6) -0.0004(6)
C9 0.0412(11) 0.0192(8) 0.0295(9) 0.0006(7) -0.0152(8) -0.0074(7)
C2 0.0224(8) 0.0398(11) 0.0334(10) 0.0025(9) -0.0030(7) -0.0151(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F1 1.8793(16) . ?
Sb1 F6 1.8750(14) . ?
Sb1 F5 1.8729(14) . ?
Sb1 F2 1.8636(14) . ?
Sb1 F4 1.8718(16) . ?
Sb1 F3 1.8754(14) . ?
P1 C1 1.8551(16) . ?
P1 C12 1.8200(16) . ?
P1 C6 1.8178(17) . ?
N2 C1 1.322(2) . ?
N2 C5 1.454(2) . ?
N2 C4 1.479(2) . ?
N1 C1 1.332(2) . ?
N1 C3 1.468(2) . ?
N1 C2 1.452(3) . ?
C13 C12 1.398(2) . ?
C13 C14 1.392(2) . ?
C12 C17 1.398(2) . ?
C6 C11 1.402(2) . ?
C6 C7 1.397(2) . ?
C17 C16 1.395(2) . ?
C11 C10 1.390(3) . ?
C14 C15 1.398(3) . ?
C10 C9 1.385(3) . ?
C3 C4 1.531(3) . ?
C8 C7 1.392(3) . ?
C8 C9 1.394(3) . ?
C15 C16 1.386(3) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F6 Sb1 F1 90.51(6) . . ?
F6 Sb1 F3 89.69(6) . . ?
F5 Sb1 F1 89.72(6) . . ?
F5 Sb1 F6 178.68(7) . . ?
F5 Sb1 F3 90.06(6) . . ?
F2 Sb1 F1 90.71(8) . . ?
F2 Sb1 F6 90.33(8) . . ?
F2 Sb1 F5 90.97(8) . . ?
F2 Sb1 F4 179.08(7) . . ?
F2 Sb1 F3 90.06(8) . . ?
F4 Sb1 F1 89.70(10) . . ?
F4 Sb1 F6 88.85(9) . . ?
F4 Sb1 F5 89.86(9) . . ?
F4 Sb1 F3 89.54(10) . . ?
F3 Sb1 F1 179.21(9) . . ?
C12 P1 C1 98.93(7) . . ?
C6 P1 C1 104.52(7) . . ?
C6 P1 C12 107.28(7) . . ?
C1 N2 C5 130.75(14) . . ?
C1 N2 C4 110.94(13) . . ?
C5 N2 C4 118.27(14) . . ?
C1 N1 C3 111.51(15) . . ?
C1 N1 C2 127.02(17) . . ?
C2 N1 C3 120.67(16) . . ?
C14 C13 C12 119.93(16) . . ?
N2 C1 P1 131.62(12) . . ?
N2 C1 N1 111.38(14) . . ?
N1 C1 P1 116.71(12) . . ?
C13 C12 P1 124.08(12) . . ?
C13 C12 C17 119.64(15) . . ?
C17 C12 P1 116.26(12) . . ?
C11 C6 P1 115.45(13) . . ?
C7 C6 P1 124.76(13) . . ?
C7 C6 C11 119.49(15) . . ?
C16 C17 C12 120.18(16) . . ?
C10 C11 C6 120.06(17) . . ?
C13 C14 C15 120.08(16) . . ?
C9 C10 C11 120.27(17) . . ?
N1 C3 C4 102.78(13) . . ?
C7 C8 C9 120.15(19) . . ?
N2 C4 C3 103.14(14) . . ?
C8 C7 C6 119.98(17) . . ?
C16 C15 C14 120.15(16) . . ?
C15 C16 C17 119.98(17) . . ?
C10 C9 C8 120.03(18) . . ?
_shelx_res_file
;
9314sadabs.res created by SHELXL-2014/7
TITL 9314sadabs in P21/c #14
REM reset to P21/c #14
CELL 0.71073 7.5835 11.105 23.5818 90 94.658 90
ZERR 4 0.00035 0.00042 0.001 0 0.0045 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F N P Sb
UNIT 68 80 24 8 4 4
L.S. 10 0 0
PLAN 20
TEMP -173
BOND
fmap 2 53
acta
REM
REM
REM
WGHT 0.053200 1.898700
FVAR 0.17044
SB1 6 0.294672 0.550332 0.159463 11.00000 0.01642 0.01957 =
0.01909 -0.00097 0.00128 0.00463
P1 5 0.988285 -0.052457 0.090146 11.00000 0.01591 0.01418 =
0.01477 -0.00100 0.00198 0.00046
F1 3 0.302233 0.382383 0.169153 11.00000 0.03743 0.02437 =
0.07059 0.01762 0.02612 0.01159
F6 3 0.051882 0.550946 0.169424 11.00000 0.02039 0.03160 =
0.05420 0.00780 0.01398 0.00640
F5 3 0.538250 0.550873 0.151256 11.00000 0.01575 0.03353 =
0.05533 -0.00985 0.00417 0.00239
N2 4 0.940733 -0.166494 0.198778 11.00000 0.01463 0.01806 =
0.01438 0.00033 -0.00110 -0.00039
N1 4 1.172155 -0.049566 0.194440 11.00000 0.01521 0.01930 =
0.02036 -0.00111 -0.00389 -0.00220
C13 1 0.743381 0.117927 0.128471 11.00000 0.01723 0.01712 =
0.01797 -0.00209 0.00388 -0.00072
AFIX 43
H13 2 0.690079 0.053869 0.147599 11.00000 -1.20000
AFIX 0
C1 1 1.025889 -0.092683 0.166522 11.00000 0.01235 0.01357 =
0.01597 -0.00219 -0.00113 0.00140
F2 3 0.245716 0.531780 0.081224 11.00000 0.04300 0.04417 =
0.02040 -0.00910 -0.00244 -0.00255
C12 1 0.889810 0.095568 0.097641 11.00000 0.01529 0.01369 =
0.01419 -0.00112 0.00124 -0.00027
C6 1 0.813017 -0.153235 0.062459 11.00000 0.02076 0.01398 =
0.01278 -0.00064 -0.00152 0.00054
F4 3 0.340305 0.570138 0.238111 11.00000 0.06082 0.10223 =
0.01799 -0.00874 -0.00696 0.03699
C5 1 0.768288 -0.223437 0.188926 11.00000 0.01737 0.02484 =
0.02045 0.00076 0.00058 -0.00587
AFIX 137
H5A 2 0.702749 -0.185923 0.156011 11.00000 -1.50000
H5B 2 0.702149 -0.213297 0.222623 11.00000 -1.50000
H5C 2 0.783752 -0.309466 0.181506 11.00000 -1.50000
AFIX 0
C17 1 0.971451 0.191128 0.071367 11.00000 0.02129 0.01685 =
0.01903 0.00197 0.00399 0.00001
AFIX 43
H17 2 1.072082 0.176506 0.050861 11.00000 -1.20000
AFIX 0
F3 3 0.288652 0.718198 0.150812 11.00000 0.03264 0.01652 =
0.06103 -0.00666 0.00955 0.00227
C11 1 0.863777 -0.273271 0.055069 11.00000 0.02698 0.01509 =
0.01534 0.00056 -0.00014 0.00252
AFIX 43
H11 2 0.981055 -0.298060 0.066711 11.00000 -1.20000
AFIX 0
C14 1 0.675758 0.234146 0.131115 11.00000 0.02141 0.02077 =
0.01888 -0.00454 0.00196 0.00453
AFIX 43
H14 2 0.573925 0.248919 0.151020 11.00000 -1.20000
AFIX 0
C10 1 0.742659 -0.356014 0.030725 11.00000 0.03957 0.01371 =
0.01938 0.00027 -0.00417 -0.00179
AFIX 43
H10 2 0.777058 -0.437473 0.026159 11.00000 -1.20000
AFIX 0
C3 1 1.202253 -0.103303 0.251262 11.00000 0.01946 0.02915 =
0.01952 -0.00191 -0.00549 -0.00046
AFIX 23
H3A 2 1.204379 -0.040972 0.281324 11.00000 -1.20000
H3B 2 1.314726 -0.148944 0.255155 11.00000 -1.20000
AFIX 0
C8 1 0.521331 -0.200593 0.019479 11.00000 0.03146 0.02172 =
0.03737 0.00083 -0.01863 -0.00261
AFIX 43
H8 2 0.404369 -0.176097 0.007236 11.00000 -1.20000
AFIX 0
C4 1 1.042933 -0.187128 0.254019 11.00000 0.02057 0.02216 =
0.01499 -0.00004 -0.00176 0.00308
AFIX 23
H4A 2 1.080833 -0.272213 0.258087 11.00000 -1.20000
H4B 2 0.972730 -0.165538 0.286138 11.00000 -1.20000
AFIX 0
C7 1 0.641708 -0.116993 0.043748 11.00000 0.02478 0.01568 =
0.02573 -0.00061 -0.00954 0.00091
AFIX 43
H7 2 0.607362 -0.035319 0.047585 11.00000 -1.20000
AFIX 0
C15 1 0.757513 0.329128 0.104517 11.00000 0.02808 0.01632 =
0.01935 -0.00294 -0.00215 0.00447
AFIX 43
H15 2 0.711506 0.408441 0.106550 11.00000 -1.20000
AFIX 0
C16 1 0.905517 0.307864 0.075188 11.00000 0.02921 0.01516 =
0.02289 0.00273 0.00309 -0.00037
AFIX 43
H16 2 0.962075 0.372767 0.057687 11.00000 -1.20000
AFIX 0
C9 1 0.572042 -0.320191 0.013100 11.00000 0.04123 0.01920 =
0.02950 0.00055 -0.01524 -0.00738
AFIX 43
H9 2 0.489515 -0.377133 -0.003345 11.00000 -1.20000
AFIX 0
C2 1 1.307034 0.024414 0.171383 11.00000 0.02239 0.03980 =
0.03340 0.00245 -0.00301 -0.01513
AFIX 137
H2A 2 1.360967 -0.020106 0.141348 11.00000 -1.50000
H2B 2 1.398140 0.044761 0.201735 11.00000 -1.50000
H2C 2 1.253056 0.098530 0.155499 11.00000 -1.50000
AFIX 0
HKLF 4
REM 9314sadabs in P21/c #14
REM R1 = 0.0280 for 6963 Fo > 4sig(Fo) and 0.0307 for all 7487 data
REM 246 parameters refined using 0 restraints
END
WGHT 0.0532 1.8987
REM Highest difference peak 1.900, deepest hole -1.182, 1-sigma level 0.195
Q1 1 0.2937 0.5432 0.1993 11.00000 0.05 1.90
Q2 1 1.1358 -0.0530 0.0601 11.00000 0.05 1.75
Q3 1 0.3553 0.4209 0.1966 11.00000 0.05 0.82
Q4 1 0.5141 0.5873 0.1171 11.00000 0.05 0.78
Q5 1 0.8037 -0.3200 0.0402 11.00000 0.05 0.75
Q6 1 0.9965 -0.0789 0.1440 11.00000 0.05 0.65
Q7 1 0.8198 0.1055 0.1165 11.00000 0.05 0.63
Q8 1 0.6670 -0.3366 0.0199 11.00000 0.05 0.61
Q9 1 0.8325 -0.2159 0.0594 11.00000 0.05 0.61
Q10 1 0.9746 -0.1366 0.1826 11.00000 0.05 0.60
Q11 1 1.2921 0.0373 0.1397 11.00000 0.05 0.58
Q12 1 1.0987 -0.0647 0.1809 11.00000 0.05 0.58
Q13 1 1.3202 0.0733 0.1776 11.00000 0.05 0.55
Q14 1 0.3018 0.7066 0.1172 11.00000 0.05 0.52
Q15 1 0.8656 -0.1152 0.0798 11.00000 0.05 0.52
Q16 1 0.7419 -0.1325 0.0583 11.00000 0.05 0.52
Q17 1 0.7242 -0.1916 0.1812 11.00000 0.05 0.52
Q18 1 0.6391 -0.0651 0.1628 11.00000 0.05 0.51
Q19 1 0.1013 0.5589 0.2003 11.00000 0.05 0.51
Q20 1 0.7141 0.1722 0.1346 11.00000 0.05 0.51
;
_shelx_res_checksum 42001
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_iucr_refine_instructions_details
;
9314sadabs.res created by SHELXL-2014/7
TITL 9314sadabs in P21/c #14
REM reset to P21/c #14
CELL 0.71073 7.5835 11.105 23.5818 90 94.658 90
ZERR 4 0.00035 0.00042 0.001 0 0.0045 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F N P Sb
UNIT 68 80 24 8 4 4
L.S. 10 0 0
PLAN 20
TEMP -173
BOND
fmap 2 53
acta
REM
REM
REM
WGHT 0.053200 1.898700
FVAR 0.17044
SB1 6 0.294672 0.550332 0.159463 11.00000 0.01642 0.01957 =
0.01909 -0.00097 0.00128 0.00463
P1 5 0.988285 -0.052457 0.090146 11.00000 0.01591 0.01418 =
0.01477 -0.00100 0.00198 0.00046
F1 3 0.302233 0.382383 0.169153 11.00000 0.03743 0.02437 =
0.07059 0.01762 0.02612 0.01159
F6 3 0.051882 0.550946 0.169424 11.00000 0.02039 0.03160 =
0.05420 0.00780 0.01398 0.00640
F5 3 0.538250 0.550873 0.151256 11.00000 0.01575 0.03353 =
0.05533 -0.00985 0.00417 0.00239
N2 4 0.940733 -0.166494 0.198778 11.00000 0.01463 0.01806 =
0.01438 0.00033 -0.00110 -0.00039
N1 4 1.172155 -0.049566 0.194440 11.00000 0.01521 0.01930 =
0.02036 -0.00111 -0.00389 -0.00220
C13 1 0.743381 0.117927 0.128471 11.00000 0.01723 0.01712 =
0.01797 -0.00209 0.00388 -0.00072
AFIX 43
H13 2 0.690079 0.053869 0.147599 11.00000 -1.20000
AFIX 0
C1 1 1.025889 -0.092683 0.166522 11.00000 0.01235 0.01357 =
0.01597 -0.00219 -0.00113 0.00140
F2 3 0.245716 0.531780 0.081224 11.00000 0.04300 0.04417 =
0.02040 -0.00910 -0.00244 -0.00255
C12 1 0.889810 0.095568 0.097641 11.00000 0.01529 0.01369 =
0.01419 -0.00112 0.00124 -0.00027
C6 1 0.813017 -0.153235 0.062459 11.00000 0.02076 0.01398 =
0.01278 -0.00064 -0.00152 0.00054
F4 3 0.340305 0.570138 0.238111 11.00000 0.06082 0.10223 =
0.01799 -0.00874 -0.00696 0.03699
C5 1 0.768288 -0.223437 0.188926 11.00000 0.01737 0.02484 =
0.02045 0.00076 0.00058 -0.00587
AFIX 137
H5A 2 0.702749 -0.185923 0.156011 11.00000 -1.50000
H5B 2 0.702149 -0.213297 0.222623 11.00000 -1.50000
H5C 2 0.783752 -0.309466 0.181506 11.00000 -1.50000
AFIX 0
C17 1 0.971451 0.191128 0.071367 11.00000 0.02129 0.01685 =
0.01903 0.00197 0.00399 0.00001
AFIX 43
H17 2 1.072082 0.176506 0.050861 11.00000 -1.20000
AFIX 0
F3 3 0.288652 0.718198 0.150812 11.00000 0.03264 0.01652 =
0.06103 -0.00666 0.00955 0.00227
C11 1 0.863777 -0.273271 0.055069 11.00000 0.02698 0.01509 =
0.01534 0.00056 -0.00014 0.00252
AFIX 43
H11 2 0.981055 -0.298060 0.066711 11.00000 -1.20000
AFIX 0
C14 1 0.675758 0.234146 0.131115 11.00000 0.02141 0.02077 =
0.01888 -0.00454 0.00196 0.00453
AFIX 43
H14 2 0.573925 0.248919 0.151020 11.00000 -1.20000
AFIX 0
C10 1 0.742659 -0.356014 0.030725 11.00000 0.03957 0.01371 =
0.01938 0.00027 -0.00417 -0.00179
AFIX 43
H10 2 0.777058 -0.437473 0.026159 11.00000 -1.20000
AFIX 0
C3 1 1.202253 -0.103303 0.251262 11.00000 0.01946 0.02915 =
0.01952 -0.00191 -0.00549 -0.00046
AFIX 23
H3A 2 1.204379 -0.040972 0.281324 11.00000 -1.20000
H3B 2 1.314726 -0.148944 0.255155 11.00000 -1.20000
AFIX 0
C8 1 0.521331 -0.200593 0.019479 11.00000 0.03146 0.02172 =
0.03737 0.00083 -0.01863 -0.00261
AFIX 43
H8 2 0.404369 -0.176097 0.007236 11.00000 -1.20000
AFIX 0
C4 1 1.042933 -0.187128 0.254019 11.00000 0.02057 0.02216 =
0.01499 -0.00004 -0.00176 0.00308
AFIX 23
H4A 2 1.080833 -0.272213 0.258087 11.00000 -1.20000
H4B 2 0.972730 -0.165538 0.286138 11.00000 -1.20000
AFIX 0
C7 1 0.641708 -0.116993 0.043748 11.00000 0.02478 0.01568 =
0.02573 -0.00061 -0.00954 0.00091
AFIX 43
H7 2 0.607362 -0.035319 0.047585 11.00000 -1.20000
AFIX 0
C15 1 0.757513 0.329128 0.104517 11.00000 0.02808 0.01632 =
0.01935 -0.00294 -0.00215 0.00447
AFIX 43
H15 2 0.711506 0.408441 0.106550 11.00000 -1.20000
AFIX 0
C16 1 0.905517 0.307864 0.075188 11.00000 0.02921 0.01516 =
0.02289 0.00273 0.00309 -0.00037
AFIX 43
H16 2 0.962075 0.372767 0.057687 11.00000 -1.20000
AFIX 0
C9 1 0.572042 -0.320191 0.013100 11.00000 0.04123 0.01920 =
0.02950 0.00055 -0.01524 -0.00738
AFIX 43
H9 2 0.489515 -0.377133 -0.003345 11.00000 -1.20000
AFIX 0
C2 1 1.307034 0.024414 0.171383 11.00000 0.02239 0.03980 =
0.03340 0.00245 -0.00301 -0.01513
AFIX 137
H2A 2 1.360967 -0.020106 0.141348 11.00000 -1.50000
H2B 2 1.398140 0.044761 0.201735 11.00000 -1.50000
H2C 2 1.253056 0.098530 0.155499 11.00000 -1.50000
AFIX 0
HKLF 4
REM 9314sadabs in P21/c #14
REM R1 = 0.0280 for 6963 Fo > 4sig(Fo) and 0.0307 for all 7487 data
REM 246 parameters refined using 0 restraints
END
WGHT 0.0532 1.8987
REM Highest difference peak 1.900, deepest hole -1.182, 1-sigma level 0.195
Q1 1 0.2937 0.5432 0.1993 11.00000 0.05 1.90
Q2 1 1.1358 -0.0530 0.0601 11.00000 0.05 1.75
Q3 1 0.3553 0.4209 0.1966 11.00000 0.05 0.82
Q4 1 0.5141 0.5873 0.1171 11.00000 0.05 0.78
Q5 1 0.8037 -0.3200 0.0402 11.00000 0.05 0.75
Q6 1 0.9965 -0.0789 0.1440 11.00000 0.05 0.65
Q7 1 0.8198 0.1055 0.1165 11.00000 0.05 0.63
Q8 1 0.6670 -0.3366 0.0199 11.00000 0.05 0.61
Q9 1 0.8325 -0.2159 0.0594 11.00000 0.05 0.61
Q10 1 0.9746 -0.1366 0.1826 11.00000 0.05 0.60
Q11 1 1.2921 0.0373 0.1397 11.00000 0.05 0.58
Q12 1 1.0987 -0.0647 0.1809 11.00000 0.05 0.58
Q13 1 1.3202 0.0733 0.1776 11.00000 0.05 0.55
Q14 1 0.3018 0.7066 0.1172 11.00000 0.05 0.52
Q15 1 0.8656 -0.1152 0.0798 11.00000 0.05 0.52
Q16 1 0.7419 -0.1325 0.0583 11.00000 0.05 0.52
Q17 1 0.7242 -0.1916 0.1812 11.00000 0.05 0.52
Q18 1 0.6391 -0.0651 0.1628 11.00000 0.05 0.51
Q19 1 0.1013 0.5589 0.2003 11.00000 0.05 0.51
Q20 1 0.7141 0.1722 0.1346 11.00000 0.05 0.51
REM The information below was added by Olex2.
REM
REM R1 = 0.0280 for 6963 Fo > 4sig(Fo) and 0.0307 for all 51919 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.90, deepest hole -1.18
REM Mean Shift 0, Max Shift 0.003.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0307
REM R1_gt = 0.0280
REM wR_ref = 0.0976
REM GOOF = 1.173
REM Shift_max = 0.003
REM Shift_mean = 0
REM Reflections_all = 51919
REM Reflections_gt = 6963
REM Parameters = n/a
REM Hole = -1.18
REM Peak = 1.90
REM Flack = n/a
;
_exptl_special_details
;
Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;
_chemical_absolute_configuration rmad