##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
# http://www.iucr.org/resources/cif/software. #
# #
# This file may be used for bona fide research purposes within the #
# scientific community so long as proper attribution is given to the journal #
# article from which it was obtained. #
# #
##############################################################################
data_global
_audit_creation_method 'form.cif (version 2.0)'
_journal_data_validation_number ?
_journal_date_recd_electronic 2012-11-21
_journal_date_accepted 2012-11-29
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2013
_journal_volume 69
_journal_issue 1
_journal_page_first m46
_journal_page_last m46
_journal_paper_category QM
_journal_paper_doi 10.1107/S1600536812049069
_journal_coeditor_code IS5223
_publ_contact_author_name 'Dr. Abri, Abdolreza'
_publ_contact_author_address
;
Department of Chemistry,
Azarbaijan Shahid Madani University,
Tabriz,
Iran
;
_publ_contact_author_email 'zsrkk@yahoo.com & Ar.abri@azaruniv.edu'
_publ_contact_author_fax '+98-(0)412-4327541'
_publ_contact_author_phone '+98-(0)412-4327541'
_publ_section_title
;
1,1'-Bis(tert-butyldimethylsilyl)ferrocene
;
loop_
_publ_author_name
_publ_author_address
'Abri, Abdolreza'
;
Department of Chemistry,
Azarbaijan Shahid Madani University,
Tabriz,
Iran
;
'Soltani, Behzad'
;
Department of Chemistry,
Azarbaijan Shahid Madani University,
Tabriz,
Iran
;
'Ziegler, Christopher J.'
;
Department of Chemistry,
University of Akron,
Akron,
OH,
USA
;
'Engle, James T.'
;
Department of Chemistry,
University of Akron,
Akron,
OH,
USA
;
'Kia, Reza'
;
Department of Chemistry,
Science and Rsearch Branch,
Islamic Azad University
Tehran,
Iran
;
data_I
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
1,1'-Bis(tert-butyldimethylsilyl)ferrocene
;
_chemical_name_common '1,1'-bis(tert-butyldimethylsilyl)ferrocene'
_chemical_formula_moiety 'C22 H38 Fe Si2'
_chemical_formula_sum 'C22 H38 Fe Si2'
_chemical_formula_iupac '[Fe (C11 H19 Si)2]'
_chemical_formula_weight 414.55
_chemical_melting_point ?
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M 'P b c n'
_symmetry_space_group_name_Hall '-P 2n 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
_cell_length_a 7.1282(6)
_cell_length_b 12.1466(10)
_cell_length_c 26.363(2)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 2282.6(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9976
_cell_measurement_theta_min 2.32
_cell_measurement_theta_max 27.16
_cell_measurement_temperature 100(2)
_exptl_crystal_description block
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.10
_exptl_crystal_density_diffrn 1.206
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 896
_exptl_absorpt_coefficient_mu 0.769
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Bruker, 2005)'
_exptl_absorpt_correction_T_min 0.8614
_exptl_absorpt_correction_T_max 0.9271
_exptl_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 17220
_diffrn_reflns_av_R_equivalents 0.0372
_diffrn_reflns_av_sigmaI/netI 0.0233
_diffrn_reflns_theta_min 3.09
_diffrn_reflns_theta_max 27.18
_diffrn_reflns_theta_full 27.18
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_limit_l_max 33
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% .
_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^ >
\s(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.
;
_reflns_number_total 2529
_reflns_number_gt 2323
_reflns_threshold_expression I>2\s(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0288
_refine_ls_R_factor_gt 0.0262
_refine_ls_wR_factor_gt 0.0654
_refine_ls_wR_factor_ref 0.0672
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_restrained_S_all 1.045
_refine_ls_number_reflns 2529
_refine_ls_number_parameters 114
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+1.1338P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.361
_refine_diff_density_min -0.241
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
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'
'Fe' 'Fe' 0.3463 0.8444
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Si' 'Si' 0.0817 0.0704
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection 'APEX2 (Bruker, 2005)'
_computing_cell_refinement 'SAINT (Bruker, 2005)'
_computing_data_reduction 'SAINT (Bruker, 2005)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 1.0000 0.03916(2) 0.2500 0.01182(9) Uani d S 1 2 . .
Si Si1 0.96501(5) 0.11765(3) 0.122364(13) 0.01274(10) Uani d . 1 1 . .
C C1 0.7486(2) -0.04225(12) 0.24866(5) 0.0212(3) Uani d . 1 1 . .
H H1 0.7161 -0.1051 0.2682 0.025 Uiso calc R 1 1 . .
C C2 0.8338(2) -0.04320(11) 0.19970(5) 0.0181(3) Uani d . 1 1 . .
H H2 0.8674 -0.1072 0.1811 0.022 Uiso calc R 1 1 . .
C C3 0.86070(18) 0.06855(10) 0.18305(5) 0.0143(3) Uani d . 1 1 . .
C C4 0.78856(18) 0.13706(11) 0.22318(5) 0.0167(3) Uani d . 1 1 . .
H H4 0.7866 0.2153 0.2230 0.020 Uiso calc R 1 1 . .
C C5 0.72076(18) 0.06891(12) 0.26299(5) 0.0197(3) Uani d . 1 1 . .
H H5 0.6663 0.0936 0.2938 0.024 Uiso calc R 1 1 . .
C C6 1.14332(19) 0.01654(11) 0.09925(5) 0.0198(3) Uani d . 1 1 . .
H H6A 1.2446 0.0103 0.1242 0.030 Uiso calc R 1 1 . .
H H6B 1.1949 0.0419 0.0668 0.030 Uiso calc R 1 1 . .
H H6C 1.0839 -0.0555 0.0946 0.030 Uiso calc R 1 1 . .
C C7 1.0752(2) 0.25562(11) 0.13317(5) 0.0203(3) Uani d . 1 1 . .
H H7A 1.1764 0.2486 0.1581 0.030 Uiso calc R 1 1 . .
H H7B 0.9803 0.3071 0.1459 0.030 Uiso calc R 1 1 . .
H H7C 1.1266 0.2833 0.1012 0.030 Uiso calc R 1 1 . .
C C8 0.76825(18) 0.13000(10) 0.07396(5) 0.0156(3) Uani d . 1 1 . .
C C9 0.6877(2) 0.01524(12) 0.06271(5) 0.0231(3) Uani d . 1 1 . .
H H9A 0.5864 0.0216 0.0378 0.035 Uiso calc R 1 1 . .
H H9B 0.6384 -0.0170 0.0941 0.035 Uiso calc R 1 1 . .
H H9D 0.7870 -0.0321 0.0491 0.035 Uiso calc R 1 1 . .
C C10 0.61107(19) 0.20356(12) 0.09496(5) 0.0212(3) Uani d . 1 1 . .
H H10A 0.5103 0.2095 0.0698 0.032 Uiso calc R 1 1 . .
H H10D 0.6613 0.2770 0.1022 0.032 Uiso calc R 1 1 . .
H H10B 0.5613 0.1711 0.1262 0.032 Uiso calc R 1 1 . .
C C11 0.8419(2) 0.18068(12) 0.02429(5) 0.0233(3) Uani d . 1 1 . .
H H11D 0.7389 0.1864 -0.0002 0.035 Uiso calc R 1 1 . .
H H11A 0.9409 0.1337 0.0103 0.035 Uiso calc R 1 1 . .
H H11B 0.8927 0.2542 0.0311 0.035 Uiso calc R 1 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Fe1 0.01172(14) 0.01365(14) 0.01008(14) 0.000 -0.00130(9) 0.000
Si1 0.01328(17) 0.01321(18) 0.01173(17) -0.00049(13) -0.00074(13)
0.00000(12)
C1 0.0187(7) 0.0279(8) 0.0170(7) -0.0100(6) -0.0031(5) 0.0032(5)
C2 0.0212(7) 0.0189(7) 0.0142(6) -0.0060(5) -0.0039(5) -0.0003(5)
C3 0.0130(6) 0.0168(6) 0.0130(6) -0.0010(5) -0.0042(5) -0.0004(5)
C4 0.0135(6) 0.0221(7) 0.0146(6) 0.0036(5) -0.0030(5) -0.0009(5)
C5 0.0107(6) 0.0339(8) 0.0145(6) 0.0004(6) -0.0010(5) -0.0009(5)
C6 0.0175(6) 0.0218(7) 0.0202(7) 0.0021(6) 0.0002(5) -0.0022(5)
C7 0.0217(7) 0.0179(7) 0.0212(7) -0.0034(6) -0.0016(6) 0.0004(5)
C8 0.0171(6) 0.0177(6) 0.0121(6) 0.0005(5) -0.0012(5) 0.0011(5)
C9 0.0236(7) 0.0245(7) 0.0213(7) -0.0034(6) -0.0079(6) -0.0021(5)
C10 0.0185(7) 0.0271(7) 0.0179(6) 0.0051(6) -0.0019(5) 0.0022(5)
C11 0.0244(7) 0.0309(8) 0.0146(6) 0.0029(6) 0.0009(6) 0.0043(5)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 C2 4_755 2.0401(13) ?
Fe1 C2 . 2.0402(13) ?
Fe1 C4 . 2.0460(13) ?
Fe1 C4 4_755 2.0460(13) ?
Fe1 C1 4_755 2.0473(15) ?
Fe1 C1 . 2.0473(15) ?
Fe1 C5 4_755 2.0518(13) ?
Fe1 C5 . 2.0518(13) ?
Fe1 C3 . 2.0564(12) ?
Fe1 C3 4_755 2.0565(12) ?
Si1 C3 . 1.8622(13) ?
Si1 C6 . 1.8696(14) ?
Si1 C7 . 1.8726(14) ?
Si1 C8 . 1.9022(13) ?
C1 C5 . 1.416(2) ?
C1 C2 . 1.4267(19) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.4394(17) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.4409(17) ?
C4 C5 . 1.4214(19) ?
C4 H4 . 0.9500 ?
C5 H5 . 0.9500 ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 C9 . 1.5363(19) ?
C8 C10 . 1.5364(18) ?
C8 C11 . 1.5391(17) ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9D . 0.9800 ?
C10 H10A . 0.9800 ?
C10 H10D . 0.9800 ?
C10 H10B . 0.9800 ?
C11 H11D . 0.9800 ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 Fe1 C2 4_755 . 121.27(8) ?
C2 Fe1 C4 4_755 . 159.61(5) ?
C2 Fe1 C4 . . 68.45(5) ?
C2 Fe1 C4 4_755 4_755 68.45(5) ?
C2 Fe1 C4 . 4_755 159.61(5) ?
C4 Fe1 C4 . 4_755 108.92(8) ?
C2 Fe1 C1 4_755 4_755 40.86(5) ?
C2 Fe1 C1 . 4_755 106.42(6) ?
C4 Fe1 C1 . 4_755 158.69(5) ?
C4 Fe1 C1 4_755 4_755 68.27(6) ?
C2 Fe1 C1 4_755 . 106.42(6) ?
C2 Fe1 C1 . . 40.86(5) ?
C4 Fe1 C1 . . 68.27(6) ?
C4 Fe1 C1 4_755 . 158.69(5) ?
C1 Fe1 C1 4_755 . 122.24(9) ?
C2 Fe1 C5 4_755 4_755 68.38(6) ?
C2 Fe1 C5 . 4_755 122.76(6) ?
C4 Fe1 C5 . 4_755 123.69(6) ?
C4 Fe1 C5 4_755 4_755 40.59(5) ?
C1 Fe1 C5 4_755 4_755 40.42(6) ?
C1 Fe1 C5 . 4_755 158.67(6) ?
C2 Fe1 C5 4_755 . 122.76(6) ?
C2 Fe1 C5 . . 68.38(6) ?
C4 Fe1 C5 . . 40.59(5) ?
C4 Fe1 C5 4_755 . 123.68(6) ?
C1 Fe1 C5 4_755 . 158.67(6) ?
C1 Fe1 C5 . . 40.42(6) ?
C5 Fe1 C5 4_755 . 159.71(9) ?
C2 Fe1 C3 4_755 . 157.42(5) ?
C2 Fe1 C3 . . 41.14(5) ?
C4 Fe1 C3 . . 41.13(5) ?
C4 Fe1 C3 4_755 . 123.47(5) ?
C1 Fe1 C3 4_755 . 121.43(5) ?
C1 Fe1 C3 . . 69.29(5) ?
C5 Fe1 C3 4_755 . 107.13(5) ?
C5 Fe1 C3 . . 69.16(5) ?
C2 Fe1 C3 4_755 4_755 41.14(5) ?
C2 Fe1 C3 . 4_755 157.42(5) ?
C4 Fe1 C3 . 4_755 123.46(5) ?
C4 Fe1 C3 4_755 4_755 41.13(5) ?
C1 Fe1 C3 4_755 4_755 69.29(5) ?
C1 Fe1 C3 . 4_755 121.42(5) ?
C5 Fe1 C3 4_755 4_755 69.16(5) ?
C5 Fe1 C3 . 4_755 107.13(5) ?
C3 Fe1 C3 . 4_755 160.00(7) ?
C3 Si1 C6 . . 109.94(6) ?
C3 Si1 C7 . . 108.87(6) ?
C6 Si1 C7 . . 110.63(6) ?
C3 Si1 C8 . . 107.89(6) ?
C6 Si1 C8 . . 109.53(6) ?
C7 Si1 C8 . . 109.93(6) ?
C5 C1 C2 . . 107.98(12) ?
C5 C1 Fe1 . . 69.96(8) ?
C2 C1 Fe1 . . 69.30(8) ?
C5 C1 H1 . . 126.0 ?
C2 C1 H1 . . 126.0 ?
Fe1 C1 H1 . . 126.3 ?
C1 C2 C3 . . 108.96(12) ?
C1 C2 Fe1 . . 69.84(8) ?
C3 C2 Fe1 . . 70.04(7) ?
C1 C2 H2 . . 125.5 ?
C3 C2 H2 . . 125.5 ?
Fe1 C2 H2 . . 126.2 ?
C2 C3 C4 . . 105.85(11) ?
C2 C3 Si1 . . 128.11(10) ?
C4 C3 Si1 . . 126.04(10) ?
C2 C3 Fe1 . . 68.82(7) ?
C4 C3 Fe1 . . 69.05(7) ?
Si1 C3 Fe1 . . 126.88(7) ?
C5 C4 C3 . . 109.09(12) ?
C5 C4 Fe1 . . 69.92(7) ?
C3 C4 Fe1 . . 69.83(7) ?
C5 C4 H4 . . 125.5 ?
C3 C4 H4 . . 125.5 ?
Fe1 C4 H4 . . 126.4 ?
C1 C5 C4 . . 108.11(12) ?
C1 C5 Fe1 . . 69.62(8) ?
C4 C5 Fe1 . . 69.48(7) ?
C1 C5 H5 . . 125.9 ?
C4 C5 H5 . . 125.9 ?
Fe1 C5 H5 . . 126.5 ?
Si1 C6 H6A . . 109.5 ?
Si1 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
Si1 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
Si1 C7 H7A . . 109.5 ?
Si1 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
Si1 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C9 C8 C10 . . 108.95(11) ?
C9 C8 C11 . . 109.03(11) ?
C10 C8 C11 . . 108.82(11) ?
C9 C8 Si1 . . 109.48(9) ?
C10 C8 Si1 . . 109.98(9) ?
C11 C8 Si1 . . 110.54(9) ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C8 C9 H9D . . 109.5 ?
H9A C9 H9D . . 109.5 ?
H9B C9 H9D . . 109.5 ?
C8 C10 H10A . . 109.5 ?
C8 C10 H10D . . 109.5 ?
H10A C10 H10D . . 109.5 ?
C8 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
H10D C10 H10B . . 109.5 ?
C8 C11 H11D . . 109.5 ?
C8 C11 H11A . . 109.5 ?
H11D C11 H11A . . 109.5 ?
C8 C11 H11B . . 109.5 ?
H11D C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 Fe1 C1 C5 4_755 . . . 121.60(8) ?
C2 Fe1 C1 C5 . . . . -119.28(11) ?
C4 Fe1 C1 C5 . . . . -37.55(8) ?
C4 Fe1 C1 C5 4_755 . . . 48.96(18) ?
C1 Fe1 C1 C5 4_755 . . . 163.33(9) ?
C5 Fe1 C1 C5 4_755 . . . -165.93(10) ?
C3 Fe1 C1 C5 . . . . -81.80(8) ?
C3 Fe1 C1 C5 4_755 . . . 79.33(9) ?
C2 Fe1 C1 C2 4_755 . . . -119.12(9) ?
C4 Fe1 C1 C2 . . . . 81.73(8) ?
C4 Fe1 C1 C2 4_755 . . . 168.24(14) ?
C1 Fe1 C1 C2 4_755 . . . -77.39(8) ?
C5 Fe1 C1 C2 4_755 . . . -46.65(18) ?
C5 Fe1 C1 C2 . . . . 119.28(11) ?
C3 Fe1 C1 C2 . . . . 37.48(8) ?
C3 Fe1 C1 C2 4_755 . . . -161.39(8) ?
C5 C1 C2 C3 . . . . 0.20(16) ?
Fe1 C1 C2 C3 . . . . -59.29(10) ?
C5 C1 C2 Fe1 . . . . 59.49(10) ?
C2 Fe1 C2 C1 4_755 . . . 78.66(8) ?
C4 Fe1 C2 C1 . . . . -81.27(9) ?
C4 Fe1 C2 C1 4_755 . . . -167.72(15) ?
C1 Fe1 C2 C1 4_755 . . . 120.62(11) ?
C5 Fe1 C2 C1 4_755 . . . 161.66(9) ?
C5 Fe1 C2 C1 . . . . -37.47(8) ?
C3 Fe1 C2 C1 . . . . -120.11(12) ?
C3 Fe1 C2 C1 4_755 . . . 45.19(18) ?
C2 Fe1 C2 C3 4_755 . . . -161.23(9) ?
C4 Fe1 C2 C3 . . . . 38.84(8) ?
C4 Fe1 C2 C3 4_755 . . . -47.61(19) ?
C1 Fe1 C2 C3 4_755 . . . -119.27(8) ?
C1 Fe1 C2 C3 . . . . 120.11(12) ?
C5 Fe1 C2 C3 4_755 . . . -78.22(10) ?
C5 Fe1 C2 C3 . . . . 82.65(8) ?
C3 Fe1 C2 C3 4_755 . . . 165.30(9) ?
C1 C2 C3 C4 . . . . -0.26(15) ?
Fe1 C2 C3 C4 . . . . -59.42(8) ?
C1 C2 C3 Si1 . . . . -179.89(10) ?
Fe1 C2 C3 Si1 . . . . 120.94(11) ?
C1 C2 C3 Fe1 . . . . 59.17(10) ?
C6 Si1 C3 C2 . . . . -30.07(14) ?
C7 Si1 C3 C2 . . . . -151.41(12) ?
C8 Si1 C3 C2 . . . . 89.33(13) ?
C6 Si1 C3 C4 . . . . 150.36(11) ?
C7 Si1 C3 C4 . . . . 29.03(13) ?
C8 Si1 C3 C4 . . . . -90.24(12) ?
C6 Si1 C3 Fe1 . . . . 60.76(9) ?
C7 Si1 C3 Fe1 . . . . -60.57(10) ?
C8 Si1 C3 Fe1 . . . . -179.84(7) ?
C2 Fe1 C3 C2 4_755 . . . 45.8(2) ?
C4 Fe1 C3 C2 . . . . -117.52(11) ?
C4 Fe1 C3 C2 4_755 . . . 162.04(8) ?
C1 Fe1 C3 C2 4_755 . . . 78.70(10) ?
C1 Fe1 C3 C2 . . . . -37.23(8) ?
C5 Fe1 C3 C2 4_755 . . . 120.52(9) ?
C5 Fe1 C3 C2 . . . . -80.59(9) ?
C3 Fe1 C3 C2 4_755 . . . -163.45(8) ?
C2 Fe1 C3 C4 4_755 . . . 163.27(13) ?
C2 Fe1 C3 C4 . . . . 117.52(11) ?
C4 Fe1 C3 C4 4_755 . . . -80.44(11) ?
C1 Fe1 C3 C4 4_755 . . . -163.78(8) ?
C1 Fe1 C3 C4 . . . . 80.29(8) ?
C5 Fe1 C3 C4 4_755 . . . -121.96(8) ?
C5 Fe1 C3 C4 . . . . 36.93(8) ?
C3 Fe1 C3 C4 4_755 . . . -45.93(7) ?
C2 Fe1 C3 Si1 4_755 . . . -76.71(17) ?
C2 Fe1 C3 Si1 . . . . -122.46(12) ?
C4 Fe1 C3 Si1 . . . . 120.02(12) ?
C4 Fe1 C3 Si1 4_755 . . . 39.57(11) ?
C1 Fe1 C3 Si1 4_755 . . . -43.76(11) ?
C1 Fe1 C3 Si1 . . . . -159.69(10) ?
C5 Fe1 C3 Si1 4_755 . . . -1.95(10) ?
C5 Fe1 C3 Si1 . . . . 156.94(10) ?
C3 Fe1 C3 Si1 4_755 . . . 74.08(7) ?
C2 C3 C4 C5 . . . . 0.22(14) ?
Si1 C3 C4 C5 . . . . 179.86(9) ?
Fe1 C3 C4 C5 . . . . -59.06(9) ?
C2 C3 C4 Fe1 . . . . 59.28(9) ?
Si1 C3 C4 Fe1 . . . . -121.08(10) ?
C2 Fe1 C4 C5 4_755 . . . -41.15(19) ?
C2 Fe1 C4 C5 . . . . 81.50(9) ?
C4 Fe1 C4 C5 4_755 . . . -120.06(9) ?
C1 Fe1 C4 C5 4_755 . . . 161.35(15) ?
C1 Fe1 C4 C5 . . . . 37.39(8) ?
C5 Fe1 C4 C5 4_755 . . . -162.65(8) ?
C3 Fe1 C4 C5 . . . . 120.35(11) ?
C3 Fe1 C4 C5 4_755 . . . -76.78(10) ?
C2 Fe1 C4 C3 4_755 . . . -161.50(15) ?
C2 Fe1 C4 C3 . . . . -38.85(8) ?
C4 Fe1 C4 C3 4_755 . . . 119.58(8) ?
C1 Fe1 C4 C3 4_755 . . . 41.00(19) ?
C1 Fe1 C4 C3 . . . . -82.96(8) ?
C5 Fe1 C4 C3 4_755 . . . 76.99(9) ?
C5 Fe1 C4 C3 . . . . -120.35(11) ?
C3 Fe1 C4 C3 4_755 . . . 162.87(7) ?
C2 C1 C5 C4 . . . . -0.06(16) ?
Fe1 C1 C5 C4 . . . . 59.01(9) ?
C2 C1 C5 Fe1 . . . . -59.08(10) ?
C3 C4 C5 C1 . . . . -0.10(15) ?
Fe1 C4 C5 C1 . . . . -59.10(10) ?
C3 C4 C5 Fe1 . . . . 59.00(9) ?
C2 Fe1 C5 C1 4_755 . . . -76.28(9) ?
C2 Fe1 C5 C1 . . . . 37.86(8) ?
C4 Fe1 C5 C1 . . . . 119.54(11) ?
C4 Fe1 C5 C1 4_755 . . . -160.77(7) ?
C1 Fe1 C5 C1 4_755 . . . -41.8(2) ?
C5 Fe1 C5 C1 4_755 . . . 165.22(8) ?
C3 Fe1 C5 C1 . . . . 82.14(8) ?
C3 Fe1 C5 C1 4_755 . . . -118.66(8) ?
C2 Fe1 C5 C4 4_755 . . . 164.18(8) ?
C2 Fe1 C5 C4 . . . . -81.67(8) ?
C4 Fe1 C5 C4 4_755 . . . 79.69(11) ?
C1 Fe1 C5 C4 4_755 . . . -161.38(13) ?
C1 Fe1 C5 C4 . . . . -119.54(11) ?
C5 Fe1 C5 C4 4_755 . . . 45.68(7) ?
C3 Fe1 C5 C4 . . . . -37.39(8) ?
C3 Fe1 C5 C4 4_755 . . . 121.81(8) ?
C3 Si1 C8 C9 . . . . -65.20(10) ?
C6 Si1 C8 C9 . . . . 54.46(11) ?
C7 Si1 C8 C9 . . . . 176.22(9) ?
C3 Si1 C8 C10 . . . . 54.48(10) ?
C6 Si1 C8 C10 . . . . 174.14(9) ?
C7 Si1 C8 C10 . . . . -64.10(11) ?
C3 Si1 C8 C11 . . . . 174.68(9) ?
C6 Si1 C8 C11 . . . . -65.67(11) ?
C7 Si1 C8 C11 . . . . 56.09(11) ?
_iucr_refine_instructions_details
;
TITL pbcn Pbcn R = 0.03
CELL 0.71073 7.1282 12.1466 26.3630 90.000 90.000 90.000
ZERR 4 0.0006 0.0010 0.0020 0.000 0.000 0.000
LATT 1
SYMM 0.50000 - X , 0.50000 - Y , 0.50000 + Z
SYMM 0.50000 + X , 0.50000 - Y , - Z
SYMM - X , Y , 0.50000 - Z
SFAC C H Fe Si
UNIT 88 152 4 8
TEMP -173
L.S. 10
FMAP 2
PLAN -20
ACTA
BOND $H
CONF
WGHT 0.0312 1.1338
FVAR 0.13534
FE1 3 1.000000 0.039157 0.250000 10.50000 0.01172 0.01365 =
0.01008 0.00000 -0.00130 0.00000
SI1 4 0.965010 0.117653 0.122364 11.00000 0.01328 0.01321 =
0.01173 0.00000 -0.00074 -0.00049
C1 1 0.748558 -0.042250 0.248659 11.00000 0.01866 0.02791 =
0.01700 0.00317 -0.00309 -0.01000
AFIX 43
H1 2 0.716132 -0.105137 0.268208 11.00000 -1.20000
AFIX 0
C2 1 0.833829 -0.043201 0.199699 11.00000 0.02124 0.01888 =
0.01424 -0.00031 -0.00385 -0.00597
AFIX 43
H2 2 0.867430 -0.107222 0.181100 11.00000 -1.20000
AFIX 0
C3 1 0.860705 0.068551 0.183048 11.00000 0.01302 0.01681 =
0.01297 -0.00038 -0.00417 -0.00096
C4 1 0.788556 0.137063 0.223178 11.00000 0.01355 0.02210 =
0.01459 -0.00092 -0.00300 0.00363
AFIX 43
H4 2 0.786611 0.215265 0.223049 11.00000 -1.20000
AFIX 0
C5 1 0.720760 0.068907 0.262989 11.00000 0.01073 0.03390 =
0.01446 -0.00092 -0.00096 0.00041
AFIX 43
H5 2 0.666282 0.093629 0.293841 11.00000 -1.20000
AFIX 0
C6 1 1.143318 0.016541 0.099248 11.00000 0.01749 0.02177 =
0.02019 -0.00217 0.00024 0.00210
AFIX 33
H6A 2 1.244633 0.010252 0.124208 11.00000 -1.50000
H6B 2 1.194939 0.041864 0.066830 11.00000 -1.50000
H6C 2 1.083850 -0.055496 0.094588 11.00000 -1.50000
AFIX 0
C7 1 1.075210 0.255618 0.133174 11.00000 0.02172 0.01792 =
0.02115 0.00044 -0.00160 -0.00344
AFIX 33
H7A 2 1.176360 0.248629 0.158144 11.00000 -1.50000
H7B 2 0.980330 0.307079 0.145884 11.00000 -1.50000
H7C 2 1.126613 0.283349 0.101152 11.00000 -1.50000
AFIX 0
C8 1 0.768254 0.129999 0.073955 11.00000 0.01710 0.01774 =
0.01210 0.00114 -0.00116 0.00054
C9 1 0.687734 0.015243 0.062707 11.00000 0.02362 0.02454 =
0.02128 -0.00214 -0.00793 -0.00336
AFIX 33
H9A 2 0.586395 0.021609 0.037758 11.00000 -1.50000
H9B 2 0.638407 -0.016961 0.094073 11.00000 -1.50000
H9D 2 0.787036 -0.032119 0.049116 11.00000 -1.50000
AFIX 0
C10 1 0.611066 0.203562 0.094961 11.00000 0.01846 0.02712 =
0.01791 0.00217 -0.00185 0.00514
AFIX 33
H10A 2 0.510325 0.209497 0.069813 11.00000 -1.50000
H10D 2 0.661306 0.276981 0.102242 11.00000 -1.50000
H10B 2 0.561303 0.171129 0.126226 11.00000 -1.50000
AFIX 0
C11 1 0.841878 0.180684 0.024291 11.00000 0.02438 0.03093 =
0.01457 0.00428 0.00094 0.00289
AFIX 33
H11D 2 0.738882 0.186445 -0.000189 11.00000 -1.50000
H11A 2 0.940947 0.133720 0.010287 11.00000 -1.50000
H11B 2 0.892684 0.254161 0.031150 11.00000 -1.50000
HKLF 4
;