data_ps302b loop_ _publ_author_name _publ_author_address 'Samuel, P. P.' ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstr. 4, 37077 G\"ottingen (Germany) ; 'Yan Li' ; State Key Laboratory of Physical Chemistry of Solid Surfaces College of Chemistry and Chemical Engineering Xiamen University Xiamen, Fujian, 361005, China ; 'Roesky, H. W.' ; Institut f\"r Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammanstr. 4, 37077 G\"ottingen (Germany) ; 'Veniamin Chevelkov' ; Division of Solid-State NMR spectroscopy, Max Planck Institute for Biophysical Chemistry , Am Fassberg 11, D-37077, G\"ottingen, (Germany) ; 'Adam Lange' ; Division of Solid-State NMR spectroscopy, Max Planck Institute for Biophysical Chemistry , Am Fassberg 11, D-37077, G\"ottingen, (Germany) ; 'Burkhardt, A.' ; Deutsches Electronen-Synchrotron Notkestr. 85, 22607 Hamburg (Germany) ; 'Dittrich, B.' ; nstitut f\"ur Anorganische und Angewandte Chemie, Universit\"at Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg, (Germany) ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H25 N2, 0.5(F6 Sn2)' _chemical_formula_sum 'C15 H25 F3 N2 Sn' _chemical_formula_weight 408.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0034 0.0017 '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' 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0180 0.0106 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6324 1.4479 '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 21/c' _space_group_name_Hall '-P 2ybc' _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, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _cell_length_a 9.573(5) _cell_length_b 17.473(4) _cell_length_c 11.177(12) _cell_angle_alpha 90 _cell_angle_beta 105.99(5) _cell_angle_gamma 90 _cell_volume 1797(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8322 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 21.7 #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'XDS (Kabsch, 2010)' _computing_cell_refinement 'XDS (Kabsch, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_publication_material 'enCIFer 1.4, CCDC, 2011' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Shelxle (Huebschle, 2013)' #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_F_000 824 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6320 _exptl_absorpt_correction_T_max 0.7447 _exptl_absorpt_process_details ; SADABS version 2008/2, multi-scan. (G. M. Sheldrick, 2008) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6199 _diffrn_radiation_type 'synchrotron' _diffrn_source 'monochromated X-rays on beamline P11' _diffrn_measurement_method '\f scans' _diffrn_measurement_device_type 'Microdiffractometer at P11 (PetraIII)' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9783 _diffrn_reflns_av_unetI/netI 0.0497 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.930 _diffrn_reflns_theta_max 21.793 _diffrn_reflns_theta_full 21.835 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_point_group_measured_fraction_full 0.983 _reflns_number_total 3192 _reflns_number_gt 2973 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The data were measured at the PetraIII synchrotron, beamline P11 at DESY in Hamburg, Germany. A photon energy of 20keV, corresponding to a wavelength of 0.6199 Angstroem, was used. ; _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^)+(0.0332P)^2^+1.5365P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0318(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3192 _refine_ls_number_parameters 251 _refine_ls_number_restraints 106 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.007 _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 Sn1A Sn 0.4569(7) 0.5048(4) 0.3573(14) 0.076(2) Uani 0.293(15) 1 d . U P A 1 Sn2A Sn 0.4557(2) 0.50801(9) 0.3291(4) 0.0378(8) Uani 0.494(16) 1 d . U P A 2 Sn3A Sn 0.4706(12) 0.5083(5) 0.2984(16) 0.0678(19) Uani 0.209(14) 1 d . U P A 3 F1 F 0.40067(19) 0.39660(10) 0.32931(17) 0.0512(5) Uani 1 1 d . U . . . F2 F 0.2486(2) 0.52218(12) 0.2205(2) 0.0658(6) Uani 1 1 d . U . . . F3 F 0.3707(3) 0.52961(15) 0.4744(3) 0.0874(9) Uani 1 1 d . U . . . N1 N 0.1884(2) 0.33004(13) 0.13907(18) 0.0309(5) Uani 1 1 d . U . . . H1 H 0.2536 0.3561 0.1951 0.042(8) Uiso 1 1 calc R . . . . N2 N 0.0333(2) 0.41833(14) 0.17681(19) 0.0348(5) Uani 1 1 d . U . . . H2 H 0.1101 0.4483 0.1926 0.040(8) Uiso 1 1 calc R . . . . C1 C 0.0531(3) 0.35189(15) 0.1280(2) 0.0283(5) Uani 1 1 d . U . . . C2 C -0.0722(3) 0.30368(15) 0.0625(2) 0.0295(5) Uani 1 1 d . U . . . C3 C -0.0985(3) 0.23492(16) 0.1135(3) 0.0367(6) Uani 1 1 d . U . . . H3 H -0.0346 0.2181 0.1900 0.044 Uiso 1 1 calc R U . . . C4 C -0.2170(3) 0.19032(18) 0.0544(3) 0.0436(7) Uani 1 1 d . U . . . H4 H -0.2348 0.1433 0.0902 0.052 Uiso 1 1 calc R U . . . C5 C -0.3094(3) 0.21490(19) -0.0572(3) 0.0451(7) Uani 1 1 d . U . . . H5 H -0.3909 0.1846 -0.0982 0.054 Uiso 1 1 calc R U . . . C6 C -0.2835(3) 0.28330(19) -0.1091(3) 0.0431(7) Uani 1 1 d . U . . . H6 H -0.3472 0.2996 -0.1860 0.052 Uiso 1 1 calc R U . . . C7 C -0.1654(3) 0.32850(17) -0.0501(2) 0.0345(6) Uani 1 1 d . U . . . H7 H -0.1483 0.3757 -0.0858 0.041 Uiso 1 1 calc R U . . . C8 C -0.0937(3) 0.45287(16) 0.2107(3) 0.0392(6) Uani 1 1 d . U . . . C12 C 0.2522(3) 0.26975(17) 0.0752(2) 0.0355(6) Uani 1 1 d . U . . . C13 C 0.1605(3) 0.2528(2) -0.0566(3) 0.0476(8) Uani 1 1 d . U . . . H13A H 0.2168 0.2216 -0.0995 0.071 Uiso 1 1 calc R U . . . H13B H 0.1327 0.3010 -0.1017 0.071 Uiso 1 1 calc R U . . . H13C H 0.0728 0.2249 -0.0534 0.071 Uiso 1 1 calc R U . . . C14 C 0.2783(4) 0.1970(2) 0.1537(3) 0.0607(9) Uani 1 1 d . U . . . H14A H 0.3276 0.1590 0.1151 0.091 Uiso 1 1 calc R U . . . H14B H 0.1850 0.1763 0.1588 0.091 Uiso 1 1 calc R U . . . H14C H 0.3391 0.2089 0.2376 0.091 Uiso 1 1 calc R U . . . C15 C 0.3976(3) 0.3030(2) 0.0681(3) 0.0541(8) Uani 1 1 d . U . . . H15A H 0.3805 0.3510 0.0208 0.081 Uiso 1 1 calc R U . . . H15B H 0.4461 0.2664 0.0264 0.081 Uiso 1 1 calc R U . . . H15C H 0.4593 0.3129 0.1524 0.081 Uiso 1 1 calc R U . . . C9A C -0.2165(9) 0.3948(4) 0.2113(10) 0.0611(18) Uani 0.77(2) 1 d . U P B 4 H91A H -0.2657 0.3797 0.1256 0.092 Uiso 0.77(2) 1 calc R U P B 4 H92A H -0.2867 0.4187 0.2490 0.092 Uiso 0.77(2) 1 calc R U P B 4 H93A H -0.1745 0.3495 0.2595 0.092 Uiso 0.77(2) 1 calc R U P B 4 C10A C -0.151(2) 0.5160(13) 0.1208(19) 0.072(4) Uani 0.77(2) 1 d . U P B 4 H111 H -0.0768 0.5557 0.1292 0.108 Uiso 0.77(2) 1 calc R U P B 4 H121 H -0.2377 0.5381 0.1382 0.108 Uiso 0.77(2) 1 calc R U P B 4 H131 H -0.1773 0.4957 0.0358 0.108 Uiso 0.77(2) 1 calc R U P B 4 C11A C -0.0360(9) 0.4811(7) 0.3433(7) 0.071(2) Uani 0.77(2) 1 d . U P B 4 H141 H -0.1129 0.5087 0.3677 0.107 Uiso 0.77(2) 1 calc R U P B 4 H151 H 0.0465 0.5155 0.3491 0.107 Uiso 0.77(2) 1 calc R U P B 4 H161 H -0.0042 0.4373 0.3990 0.107 Uiso 0.77(2) 1 calc R U P B 4 C9B C -0.168(3) 0.4029(15) 0.262(3) 0.063(3) Uani 0.23(2) 1 d . U P B 5 H91B H -0.1023 0.3809 0.3372 0.095 Uiso 0.23(2) 1 calc R U P B 5 H92B H -0.2067 0.3619 0.2019 0.095 Uiso 0.23(2) 1 calc R U P B 5 H93B H -0.2478 0.4294 0.2828 0.095 Uiso 0.23(2) 1 calc R U P B 5 C10B C -0.017(3) 0.514(2) 0.312(3) 0.071(5) Uani 0.23(2) 1 d . U P B 5 H112 H 0.0264 0.5539 0.2729 0.106 Uiso 0.23(2) 1 calc R U P B 5 H122 H 0.0589 0.4884 0.3770 0.106 Uiso 0.23(2) 1 calc R U P B 5 H132 H -0.0891 0.5363 0.3491 0.106 Uiso 0.23(2) 1 calc R U P B 5 C11B C -0.176(9) 0.505(5) 0.103(7) 0.071(6) Uani 0.23(2) 1 d . U P B 5 H142 H -0.2264 0.5450 0.1358 0.107 Uiso 0.23(2) 1 calc R U P B 5 H152 H -0.2465 0.4742 0.0418 0.107 Uiso 0.23(2) 1 calc R U P B 5 H162 H -0.1064 0.5280 0.0639 0.107 Uiso 0.23(2) 1 calc R U P B 5 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 Sn1A 0.0527(15) 0.068(2) 0.093(4) -0.0278(19) -0.0029(15) -0.0123(10) Sn2A 0.0260(7) 0.0237(8) 0.0548(17) -0.0060(7) -0.0039(7) -0.0013(4) Sn3A 0.044(2) 0.0588(18) 0.083(4) -0.0072(19) -0.012(2) -0.0040(11) F1 0.0446(10) 0.0379(9) 0.0546(10) -0.0128(8) -0.0138(8) 0.0043(8) F2 0.0512(12) 0.0405(10) 0.0872(15) 0.0140(10) -0.0119(10) -0.0083(9) F3 0.0585(13) 0.0760(16) 0.0993(18) -0.0454(14) -0.0256(12) 0.0299(12) N1 0.0288(11) 0.0344(12) 0.0241(10) -0.0038(9) -0.0020(8) -0.0012(9) N2 0.0348(12) 0.0329(12) 0.0344(12) -0.0053(9) 0.0059(9) -0.0028(9) C1 0.0320(13) 0.0319(13) 0.0184(11) 0.0029(9) 0.0026(9) -0.0003(10) C2 0.0275(12) 0.0319(13) 0.0264(12) -0.0034(10) 0.0029(9) 0.0012(10) C3 0.0369(14) 0.0356(14) 0.0348(14) 0.0020(11) 0.0051(11) -0.0009(11) C4 0.0433(16) 0.0373(15) 0.0524(17) -0.0035(13) 0.0166(13) -0.0085(12) C5 0.0330(14) 0.0522(18) 0.0494(17) -0.0204(14) 0.0101(12) -0.0101(13) C6 0.0303(14) 0.0580(19) 0.0347(14) -0.0110(13) -0.0014(11) 0.0027(13) C7 0.0314(13) 0.0408(15) 0.0276(12) 0.0014(11) 0.0016(10) 0.0016(11) C8 0.0429(15) 0.0359(15) 0.0398(15) -0.0020(12) 0.0131(12) 0.0049(12) C12 0.0341(14) 0.0410(15) 0.0289(13) -0.0018(11) 0.0043(11) 0.0072(11) C13 0.0443(17) 0.060(2) 0.0346(15) -0.0160(14) 0.0048(12) 0.0062(14) C14 0.072(2) 0.0497(19) 0.061(2) 0.0105(16) 0.0181(18) 0.0258(17) C15 0.0351(15) 0.074(2) 0.0532(18) -0.0123(17) 0.0114(13) 0.0009(15) C9A 0.061(4) 0.049(3) 0.090(5) -0.018(3) 0.047(4) -0.011(3) C10A 0.074(8) 0.068(7) 0.083(7) 0.027(6) 0.038(6) 0.033(5) C11A 0.077(4) 0.081(5) 0.060(4) -0.026(3) 0.025(3) 0.005(4) C9B 0.068(7) 0.054(6) 0.080(7) -0.005(6) 0.040(6) 0.004(6) C10B 0.072(8) 0.076(10) 0.069(9) -0.040(7) 0.027(7) 0.001(7) C11B 0.074(13) 0.073(12) 0.070(9) 0.019(8) 0.024(8) 0.040(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 Sn1A F3 1.783(13) . ? Sn1A F1 1.967(7) . ? Sn1A F2 2.174(9) . ? Sn1A F3 2.217(12) 3_666 ? Sn1A Sn1A 3.07(3) 3_666 ? Sn2A F1 2.017(3) . ? Sn2A F2 2.035(3) . ? Sn2A F3 2.043(5) . ? Sn2A F3 2.451(5) 3_666 ? Sn3A F2 2.077(10) . ? Sn3A F1 2.122(10) . ? Sn3A F3 2.44(2) . ? F3 Sn1A 2.217(12) 3_666 ? F3 Sn2A 2.451(5) 3_666 ? N1 C1 1.323(3) . ? N1 C12 1.494(3) . ? N2 C1 1.319(4) . ? N2 C8 1.497(4) . ? C1 C2 1.484(3) . ? C2 C3 1.383(4) . ? C2 C7 1.396(4) . ? C3 C4 1.385(4) . ? C4 C5 1.384(5) . ? C5 C6 1.381(5) . ? C6 C7 1.388(4) . ? C8 C9B 1.35(3) . ? C8 C10A 1.49(2) . ? C8 C11A 1.515(8) . ? C8 C11B 1.54(7) . ? C8 C9A 1.554(7) . ? C8 C10B 1.58(2) . ? C12 C13 1.521(4) . ? C12 C14 1.526(4) . ? C12 C15 1.531(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 F3 Sn1A F1 100.9(6) . . ? F3 Sn1A F2 87.8(3) . . ? F1 Sn1A F2 82.2(3) . . ? F3 Sn1A F3 80.2(6) . 3_666 ? F1 Sn1A F3 89.0(4) . 3_666 ? F2 Sn1A F3 163.5(7) . 3_666 ? F3 Sn1A Sn1A 45.3(4) . 3_666 ? F1 Sn1A Sn1A 95.5(6) . 3_666 ? F2 Sn1A Sn1A 132.0(6) . 3_666 ? F3 Sn1A Sn1A 34.9(2) 3_666 3_666 ? F1 Sn2A F2 84.61(11) . . ? F1 Sn2A F3 90.89(18) . . ? F2 Sn2A F3 85.12(16) . . ? F1 Sn2A F3 81.54(13) . 3_666 ? F2 Sn2A F3 151.1(2) . 3_666 ? F3 Sn2A F3 69.96(17) . 3_666 ? F2 Sn3A F1 81.0(4) . . ? F2 Sn3A F3 74.8(6) . . ? F1 Sn3A F3 78.4(6) . . ? Sn1A F3 Sn1A 99.8(6) . 3_666 ? Sn2A F3 Sn2A 110.04(17) . 3_666 ? C1 N1 C12 132.6(2) . . ? C1 N2 C8 132.8(2) . . ? N2 C1 N1 117.6(2) . . ? N2 C1 C2 121.0(2) . . ? N1 C1 C2 121.3(2) . . ? C3 C2 C7 119.9(2) . . ? C3 C2 C1 120.3(2) . . ? C7 C2 C1 119.8(2) . . ? C2 C3 C4 120.7(3) . . ? C5 C4 C3 119.4(3) . . ? C6 C5 C4 120.3(3) . . ? C5 C6 C7 120.6(3) . . ? C6 C7 C2 119.1(3) . . ? C9B C8 N2 113.8(11) . . ? C10A C8 N2 107.7(10) . . ? C10A C8 C11A 112.7(9) . . ? N2 C8 C11A 106.0(4) . . ? C9B C8 C11B 120(3) . . ? N2 C8 C11B 108(3) . . ? C10A C8 C9A 110.2(8) . . ? N2 C8 C9A 114.0(3) . . ? C11A C8 C9A 106.3(4) . . ? C9B C8 C10B 109.1(13) . . ? N2 C8 C10B 101.8(10) . . ? C11B C8 C10B 102(3) . . ? N1 C12 C13 113.4(2) . . ? N1 C12 C14 109.7(2) . . ? C13 C12 C14 110.7(3) . . ? N1 C12 C15 104.7(2) . . ? C13 C12 C15 108.3(2) . . ? C14 C12 C15 109.8(3) . . ? _refine_diff_density_max 0.410 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.072 _shelxl_version_number 2013-4 _shelx_res_file ; TITL solve in P2(1)/c CELL 0.6199 9.573 17.473 11.177 90.000 105.99 90.000 ZERR 4.00 0.005 0.004 0.012 0.000 0.05 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N F Sn DISP $C 0.00341 0.00169 11.495!source kissel DISP $H -0.00002 0.00000 0.623989!source kissel DISP $N 0.00664 0.00342 19.5902!source kissel DISP $F 0.01796 0.01064 51.4704!source kissel DISP $Sn -0.63245 1.44791 6106.48!source kissel UNIT 60 100 8 12 4 OMIT 0 4 0 OMIT -1 1 1 L.S. 10 BOND ACTA LIST 6 FMAP 2 PLAN 20 TEMP -153 DELU ISOR 0.01 SN1A SN2A SN3A SUMP 1 0.001 1.0 3 1.0 4 1.0 5 SIMU 0.005 C10A C10B C9A C9B C11A C11B WGHT 0.033200 1.536500 EXTI 0.031820 FVAR 0.55269 0.76576 0.29294 0.49393 0.20938 PART 1 SN1A 5 0.456942 0.504777 0.357309 31.00000 0.05267 0.06786 = 0.09324 -0.02776 -0.00288 -0.01232 PART 2 SN2A 5 0.455750 0.508010 0.329058 41.00000 0.02596 0.02372 = 0.05482 -0.00596 -0.00390 -0.00133 PART 3 SN3A 5 0.470566 0.508287 0.298431 51.00000 0.04420 0.05877 = 0.08283 -0.00722 -0.01183 -0.00399 PART 0 F1 4 0.400672 0.396604 0.329307 11.00000 0.04462 0.03794 = 0.05458 -0.01278 -0.01379 0.00427 F2 4 0.248593 0.522176 0.220534 11.00000 0.05119 0.04053 = 0.08720 0.01395 -0.01193 -0.00828 F3 4 0.370653 0.529612 0.474382 11.00000 0.05855 0.07598 = 0.09933 -0.04541 -0.02563 0.02987 N1 3 0.188373 0.330044 0.139067 11.00000 0.02880 0.03438 = 0.02411 -0.00381 -0.00199 -0.00121 AFIX 43 H1 2 0.253614 0.356145 0.195063 11.00000 0.04244 AFIX 0 N2 3 0.033344 0.418330 0.176810 11.00000 0.03480 0.03290 = 0.03438 -0.00530 0.00586 -0.00276 AFIX 43 H2 2 0.110104 0.448329 0.192635 11.00000 0.04024 AFIX 0 C1 1 0.053112 0.351889 0.127965 11.00000 0.03201 0.03192 = 0.01841 0.00294 0.00257 -0.00033 C2 1 -0.072214 0.303681 0.062465 11.00000 0.02748 0.03189 = 0.02637 -0.00340 0.00289 0.00116 C3 1 -0.098496 0.234925 0.113537 11.00000 0.03694 0.03565 = 0.03481 0.00203 0.00514 -0.00086 AFIX 43 H3 2 -0.034593 0.218100 0.189968 11.00000 -1.20000 AFIX 0 C4 1 -0.217031 0.190318 0.054422 11.00000 0.04330 0.03732 = 0.05237 -0.00354 0.01660 -0.00851 AFIX 43 H4 2 -0.234781 0.143252 0.090198 11.00000 -1.20000 AFIX 0 C5 1 -0.309371 0.214903 -0.057198 11.00000 0.03296 0.05222 = 0.04943 -0.02037 0.01006 -0.01007 AFIX 43 H5 2 -0.390876 0.184594 -0.098243 11.00000 -1.20000 AFIX 0 C6 1 -0.283521 0.283304 -0.109149 11.00000 0.03032 0.05803 = 0.03472 -0.01103 -0.00143 0.00273 AFIX 43 H6 2 -0.347177 0.299592 -0.186048 11.00000 -1.20000 AFIX 0 C7 1 -0.165426 0.328500 -0.050105 11.00000 0.03137 0.04078 = 0.02756 0.00139 0.00157 0.00159 AFIX 43 H7 2 -0.148251 0.375693 -0.085817 11.00000 -1.20000 AFIX 0 C8 1 -0.093665 0.452875 0.210695 11.00000 0.04291 0.03591 = 0.03980 -0.00195 0.01309 0.00489 C12 1 0.252152 0.269749 0.075198 11.00000 0.03409 0.04097 = 0.02890 -0.00177 0.00433 0.00720 C13 1 0.160454 0.252804 -0.056555 11.00000 0.04431 0.06022 = 0.03455 -0.01605 0.00478 0.00618 AFIX 137 H13A 2 0.216807 0.221632 -0.099476 11.00000 -1.50000 H13B 2 0.132703 0.301000 -0.101689 11.00000 -1.50000 H13C 2 0.072785 0.224865 -0.053370 11.00000 -1.50000 AFIX 0 C14 1 0.278305 0.196981 0.153677 11.00000 0.07180 0.04965 = 0.06063 0.01049 0.01813 0.02575 AFIX 137 H14A 2 0.327611 0.159043 0.115089 11.00000 -1.50000 H14B 2 0.184984 0.176278 0.158797 11.00000 -1.50000 H14C 2 0.339121 0.208882 0.237556 11.00000 -1.50000 AFIX 0 C15 1 0.397616 0.303006 0.068055 11.00000 0.03508 0.07360 = 0.05324 -0.01232 0.01145 0.00092 AFIX 137 H15A 2 0.380517 0.350974 0.020822 11.00000 -1.50000 H15B 2 0.446087 0.266381 0.026416 11.00000 -1.50000 H15C 2 0.459346 0.312947 0.152355 11.00000 -1.50000 AFIX 0 PART 4 C9A 1 -0.216494 0.394834 0.211257 21.00000 0.06073 0.04862 = 0.08984 -0.01800 0.04745 -0.01090 AFIX 137 H91A 2 -0.265745 0.379676 0.125597 21.00000 -1.50000 H92A 2 -0.286711 0.418719 0.249015 21.00000 -1.50000 H93A 2 -0.174480 0.349508 0.259514 21.00000 -1.50000 AFIX 0 C10A 1 -0.151299 0.516013 0.120773 21.00000 0.07363 0.06849 = 0.08290 0.02723 0.03831 0.03322 AFIX 137 H111 2 -0.076790 0.555659 0.129246 21.00000 -1.50000 H121 2 -0.237672 0.538150 0.138247 21.00000 -1.50000 H131 2 -0.177292 0.495701 0.035764 21.00000 -1.50000 AFIX 0 C11A 1 -0.035988 0.481093 0.343337 21.00000 0.07702 0.08096 = 0.05957 -0.02637 0.02540 0.00477 AFIX 137 H141 2 -0.112925 0.508718 0.367731 21.00000 -1.50000 H151 2 0.046463 0.515486 0.349061 21.00000 -1.50000 H161 2 -0.004191 0.437332 0.399027 21.00000 -1.50000 AFIX 0 PART 5 C9B 1 -0.167666 0.402854 0.261607 -21.00000 0.06813 0.05352 = 0.07971 -0.00461 0.04012 0.00399 AFIX 137 H91B 2 -0.102345 0.380892 0.337156 -21.00000 -1.50000 H92B 2 -0.206697 0.361854 0.201932 -21.00000 -1.50000 H93B 2 -0.247837 0.429397 0.282803 -21.00000 -1.50000 AFIX 0 C10B 1 -0.017107 0.513602 0.312014 -21.00000 0.07178 0.07559 = 0.06862 -0.04035 0.02683 0.00122 AFIX 137 H112 2 0.026423 0.553877 0.272898 -21.00000 -1.50000 H122 2 0.058920 0.488397 0.377034 -21.00000 -1.50000 H132 2 -0.089102 0.536262 0.349058 -21.00000 -1.50000 AFIX 0 C11B 1 -0.175657 0.504720 0.103305 -21.00000 0.07401 0.07251 = 0.06957 0.01867 0.02441 0.03971 AFIX 137 H142 2 -0.226395 0.545022 0.135754 -21.00000 -1.50000 H152 2 -0.246475 0.474191 0.041761 -21.00000 -1.50000 H162 2 -0.106423 0.528031 0.063871 -21.00000 -1.50000 PART 0 AFIX 0 HKLF 4 REM solve in P2(1)/c REM R1 = 0.0362 for 2973 Fo > 4sig(Fo) and 0.0377 for all 3192 data REM 251 parameters refined using 106 restraints END WGHT 0.0333 1.5396 REM Highest difference peak 0.410, deepest hole -0.457, 1-sigma level 0.072 Q1 1 0.3954 0.4689 0.2758 11.00000 0.05 0.41 Q2 1 0.2790 0.5102 0.1571 11.00000 0.05 0.32 Q3 1 0.2207 0.2984 0.1149 11.00000 0.05 0.31 Q4 1 -0.0158 0.3289 0.0958 11.00000 0.05 0.30 Q5 1 0.5341 0.5409 0.4029 11.00000 0.05 0.30 Q6 1 -0.1278 0.2764 0.0877 11.00000 0.05 0.30 Q7 1 0.3053 0.4674 0.2143 11.00000 0.05 0.29 Q8 1 -0.0783 0.5336 0.1955 11.00000 0.05 0.28 Q9 1 -0.0275 0.4303 0.1830 11.00000 0.05 0.27 Q10 1 0.4596 0.5572 0.5801 11.00000 0.05 0.27 Q11 1 -0.0615 0.4343 0.3359 11.00000 0.05 0.26 Q12 1 -0.3178 0.2575 -0.0800 11.00000 0.05 0.26 Q13 1 -0.2772 0.2083 0.0146 11.00000 0.05 0.25 Q14 1 -0.2604 0.4241 0.0918 11.00000 0.05 0.24 Q15 1 0.1256 0.3204 0.1476 11.00000 0.05 0.24 Q16 1 0.0253 0.3836 0.1440 11.00000 0.05 0.23 Q17 1 -0.1057 0.3120 0.0296 11.00000 0.05 0.23 Q18 1 0.2830 0.2445 0.0993 11.00000 0.05 0.23 Q19 1 0.3840 0.5520 0.3853 11.00000 0.05 0.22 Q20 1 0.4110 0.5516 0.3086 11.00000 0.05 0.21 ; _shelx_res_checksum 95947 _shelx_hkl_file ; -1 0 0 1127.87 83.8520 1 1 0 0 1424.75 105.811 1 -2 0 0 927.210 69.2240 1 2 0 0 971.810 72.5562 1 3 0 0 2365.51 176.011 1 -3 0 0 2335.51 173.820 1 -4 0 0 1144.70 85.8723 1 4 0 0 1174.49 88.0200 1 5 0 0 5.27396 1.32037 1 -5 0 0 4.43703 1.18135 1 6 0 0 269.949 21.4176 1 -6 0 0 257.720 20.5256 1 7 0 0 50.3477 5.31121 1 -7 0 0 50.5684 5.18549 1 8 0 0 283.595 22.7332 1 -8 0 0 275.376 22.1223 1 -9 0 0 47.8460 5.20872 1 9 0 0 34.2449 4.29288 1 10 0 0 273.140 22.4232 1 11 0 0 271.258 22.5071 1 0 -1 0 0.32518 0.13948 1 -1 -1 0 2.13926 0.41028 1 1 -1 0 2.90002 0.51983 1 -1 1 0 3.17842 0.52480 1 1 1 0 2.28611 0.42594 1 -2 -1 0 377.024 28.4818 1 2 -1 0 362.456 27.4151 1 -2 1 0 365.886 27.6990 1 2 1 0 395.929 29.9106 1 3 -1 0 72.8836 6.18671 1 -3 -1 0 68.4572 5.80308 1 -3 1 0 75.8021 6.42808 1 3 1 0 76.2799 6.43703 1 4 -1 0 359.597 27.6425 1 -4 -1 0 348.628 26.8516 1 4 1 0 379.211 29.1296 1 -5 -1 0 0.47007 0.72470 1 5 -1 0 0.83906 0.79029 1 -5 1 0 0.82410 0.77789 1 5 1 0 0.46001 0.81557 1 6 -1 0 183.716 15.0406 1 -6 -1 0 180.670 14.8122 1 -6 1 0 181.898 14.8885 1 6 1 0 186.360 15.2001 1 -7 -1 0 3.22916 1.23001 1 -7 1 0 3.04573 1.17542 1 7 1 0 3.77946 1.35796 1 -8 -1 0 150.165 12.8266 1 8 -1 0 145.127 12.4567 1 8 1 0 142.368 12.3052 1 -8 1 0 143.280 12.3136 1 -9 -1 0 18.9680 2.86209 1 9 -1 0 20.0701 3.02495 1 -9 1 0 22.1815 3.12955 1 9 1 0 18.1546 2.96772 1 10 -1 0 0.19649 1.06575 1 10 1 0 0.53219 1.32687 1 0 -2 0 2920.63 216.681 1 0 2 0 2632.57 195.334 1 -1 -2 0 3453.86 256.314 1 1 -2 0 4508.56 334.416 1 -1 2 0 4300.09 318.962 1 1 2 0 3951.34 293.148 1 -2 -2 0 8184.38 606.922 1 2 -2 0 6561.48 486.662 1 2 2 0 6482.54 481.088 1 -2 2 0 7496.68 555.934 1 3 -2 0 1777.58 132.551 1 -3 -2 0 1853.88 138.137 1 -3 2 0 1887.19 140.734 1 3 2 0 1732.16 129.148 1 -4 -2 0 1142.71 85.7621 1 4 -2 0 1235.88 92.5990 1 4 2 0 1216.21 91.2033 1 -5 -2 0 18.2527 2.42988 1 5 -2 0 17.6070 2.37193 1 -5 2 0 13.4720 2.07044 1 5 2 0 26.0465 3.06439 1 -6 -2 0 1.79994 0.99725 1 -6 2 0 1.65122 0.96797 1 6 2 0 2.34620 1.04447 1 -7 -2 0 33.5743 3.92596 1 -7 2 0 34.3144 3.91902 1 7 2 0 28.7956 3.62595 1 8 -2 0 32.8894 3.99634 1 -8 -2 0 32.4985 3.92996 1 8 2 0 27.9679 3.64335 1 -8 2 0 35.1194 4.12654 1 9 -2 0 488.809 38.1404 1 -9 -2 0 500.241 38.8644 1 -9 2 0 503.140 39.1144 1 9 2 0 482.199 37.7519 1 10 -2 0 461.954 36.3530 1 10 2 0 479.765 37.8500 1 0 -3 0 0.24608 0.30676 1 0 3 0 0.48186 0.30034 1 1 -3 0 357.166 26.9603 1 -1 -3 0 328.054 24.7629 1 1 3 0 318.835 24.0811 1 -1 3 0 359.559 27.1487 1 2 -3 0 1.60951 0.63615 1 -2 -3 0 0.79005 0.47752 1 -2 3 0 1.72368 0.62212 1 2 3 0 1.18462 0.55085 1 3 -3 0 443.230 33.7807 1 -3 -3 0 432.859 32.8884 1 3 3 0 433.058 32.9220 1 -3 3 0 407.761 31.1670 1 4 -3 0 767.881 58.0261 1 4 3 0 903.521 67.9928 1 -4 3 0 914.695 68.9351 1 5 -3 0 7.79288 1.56478 1 -5 -3 0 7.31482 1.53725 1 -5 3 0 8.43968 1.71818 1 5 3 0 6.56757 1.46687 1 -6 -3 0 54.2159 5.32208 1 6 -3 0 57.8601 5.63685 1 6 3 0 58.7436 5.75180 1 -6 3 0 56.0373 5.56658 1 7 -3 0 0.90614 0.93403 1 -7 -3 0 1.03634 0.97437 1 7 3 0 0.88361 0.93411 1 -7 3 0 0.53752 0.80180 1 8 -3 0 55.5905 5.74506 1 -8 -3 0 51.4702 5.46743 1 8 3 0 55.6731 5.87320 1 -8 3 0 49.9526 5.33910 1 9 -3 0 65.9693 6.70224 1 -9 -3 0 64.5057 6.47449 1 -9 3 0 61.0806 6.21201 1 9 3 0 64.9991 6.77600 1 10 -3 0 13.2472 2.58445 1 10 3 0 12.4012 2.69180 1 0 -4 0 5530.86 410.325 1 -1 -4 0 4516.38 335.226 1 1 -4 0 4252.97 315.676 1 1 4 0 4633.82 343.900 1 -1 4 0 3248.37 241.331 1 2 -4 0 1636.08 122.023 1 -2 -4 0 2104.91 156.670 1 2 4 0 2015.18 150.099 1 -2 4 0 2046.95 152.475 1 -3 -4 0 2067.41 154.083 1 -3 4 0 1987.10 148.231 1 3 4 0 2056.70 153.339 1 4 -4 0 1340.22 100.461 1 4 4 0 1473.50 110.334 1 -4 4 0 1323.63 99.2955 1 5 -4 0 1247.76 93.7915 1 -5 -4 0 1302.81 97.8644 1 5 4 0 1102.27 83.1057 1 -5 4 0 1159.67 87.3633 1 6 -4 0 11.7702 2.06545 1 -6 -4 0 9.32850 1.84256 1 -6 4 0 11.0738 2.01379 1 7 -4 0 141.874 12.1012 1 -7 -4 0 134.249 11.5426 1 -8 -4 0 71.2714 6.93078 1 8 -4 0 68.1792 6.72345 1 -8 4 0 78.0433 7.48447 1 8 4 0 58.1693 6.17899 1 9 -4 0 372.243 29.5000 1 -9 -4 0 377.775 29.8878 1 -9 4 0 375.838 29.7485 1 9 4 0 348.181 28.0365 1 10 -4 0 356.585 28.5542 1 10 4 0 322.024 26.4430 1 0 -5 0 0.06909 0.37187 1 0 5 0 0.20007 0.33255 1 1 -5 0 555.852 41.9645 1 -1 -5 0 541.608 40.8634 1 1 5 0 482.007 36.5348 1 -1 5 0 544.096 41.0603 1 -2 -5 0 509.366 38.5430 1 2 -5 0 590.415 44.6184 1 2 5 0 522.738 39.5765 1 -2 5 0 563.768 42.6999 1 3 -5 0 597.933 45.3679 1 -3 -5 0 535.274 40.6590 1 -3 5 0 598.819 45.4354 1 3 5 0 542.522 41.3245 1 4 -5 0 30.7678 3.39872 1 4 5 0 27.1646 3.12829 1 -4 5 0 27.6187 3.16258 1 -5 -5 0 390.630 30.2222 1 5 -5 0 394.998 30.6379 1 5 5 0 372.311 29.0238 1 -5 5 0 317.158 24.9325 1 6 -5 0 36.1387 4.08039 1 -6 -5 0 33.3902 3.80982 1 6 5 0 35.2244 4.02240 1 -6 5 0 34.8793 4.00651 1 7 -5 0 3.08778 1.24003 1 -7 -5 0 3.06793 1.25067 1 8 -5 0 125.844 10.9755 1 -8 -5 0 114.324 10.2369 1 -8 5 0 125.628 11.1523 1 8 5 0 128.439 11.5550 1 -9 -5 0 1.46023 1.16861 1 9 -5 0 2.27385 1.24256 1 -9 5 0 2.05497 1.15474 1 9 5 0 1.51922 1.28870 1 10 -5 0 16.4050 2.84289 1 10 5 0 15.6461 3.02029 1 0 -6 0 5981.00 443.842 1 0 6 0 6384.41 473.889 1 -1 -6 0 3331.74 247.648 1 -1 -6 0 4138.76 307.562 1 1 -6 0 3722.19 276.690 1 -1 6 0 3683.24 273.725 1 -2 -6 0 1730.26 129.138 1 -2 6 0 1710.46 127.708 1 2 6 0 1751.74 130.783 1 3 -6 0 2724.43 202.989 1 -3 -6 0 3242.05 241.299 1 -4 -6 0 1180.17 88.6073 1 4 -6 0 1102.23 82.9925 1 4 6 0 1268.62 95.3860 1 -4 6 0 1057.01 79.6287 1 -5 -6 0 51.6995 5.12925 1 5 -6 0 50.0764 5.04655 1 -5 6 0 38.2574 4.14403 1 6 -6 0 60.2625 5.94797 1 -6 -6 0 68.4718 6.49002 1 -6 6 0 50.3859 5.25232 1 6 6 0 67.8329 6.68322 1 -7 -6 0 3.49679 1.31059 1 7 -6 0 4.71176 1.45155 1 -7 6 0 5.81589 1.57484 1 -8 -6 0 284.422 22.8370 1 8 -6 0 283.804 22.8269 1 -8 6 0 333.199 26.4930 1 -9 -6 0 154.165 13.2465 1 9 -6 0 163.079 13.9231 1 9 6 0 144.730 13.0249 1 10 -6 0 325.440 26.1664 1 10 6 0 316.210 26.0895 1 0 -7 0 0.15239 0.44327 1 0 7 0 -0.0399 0.37562 1 -1 -7 0 786.900 59.3582 1 1 -7 0 823.890 61.9708 1 -1 -7 0 854.404 64.2330 1 -1 7 0 808.093 60.8277 1 2 -7 0 531.379 40.4139 1 -2 -7 0 468.100 35.7364 1 -2 7 0 543.413 41.3920 1 2 7 0 507.153 38.7324 1 3 -7 0 646.658 49.0937 1 3 7 0 675.393 51.3076 1 -3 7 0 729.362 55.2577 1 4 -7 0 267.431 21.1624 1 -4 -7 0 256.634 20.3373 1 4 7 0 259.111 20.6742 1 -4 7 0 255.623 20.2700 1 -5 -7 0 458.772 35.4406 1 5 -7 0 460.946 35.6679 1 5 7 0 472.459 36.7723 1 -5 7 0 434.253 33.6404 1 -6 -7 0 11.8893 2.15788 1 6 7 0 13.8035 2.38615 1 -6 7 0 11.4306 2.11883 1 7 -7 0 14.3730 2.41033 1 -7 -7 0 13.9605 2.42707 1 -7 7 0 11.7713 2.17396 1 -8 -7 0 18.5201 2.89974 1 8 -7 0 18.3683 2.85708 1 8 7 0 17.9026 3.10797 1 -8 7 0 19.0777 2.82463 1 -9 -7 0 87.0021 8.22668 1 9 7 0 84.3243 8.52796 1 10 -7 0 14.0501 2.64312 1 10 7 0 13.4792 2.98726 1 0 8 0 2606.33 194.097 1 1 -8 0 3444.49 256.269 1 -1 -8 0 3841.52 285.846 1 -1 8 0 3503.09 260.647 1 2 -8 0 2207.06 164.620 1 -2 -8 0 2431.31 181.375 1 2 8 0 2662.68 198.661 1 3 -8 0 1701.45 127.320 1 -3 -8 0 1654.63 123.912 1 3 8 0 1818.76 136.326 1 -3 8 0 1570.32 117.657 1 -4 -8 0 630.217 48.1386 1 4 -8 0 587.727 44.9278 1 4 8 0 665.272 50.9363 1 -4 8 0 517.909 39.8123 1 5 -8 0 166.242 13.8360 1 -5 -8 0 176.787 14.6089 1 -5 8 0 149.552 12.6345 1 5 8 0 212.562 17.4192 1 6 -8 0 5.49321 1.50199 1 -6 -8 0 7.71647 1.76789 1 7 -8 0 98.4443 8.99900 1 -7 8 0 109.664 9.82766 1 7 8 0 81.1838 8.03332 1 8 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