Supplementary Material (ESI) for Dalton Transactions This journal is (c) the Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Trans.' loop_ _publ_author_name 'Genge, Anthony R. J.' 'Hill, Nicholas J.' 'Levason, W.' 'Reid, G.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Prof. W. Levason' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for the crystal structure of [Bi2I6{o-C6H4(AsMe2)2}2] included in manuscript number B010179F. ; _publ_contact_author_phone ' 02380 593792 ' _publ_contact_author_fax ' 02380 593781 ' _publ_contact_author_email ' wxl@soton.ac.uk ' _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; data_bidiars_BiI3_+_diars _database_code_CSD 155952 #------------------------------------------------------------------------------ _audit_creation_date '19101-01-03' _audit_creation_method 'by teXsan v1.8' #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 9.009(5) _cell_length_b 12.620(4) _cell_length_c 16.765(3) _cell_angle_alpha 90 _cell_angle_beta 90.98(2) _cell_angle_gamma 90 _cell_volume 1906(1) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.3 _cell_measurement_theta_max 8.9 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'lathe' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 3.052 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 875.77 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H16 As2 Bi I3 ' _chemical_formula_moiety 'C10 H16 As2 Bi I3 ' _chemical_formula_structural [Bi2I6{o-C6H4(AsMe2)2}2] _chemical_compound_source ? _exptl_crystal_F_000 1536.00 _exptl_absorpt_coefficient_mu 17.459 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; DIFABS (Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.622 _exptl_special_details ; The scan width was (1.21+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.59 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -1 -3 -2 -2 -5 1 1 -6 _diffrn_reflns_number 3754 _reflns_number_total 3522 _reflns_number_gt 1941 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.12269 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02447 _diffrn_orient_matrix_UB_12 -0.04741 _diffrn_orient_matrix_UB_13 -0.04572 _diffrn_orient_matrix_UB_21 -0.06425 _diffrn_orient_matrix_UB_22 -0.05673 _diffrn_orient_matrix_UB_23 0.02270 _diffrn_orient_matrix_UB_31 -0.08716 _diffrn_orient_matrix_UB_32 0.02851 _diffrn_orient_matrix_UB_33 -0.03087 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 40 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 64 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; As 0 8 -0.030 2.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; I 0 12 -0.726 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Bi 0 4 -4.861 10.559 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Bi(1) 0.11840(7) 0.08878(5) 0.10016(3) 0.0216(2) 1.000 . Uani d ? I(1) 0.4340(1) 0.1069(1) 0.15710(6) 0.0325(3) 1.000 . Uani d ? I(2) -0.1854(1) 0.12273(9) 0.01216(7) 0.0334(3) 1.000 . Uani d ? I(3) -0.0391(1) 0.0282(1) 0.25190(7) 0.0392(4) 1.000 . Uani d ? As(1) 0.0905(2) 0.2952(1) 0.15955(9) 0.0233(4) 1.000 . Uani d ? As(2) 0.2224(2) 0.2303(1) -0.02920(9) 0.0234(4) 1.000 . Uani d ? C(1) 0.197(2) 0.320(1) 0.2597(8) 0.024(4) 1.000 . Uani d ? C(2) -0.107(2) 0.343(1) 0.182(1) 0.037(5) 1.000 . Uani d ? C(3) 0.173(2) 0.399(1) 0.0882(9) 0.027(5) 1.000 . Uani d ? C(4) 0.179(2) 0.504(1) 0.113(1) 0.039(6) 1.000 . Uani d ? C(5) 0.244(2) 0.582(1) 0.069(1) 0.040(6) 1.000 . Uani d ? C(6) 0.305(2) 0.554(1) -0.004(1) 0.038(6) 1.000 . Uani d ? C(7) 0.300(2) 0.452(1) -0.030(1) 0.034(5) 1.000 . Uani d ? C(8) 0.234(1) 0.374(1) 0.0132(8) 0.020(4) 1.000 . Uani d ? C(9) 0.110(2) 0.255(2) -0.1273(9) 0.041(5) 1.000 . Uani d ? C(10) 0.421(2) 0.210(2) -0.067(1) 0.043(6) 1.000 . Uani d ? H(1) 0.1640 0.2701 0.2998 0.031 1.000 . Uiso c ? H(2) 0.3009 0.3103 0.2537 0.031 1.000 . Uiso c ? H(3) 0.1787 0.3894 0.2791 0.031 1.000 . Uiso c ? H(4) -0.1101 0.4130 0.1974 0.045 1.000 . Uiso c ? H(5) -0.1721 0.3311 0.1363 0.045 1.000 . Uiso c ? H(6) -0.1485 0.2990 0.2250 0.045 1.000 . Uiso c ? H(7) 0.1292 0.5229 0.1617 0.047 1.000 . Uiso c ? H(8) 0.2544 0.6556 0.0892 0.048 1.000 . Uiso c ? H(9) 0.3456 0.6074 -0.0378 0.047 1.000 . Uiso c ? H(10) 0.3450 0.4336 -0.0772 0.036 1.000 . Uiso c ? H(11) 0.0134 0.2879 -0.1158 0.053 1.000 . Uiso c ? H(12) 0.1598 0.3058 -0.1613 0.053 1.000 . Uiso c ? H(13) 0.0914 0.1932 -0.1565 0.053 1.000 . Uiso c ? H(14) 0.4376 0.1418 -0.0869 0.044 1.000 . Uiso c ? H(15) 0.4483 0.2621 -0.1050 0.044 1.000 . Uiso c ? H(16) 0.4939 0.2195 -0.0213 0.044 1.000 . Uiso c ? 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 Bi(1) 0.0234(3) 0.0197(3) 0.0217(3) 0.0000(3) 0.0001(2) -0.0015(3) I(1) 0.0246(6) 0.0395(8) 0.0333(6) 0.0007(5) -0.0029(4) 0.0054(5) I(2) 0.0241(6) 0.0330(7) 0.0430(7) 0.0066(5) -0.0056(5) -0.0107(6) I(3) 0.0475(8) 0.0385(8) 0.0318(6) -0.0065(6) 0.0110(5) 0.0025(6) As(1) 0.0280(9) 0.023(1) 0.0193(8) 0.0031(8) 0.0012(7) -0.0019(7) As(2) 0.0251(8) 0.026(1) 0.0188(8) 0.0003(7) 0.0018(6) -0.0020(7) C(1) 0.029(9) 0.04(1) 0.007(7) 0.004(8) -0.006(6) -0.008(7) C(2) 0.05(1) 0.02(1) 0.04(1) 0.014(9) -0.009(9) -0.008(8) C(3) 0.034(9) 0.02(1) 0.025(9) -0.002(8) -0.013(7) 0.007(8) C(4) 0.06(1) 0.03(1) 0.026(9) 0.00(1) -0.005(8) 0.004(9) C(5) 0.06(1) 0.02(1) 0.04(1) 0.003(9) 0.006(9) 0.01(1) C(6) 0.04(1) 0.04(1) 0.04(1) -0.015(9) -0.011(9) 0.020(9) C(7) 0.05(1) 0.03(1) 0.029(9) -0.013(9) 0.006(8) -0.003(8) C(8) 0.012(7) 0.03(1) 0.018(8) 0.000(7) 0.001(6) 0.002(7) C(9) 0.06(1) 0.05(1) 0.017(8) 0.00(1) -0.019(8) -0.005(8) C(10) 0.05(1) 0.04(1) 0.04(1) 0.01(1) 0.012(9) -0.01(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00008|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 1941 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0375 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_shift/su_max 0.0160 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.09 _refine_diff_density_max 1.21 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi(1) I(1) 2.992(2) . . yes Bi(1) I(2) 3.117(2) . . yes Bi(1) I(2*) 3.328(1) . 3 yes Bi(1) I(3) 3.032(1) . . yes Bi(1) As(1) 2.801(2) . . yes Bi(1) As(2) 2.974(2) . . yes As(1) C(1) 1.94(1) . . yes As(1) C(2) 1.92(2) . . yes As(1) C(3) 1.93(2) . . yes As(2) C(8) 1.95(2) . . yes As(2) C(9) 1.94(1) . . yes As(2) C(10) 1.93(2) . . yes C(1) H(1) 0.97 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.95 . . no C(2) H(4) 0.93 . . no C(2) H(5) 0.96 . . no C(2) H(6) 0.99 . . no C(3) C(4) 1.38(2) . . yes C(3) C(8) 1.42(2) . . yes C(4) C(5) 1.36(2) . . yes C(4) H(7) 0.98 . . no C(5) C(6) 1.40(2) . . yes C(5) H(8) 0.99 . . no C(6) C(7) 1.36(2) . . yes C(6) H(9) 0.96 . . no C(7) C(8) 1.36(2) . . yes C(7) H(10) 0.93 . . no C(9) H(11) 0.98 . . no C(9) H(12) 0.97 . . no C(9) H(13) 0.94 . . no C(10) H(14) 0.93 . . no C(10) H(15) 0.95 . . no C(10) H(16) 1.01 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I(1) Bi(1) I(2) 164.24(4) . . . yes I(1) Bi(1) I(2*) 93.51(4) . . 3 yes I(1) Bi(1) I(3) 101.97(4) . . . yes I(1) Bi(1) As(1) 84.60(4) . . . yes I(1) Bi(1) As(2) 82.95(4) . . . yes I(2) Bi(1) I(2) 90.50(3) . . 3 yes I(2) Bi(1) I(3) 90.69(4) . . . yes I(2) Bi(1) As(1) 87.54(4) . . . yes I(2) Bi(1) As(2) 81.79(5) . . . yes I(2) Bi(1) I(3) 111.39(4) 3 . . yes I(2) Bi(1) As(1) 164.83(4) 3 . . yes I(2) Bi(1) As(2) 90.39(4) 3 . . yes I(3) Bi(1) As(1) 83.68(4) . . . yes I(3) Bi(1) As(2) 157.09(5) . . . yes As(1) Bi(1) As(2) 74.45(5) . . . yes Bi(1) I(2) Bi(1) 89.50(3) . . 3 yes Bi(1) As(1) C(1) 114.3(5) . . . yes Bi(1) As(1) C(2) 116.5(5) . . . yes Bi(1) As(1) C(3) 111.9(5) . . . yes C(1) As(1) C(2) 103.2(6) . . . yes C(1) As(1) C(3) 103.7(6) . . . yes C(2) As(1) C(3) 106.0(7) . . . yes Bi(1) As(2) C(8) 108.0(4) . . . yes Bi(1) As(2) C(9) 123.3(6) . . . yes Bi(1) As(2) C(10) 117.9(6) . . . yes C(8) As(2) C(9) 100.4(7) . . . yes C(8) As(2) C(10) 101.6(7) . . . yes C(9) As(2) C(10) 102.4(8) . . . yes As(1) C(1) H(1) 110.1 . . . no As(1) C(1) H(2) 111.0 . . . no As(1) C(1) H(3) 111.2 . . . no H(1) C(1) H(2) 107.4 . . . no H(1) C(1) H(3) 107.9 . . . no H(2) C(1) H(3) 109.1 . . . no As(1) C(2) H(4) 112.5 . . . no As(1) C(2) H(5) 110.8 . . . no As(1) C(2) H(6) 109.2 . . . no H(4) C(2) H(5) 110.5 . . . no H(4) C(2) H(6) 107.9 . . . no H(5) C(2) H(6) 105.5 . . . no As(1) C(3) C(4) 119(1) . . . yes As(1) C(3) C(8) 124(1) . . . yes C(4) C(3) C(8) 117(2) . . . yes C(3) C(4) C(5) 123(2) . . . yes C(3) C(4) H(7) 118.0 . . . no C(5) C(4) H(7) 118.5 . . . no C(4) C(5) C(6) 117(2) . . . yes C(4) C(5) H(8) 122.9 . . . no C(6) C(5) H(8) 119.5 . . . no C(5) C(6) C(7) 121(2) . . . yes C(5) C(6) H(9) 120.2 . . . no C(7) C(6) H(9) 119.1 . . . no C(6) C(7) C(8) 122(2) . . . yes C(6) C(7) H(10) 119.6 . . . no C(8) C(7) H(10) 118.8 . . . no As(2) C(8) C(3) 121(1) . . . yes As(2) C(8) C(7) 120(1) . . . yes C(3) C(8) C(7) 120(2) . . . yes As(2) C(9) H(11) 110.6 . . . no As(2) C(9) H(12) 111.3 . . . no As(2) C(9) H(13) 113.1 . . . no H(11) C(9) H(12) 105.0 . . . no H(11) C(9) H(13) 107.6 . . . no H(12) C(9) H(13) 108.7 . . . no As(2) C(10) H(14) 113.1 . . . no As(2) C(10) H(15) 112.4 . . . no As(2) C(10) H(16) 108.9 . . . no H(14) C(10) H(15) 111.3 . . . no H(14) C(10) H(16) 105.8 . . . no H(15) C(10) H(16) 104.9 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(6) C(7) 3.59(2) . 3_665 no #------------------------------------------------------------------------------ data_nhbicl3_Bi(oPh(OPPh2)2)Cl3(thf) _database_code_CSD 155953 #------------------------------------------------------------------------------ _audit_creation_date '19101-01-03' _audit_creation_method 'by teXsan v1.8' #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 12.043(2) _cell_length_b 19.467(2) _cell_length_c 14.530(2) _cell_angle_alpha 90 _cell_angle_beta 101.80(2) _cell_angle_gamma 90 _cell_volume 3334.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150.2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.0 _cell_measurement_theta_max 8.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 861.88 _chemical_formula_analytical ? _chemical_formula_sum 'C34 H28 Bi Cl3 O3 P2 ' _chemical_formula_moiety 'C34 H28 Bi Cl3 O3 P2 ' _chemical_formula_structural [BiCl3(thf){o-C6H4(PPh2)2}] _chemical_compound_source ? _exptl_crystal_F_000 1680.00 _exptl_absorpt_coefficient_mu 5.647 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.865 _exptl_special_details ; The scan width was (1.31+0.35tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.2 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.09 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -6 -2 2 -4 -4 2 -2 -5 _diffrn_reflns_number 6374 _reflns_number_total 6074 _reflns_number_gt 3648 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.04400 _diffrn_reflns_av_sigmaI/netI 0.110 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.06510 _diffrn_orient_matrix_UB_12 -0.03183 _diffrn_orient_matrix_UB_13 -0.00027 _diffrn_orient_matrix_UB_21 -0.01578 _diffrn_orient_matrix_UB_22 -0.02365 _diffrn_orient_matrix_UB_23 0.05706 _diffrn_orient_matrix_UB_31 -0.05204 _diffrn_orient_matrix_UB_32 -0.03265 _diffrn_orient_matrix_UB_33 -0.04107 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 136 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 112 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Bi 0 4 -4.861 10.559 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 12 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 12 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Bi(1) 0.12618(3) 0.12832(2) 0.28466(2) 0.02405(7) 1.000 . Uani d ? Cl(1) 0.1420(2) 0.1369(1) 0.1149(1) 0.0359(6) 1.000 . Uani d ? Cl(2) 0.2656(2) 0.2296(1) 0.3229(2) 0.0437(7) 1.000 . Uani d ? Cl(3) -0.0635(2) 0.1950(1) 0.2663(2) 0.0392(7) 1.000 . Uani d ? P(1) 0.3425(2) -0.0133(1) 0.2777(1) 0.0243(6) 1.000 . Uani d ? P(2) 0.0515(2) -0.0503(1) 0.2222(2) 0.0265(6) 1.000 . Uani d ? O(1) 0.2686(5) 0.0355(3) 0.3176(4) 0.027(2) 1.000 . Uani d ? O(2) 0.0207(5) 0.0237(3) 0.2304(4) 0.035(2) 1.000 . Uani d ? O(3) 0.1404(5) 0.1392(3) 0.4726(4) 0.039(2) 1.000 . Uani d ? C(1) 0.2691(7) -0.0525(4) 0.1680(6) 0.027(2) 1.000 . Uani d ? C(2) 0.1520(7) -0.0670(4) 0.1455(5) 0.023(2) 1.000 . Uani d ? C(3) 0.1067(7) -0.0949(4) 0.0579(6) 0.033(3) 1.000 . Uani d ? C(4) 0.1761(8) -0.1104(5) -0.0052(6) 0.040(3) 1.000 . Uani d ? C(5) 0.2898(8) -0.0982(5) 0.0172(6) 0.035(3) 1.000 . Uani d ? C(6) 0.3360(7) -0.0692(5) 0.1032(6) 0.034(3) 1.000 . Uani d ? C(7) 0.4630(7) 0.0315(4) 0.2515(5) 0.023(2) 1.000 . Uani d ? C(8) 0.4464(7) 0.0955(5) 0.2094(6) 0.037(3) 1.000 . Uani d ? C(9) 0.5379(8) 0.1351(5) 0.1963(7) 0.043(3) 1.000 . Uani d ? C(10) 0.6470(8) 0.1111(5) 0.2243(6) 0.040(3) 1.000 . Uani d ? C(11) 0.6644(7) 0.0468(5) 0.2650(6) 0.038(3) 1.000 . Uani d ? C(12) 0.5736(8) 0.0067(4) 0.2796(6) 0.034(3) 1.000 . Uani d ? C(13) 0.3961(7) -0.0802(4) 0.3598(6) 0.024(2) 1.000 . Uani d ? C(14) 0.4327(7) -0.1436(4) 0.3327(6) 0.029(3) 1.000 . Uani d ? C(15) 0.4754(7) -0.1923(4) 0.3986(6) 0.032(3) 1.000 . Uani d ? C(16) 0.4851(8) -0.1782(5) 0.4924(6) 0.036(3) 1.000 . Uani d ? C(17) 0.4503(8) -0.1171(5) 0.5210(6) 0.039(3) 1.000 . Uani d ? C(18) 0.4059(7) -0.0663(4) 0.4550(6) 0.033(3) 1.000 . Uani d ? C(19) -0.0767(7) -0.0968(5) 0.1704(6) 0.030(3) 1.000 . Uani d ? C(20) -0.0819(8) -0.1688(5) 0.1730(7) 0.039(3) 1.000 . Uani d ? C(21) -0.1853(9) -0.2005(5) 0.1371(7) 0.048(3) 1.000 . Uani d ? C(22) -0.2812(8) -0.1635(6) 0.1015(7) 0.048(4) 1.000 . Uani d ? C(23) -0.2736(8) -0.0931(6) 0.0976(8) 0.048(4) 1.000 . Uani d ? C(24) -0.1728(8) -0.0597(5) 0.1335(7) 0.038(3) 1.000 . Uani d ? C(25) 0.1036(7) -0.0897(4) 0.3334(6) 0.024(2) 1.000 . Uani d ? C(26) 0.0824(7) -0.0568(4) 0.4138(6) 0.029(2) 1.000 . Uani d ? C(27) 0.1116(8) -0.0887(5) 0.5001(6) 0.035(3) 1.000 . Uani d ? C(28) 0.1616(8) -0.1522(5) 0.5098(6) 0.038(3) 1.000 . Uani d ? C(29) 0.1841(7) -0.1858(4) 0.4308(6) 0.032(3) 1.000 . Uani d ? C(30) 0.1545(6) -0.1545(4) 0.3432(6) 0.026(2) 1.000 . Uani d ? C(31) 0.125(1) 0.2067(5) 0.5101(8) 0.057(4) 1.000 . Uani d ? C(32) 0.186(1) 0.2091(7) 0.5982(9) 0.136(6) 1.000 . Uani d ? C(33) 0.2373(9) 0.1419(5) 0.6288(6) 0.049(3) 1.000 . Uani d ? C(34) 0.2284(8) 0.1043(5) 0.5371(7) 0.045(3) 1.000 . Uani d ? H(1) 0.0276 -0.1035 0.0408 0.039 1.000 . Uiso c ? H(2) 0.1436 -0.1296 -0.0647 0.048 1.000 . Uiso c ? H(3) 0.3368 -0.1096 -0.0257 0.042 1.000 . Uiso c ? H(4) 0.4152 -0.0604 0.1186 0.041 1.000 . Uiso c ? H(5) 0.3715 0.1125 0.1891 0.045 1.000 . Uiso c ? H(6) 0.5249 0.1791 0.1680 0.052 1.000 . Uiso c ? H(7) 0.7095 0.1383 0.2157 0.048 1.000 . Uiso c ? H(8) 0.7395 0.0296 0.2835 0.045 1.000 . Uiso c ? H(9) 0.5868 -0.0372 0.3083 0.041 1.000 . Uiso c ? H(10) 0.4281 -0.1531 0.2679 0.035 1.000 . Uiso c ? H(11) 0.4982 -0.2358 0.3794 0.038 1.000 . Uiso c ? H(12) 0.5166 -0.2116 0.5379 0.044 1.000 . Uiso c ? H(13) 0.4560 -0.1085 0.5862 0.047 1.000 . Uiso c ? H(14) 0.3829 -0.0231 0.4752 0.040 1.000 . Uiso c ? H(15) -0.0166 -0.1952 0.1986 0.047 1.000 . Uiso c ? H(16) -0.1894 -0.2492 0.1372 0.058 1.000 . Uiso c ? H(17) -0.3516 -0.1861 0.0799 0.057 1.000 . Uiso c ? H(18) -0.3386 -0.0671 0.0698 0.058 1.000 . Uiso c ? H(19) -0.1698 -0.0109 0.1326 0.045 1.000 . Uiso c ? H(20) 0.0480 -0.0127 0.4089 0.035 1.000 . Uiso c ? H(21) 0.0968 -0.0660 0.5542 0.042 1.000 . Uiso c ? H(22) 0.1808 -0.1732 0.5699 0.045 1.000 . Uiso c ? H(23) 0.2193 -0.2297 0.4369 0.039 1.000 . Uiso c ? H(24) 0.1692 -0.1775 0.2893 0.031 1.000 . Uiso c ? H(25) 0.0793 0.2426 0.4781 0.066 1.000 . Uiso c ? H(26) 0.1960 0.2493 0.6361 0.162 1.000 . Uiso c ? H(27) 0.2679 0.1264 0.6906 0.057 1.000 . Uiso c ? H(28) 0.2715 0.0659 0.5247 0.053 1.000 . Uiso c ? 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 Bi(1) 0.0257(2) 0.0223(1) 0.0242(1) -0.0013(2) 0.0052(1) 0.0010(2) Cl(1) 0.037(1) 0.045(1) 0.026(1) 0.001(1) 0.0077(9) 0.001(1) Cl(2) 0.045(2) 0.038(1) 0.045(1) -0.016(1) 0.002(1) 0.007(1) Cl(3) 0.030(1) 0.051(2) 0.038(1) 0.006(1) 0.012(1) 0.007(1) P(1) 0.025(1) 0.025(1) 0.023(1) -0.004(1) 0.0061(9) -0.003(1) P(2) 0.028(1) 0.022(1) 0.029(1) -0.002(1) 0.006(1) -0.002(1) O(1) 0.035(4) 0.022(3) 0.025(3) 0.001(3) 0.009(3) 0.000(3) O(2) 0.037(4) 0.029(3) 0.039(4) -0.005(3) 0.008(3) -0.005(3) O(3) 0.046(4) 0.039(4) 0.034(4) -0.004(3) 0.014(3) -0.007(3) C(1) 0.039(5) 0.018(4) 0.026(5) -0.003(4) 0.010(4) -0.001(4) C(2) 0.027(5) 0.017(4) 0.023(4) -0.003(4) 0.002(4) 0.004(4) C(3) 0.036(5) 0.035(5) 0.025(5) -0.004(4) 0.000(4) -0.007(4) C(4) 0.054(6) 0.041(6) 0.027(5) -0.009(5) 0.014(4) -0.007(4) C(5) 0.039(6) 0.048(6) 0.023(5) -0.005(5) 0.018(4) -0.014(4) C(6) 0.030(5) 0.040(6) 0.029(5) -0.007(4) 0.003(4) -0.004(4) C(7) 0.024(4) 0.025(5) 0.024(4) -0.004(4) 0.011(4) -0.009(4) C(8) 0.027(5) 0.042(6) 0.048(6) -0.010(4) 0.017(4) 0.021(5) C(9) 0.040(6) 0.035(6) 0.057(6) -0.009(5) 0.016(5) 0.015(5) C(10) 0.039(6) 0.044(6) 0.042(6) -0.011(5) 0.015(5) 0.005(5) C(11) 0.022(5) 0.055(7) 0.039(6) -0.001(5) 0.012(4) -0.011(5) C(12) 0.041(5) 0.025(5) 0.040(5) 0.003(4) 0.016(5) 0.004(4) C(13) 0.019(4) 0.025(5) 0.028(5) -0.003(4) 0.006(4) -0.001(4) C(14) 0.030(5) 0.034(6) 0.026(5) -0.009(4) 0.011(4) -0.012(4) C(15) 0.036(5) 0.017(5) 0.044(6) -0.002(4) 0.014(4) -0.002(4) C(16) 0.036(6) 0.036(6) 0.035(5) 0.005(4) 0.002(4) 0.001(4) C(17) 0.046(6) 0.048(7) 0.024(5) 0.010(5) 0.006(4) 0.004(5) C(18) 0.037(6) 0.029(5) 0.035(5) 0.001(4) 0.010(4) -0.006(4) C(19) 0.031(5) 0.034(5) 0.024(5) -0.003(4) 0.003(4) -0.007(4) C(20) 0.043(6) 0.029(6) 0.044(6) -0.012(5) 0.006(5) -0.011(5) C(21) 0.056(7) 0.036(6) 0.052(7) -0.022(5) 0.009(6) -0.015(5) C(22) 0.032(6) 0.059(8) 0.057(7) -0.014(6) 0.017(5) -0.011(6) C(23) 0.029(6) 0.060(8) 0.056(8) -0.001(5) 0.008(5) -0.010(6) C(24) 0.028(5) 0.040(6) 0.044(6) -0.003(5) 0.007(5) -0.009(5) C(25) 0.024(5) 0.019(5) 0.029(5) -0.002(4) 0.009(4) 0.001(4) C(26) 0.024(5) 0.032(5) 0.030(5) 0.010(4) 0.003(4) 0.005(4) C(27) 0.034(5) 0.038(6) 0.036(6) 0.008(4) 0.019(4) -0.007(5) C(28) 0.041(6) 0.046(6) 0.030(5) 0.008(5) 0.015(5) 0.014(4) C(29) 0.030(5) 0.024(5) 0.047(6) 0.003(4) 0.018(4) 0.008(4) C(30) 0.019(5) 0.028(5) 0.031(5) -0.006(4) 0.007(4) -0.003(4) C(31) 0.083(9) 0.030(6) 0.057(7) 0.011(6) 0.015(6) -0.014(5) C(32) 0.20(2) 0.08(1) 0.08(1) 0.09(1) -0.09(1) -0.060(8) C(33) 0.058(7) 0.061(8) 0.023(5) 0.021(6) -0.001(5) -0.007(5) C(34) 0.050(6) 0.034(6) 0.046(6) 0.021(5) 0.000(5) -0.009(5) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 3648 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_all 0.0334 _refine_ls_wR_factor_ref 0.0334 _refine_ls_goodness_of_fit_all 1.267 _refine_ls_goodness_of_fit_ref 1.267 _refine_ls_shift/su_max 0.0200 _refine_ls_shift/su_mean 0.0100 _refine_diff_density_min -0.82 _refine_diff_density_max 1.02 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi(1) Cl(1) 2.518(2) . . yes Bi(1) Cl(2) 2.576(2) . . yes Bi(1) Cl(3) 2.593(2) . . yes Bi(1) O(1) 2.470(5) . . yes Bi(1) O(2) 2.444(5) . . yes Bi(1) O(3) 2.709(6) . . yes P(1) O(1) 1.497(5) . . yes P(1) C(1) 1.825(8) . . yes P(1) C(7) 1.799(8) . . yes P(1) C(13) 1.793(8) . . yes P(2) O(2) 1.498(6) . . yes P(2) C(2) 1.835(8) . . yes P(2) C(19) 1.816(9) . . yes P(2) C(25) 1.782(8) . . yes O(3) C(31) 1.45(1) . . yes O(3) C(34) 1.43(1) . . yes C(1) C(2) 1.41(1) . . yes C(1) C(6) 1.40(1) . . yes C(2) C(3) 1.39(1) . . yes C(3) C(4) 1.39(1) . . yes C(3) H(1) 0.95 . . no C(4) C(5) 1.36(1) . . yes C(4) H(2) 0.95 . . no C(5) C(6) 1.38(1) . . yes C(5) H(3) 0.95 . . no C(6) H(4) 0.95 . . no C(7) C(8) 1.38(1) . . yes C(7) C(12) 1.40(1) . . yes C(8) C(9) 1.39(1) . . yes C(8) H(5) 0.95 . . no C(9) C(10) 1.38(1) . . yes C(9) H(6) 0.95 . . no C(10) C(11) 1.38(1) . . yes C(10) H(7) 0.95 . . no C(11) C(12) 1.39(1) . . yes C(11) H(8) 0.95 . . no C(12) H(9) 0.95 . . no C(13) C(14) 1.39(1) . . yes C(13) C(18) 1.39(1) . . yes C(14) C(15) 1.37(1) . . yes C(14) H(10) 0.95 . . no C(15) C(16) 1.37(1) . . yes C(15) H(11) 0.95 . . no C(16) C(17) 1.35(1) . . yes C(16) H(12) 0.95 . . no C(17) C(18) 1.40(1) . . yes C(17) H(13) 0.95 . . no C(18) H(14) 0.95 . . no C(19) C(20) 1.40(1) . . yes C(19) C(24) 1.38(1) . . yes C(20) C(21) 1.39(1) . . yes C(20) H(15) 0.95 . . no C(21) C(22) 1.37(1) . . yes C(21) H(16) 0.95 . . no C(22) C(23) 1.38(1) . . yes C(22) H(17) 0.95 . . no C(23) C(24) 1.38(1) . . yes C(23) H(18) 0.95 . . no C(24) H(19) 0.95 . . no C(25) C(26) 1.40(1) . . yes C(25) C(30) 1.40(1) . . yes C(26) C(27) 1.38(1) . . yes C(26) H(20) 0.95 . . no C(27) C(28) 1.37(1) . . yes C(27) H(21) 0.95 . . no C(28) C(29) 1.39(1) . . yes C(28) H(22) 0.95 . . no C(29) C(30) 1.39(1) . . yes C(29) H(23) 0.95 . . no C(30) H(24) 0.95 . . no C(31) C(32) 1.34(1) . . yes C(31) H(25) 0.95 . . no C(32) C(33) 1.47(1) . . yes C(32) H(26) 0.95 . . no C(33) C(34) 1.51(1) . . yes C(33) H(27) 0.95 . . no C(34) H(28) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Bi(1) Cl(2) 89.11(8) . . . yes Cl(1) Bi(1) Cl(3) 96.19(7) . . . yes Cl(1) Bi(1) O(1) 92.9(1) . . . yes Cl(1) Bi(1) O(2) 83.0(1) . . . yes Cl(1) Bi(1) O(3) 168.6(1) . . . yes Cl(2) Bi(1) Cl(3) 99.26(8) . . . yes Cl(2) Bi(1) O(1) 97.0(1) . . . yes Cl(2) Bi(1) O(2) 168.7(1) . . . yes Cl(2) Bi(1) O(3) 79.5(1) . . . yes Cl(3) Bi(1) O(1) 161.5(1) . . . yes Cl(3) Bi(1) O(2) 89.7(1) . . . yes Cl(3) Bi(1) O(3) 86.4(1) . . . yes O(1) Bi(1) O(2) 75.4(2) . . . yes O(1) Bi(1) O(3) 87.9(2) . . . yes O(2) Bi(1) O(3) 108.2(2) . . . yes O(1) P(1) C(1) 112.6(4) . . . yes O(1) P(1) C(7) 110.1(3) . . . yes O(1) P(1) C(13) 111.4(3) . . . yes C(1) P(1) C(7) 106.6(4) . . . yes C(1) P(1) C(13) 108.7(4) . . . yes C(7) P(1) C(13) 107.2(4) . . . yes O(2) P(2) C(2) 115.1(3) . . . yes O(2) P(2) C(19) 108.0(4) . . . yes O(2) P(2) C(25) 112.9(4) . . . yes C(2) P(2) C(19) 105.7(4) . . . yes C(2) P(2) C(25) 108.7(4) . . . yes C(19) P(2) C(25) 105.8(4) . . . yes Bi(1) O(1) P(1) 146.4(3) . . . yes Bi(1) O(2) P(2) 134.9(3) . . . yes Bi(1) O(3) C(31) 117.6(6) . . . yes Bi(1) O(3) C(34) 120.5(5) . . . yes C(31) O(3) C(34) 108.6(7) . . . yes P(1) C(1) C(2) 124.7(6) . . . yes P(1) C(1) C(6) 116.3(6) . . . yes C(2) C(1) C(6) 118.9(8) . . . yes P(2) C(2) C(1) 125.2(6) . . . yes P(2) C(2) C(3) 116.2(6) . . . yes C(1) C(2) C(3) 118.6(8) . . . yes C(2) C(3) C(4) 120.8(8) . . . yes C(2) C(3) H(1) 119.6 . . . no C(4) C(3) H(1) 119.6 . . . no C(3) C(4) C(5) 120.8(8) . . . yes C(3) C(4) H(2) 119.6 . . . no C(5) C(4) H(2) 119.6 . . . no C(4) C(5) C(6) 119.2(8) . . . yes C(4) C(5) H(3) 120.4 . . . no C(6) C(5) H(3) 120.4 . . . no C(1) C(6) C(5) 121.6(8) . . . yes C(1) C(6) H(4) 119.2 . . . no C(5) C(6) H(4) 119.2 . . . no P(1) C(7) C(8) 118.7(6) . . . yes P(1) C(7) C(12) 122.2(6) . . . yes C(8) C(7) C(12) 118.8(8) . . . yes C(7) C(8) C(9) 120.9(8) . . . yes C(7) C(8) H(5) 119.5 . . . no C(9) C(8) H(5) 119.6 . . . no C(8) C(9) C(10) 120.5(9) . . . yes C(8) C(9) H(6) 119.7 . . . no C(10) C(9) H(6) 119.8 . . . no C(9) C(10) C(11) 119.1(8) . . . yes C(9) C(10) H(7) 120.4 . . . no C(11) C(10) H(7) 120.4 . . . no C(10) C(11) C(12) 121.0(8) . . . yes C(10) C(11) H(8) 119.5 . . . no C(12) C(11) H(8) 119.5 . . . no C(7) C(12) C(11) 119.6(8) . . . yes C(7) C(12) H(9) 120.2 . . . no C(11) C(12) H(9) 120.2 . . . no P(1) C(13) C(14) 123.1(6) . . . yes P(1) C(13) C(18) 117.8(6) . . . yes C(14) C(13) C(18) 119.0(8) . . . yes C(13) C(14) C(15) 120.7(8) . . . yes C(13) C(14) H(10) 119.7 . . . no C(15) C(14) H(10) 119.7 . . . no C(14) C(15) C(16) 120.0(8) . . . yes C(14) C(15) H(11) 120.0 . . . no C(16) C(15) H(11) 120.0 . . . no C(15) C(16) C(17) 120.8(8) . . . yes C(15) C(16) H(12) 119.6 . . . no C(17) C(16) H(12) 119.6 . . . no C(16) C(17) C(18) 120.5(8) . . . yes C(16) C(17) H(13) 119.7 . . . no C(18) C(17) H(13) 119.7 . . . no C(13) C(18) C(17) 119.0(8) . . . yes C(13) C(18) H(14) 120.5 . . . no C(17) C(18) H(14) 120.5 . . . no P(2) C(19) C(20) 121.8(7) . . . yes P(2) C(19) C(24) 118.4(7) . . . yes C(20) C(19) C(24) 119.7(9) . . . yes C(19) C(20) C(21) 118(1) . . . yes C(19) C(20) H(15) 120.8 . . . no C(21) C(20) H(15) 120.9 . . . no C(20) C(21) C(22) 122.0(9) . . . yes C(20) C(21) H(16) 119.0 . . . no C(22) C(21) H(16) 119.0 . . . no C(21) C(22) C(23) 119(1) . . . yes C(21) C(22) H(17) 120.6 . . . no C(23) C(22) H(17) 120.7 . . . no C(22) C(23) C(24) 121(1) . . . yes C(22) C(23) H(18) 119.4 . . . no C(24) C(23) H(18) 119.6 . . . no C(19) C(24) C(23) 120.2(9) . . . yes C(19) C(24) H(19) 119.9 . . . no C(23) C(24) H(19) 119.9 . . . no P(2) C(25) C(26) 118.0(6) . . . yes P(2) C(25) C(30) 123.2(6) . . . yes C(26) C(25) C(30) 118.5(8) . . . yes C(25) C(26) C(27) 119.8(8) . . . yes C(25) C(26) H(20) 120.1 . . . no C(27) C(26) H(20) 120.1 . . . no C(26) C(27) C(28) 121.6(8) . . . yes C(26) C(27) H(21) 119.2 . . . no C(28) C(27) H(21) 119.2 . . . no C(27) C(28) C(29) 119.6(8) . . . yes C(27) C(28) H(22) 120.2 . . . no C(29) C(28) H(22) 120.2 . . . no C(28) C(29) C(30) 119.5(8) . . . yes C(28) C(29) H(23) 120.2 . . . no C(30) C(29) H(23) 120.3 . . . no C(25) C(30) C(29) 120.9(8) . . . yes C(25) C(30) H(24) 119.5 . . . no C(29) C(30) H(24) 119.5 . . . no O(3) C(31) C(32) 107.6(9) . . . yes O(3) C(31) H(25) 126.1 . . . no C(32) C(31) H(25) 126.3 . . . no C(31) C(32) C(33) 112(1) . . . yes C(31) C(32) H(26) 124.0 . . . no C(33) C(32) H(26) 124.2 . . . no C(32) C(33) C(34) 102.4(8) . . . yes C(32) C(33) H(27) 128.7 . . . no C(34) C(33) H(27) 128.9 . . . no O(3) C(34) C(33) 104.9(7) . . . yes O(3) C(34) H(28) 127.5 . . . no C(33) C(34) H(28) 127.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(3) 3.588(9) . 3 no Cl(2) C(30) 3.577(8) . 2 no Cl(3) C(15) 3.568(9) . 2 no O(3) C(27) 3.29(1) . 3_556 no C(18) C(18) 3.51(2) . 3_656 no C(28) C(31) 3.57(1) . 3_556 no #------------------------------------------------------------------------------ data_sbclas2_SbCl3_+_Diars _database_code_CSD 155954 #------------------------------------------------------------------------------ _audit_creation_date '19101-01-03' _audit_creation_method 'by teXsan v1.8' #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 8.487(2) _cell_length_b 14.839(4) _cell_length_c 16.866(3) _cell_angle_alpha 90 _cell_angle_beta 98.93(1) _cell_angle_gamma 90 _cell_volume 2098.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.1 _cell_measurement_theta_max 7.9 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'lozenge-shaped crystal' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_diffrn 2.350 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 742.30 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H16 As2 Cl6 Sb2 ' _chemical_formula_moiety 'C10 H16 As2 Cl6 Sb2 ' _chemical_formula_structural '[(SbCl3)2{o-C6H4(AsMe2)2}]' _chemical_compound_source ? _exptl_crystal_F_000 1384.00 _exptl_absorpt_coefficient_mu 6.454 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; DIFABS (Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.650 _exptl_special_details ; The scan width was (1.21+0.35tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.74 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -1 -6 1 -2 -6 -3 -2 0 _diffrn_reflns_number 4129 _reflns_number_total 3855 _reflns_number_gt 3231 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.04672 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.08817 _diffrn_orient_matrix_UB_12 -0.00300 _diffrn_orient_matrix_UB_13 -0.04673 _diffrn_orient_matrix_UB_21 0.05151 _diffrn_orient_matrix_UB_22 0.04953 _diffrn_orient_matrix_UB_23 -0.02704 _diffrn_orient_matrix_UB_31 0.06164 _diffrn_orient_matrix_UB_32 -0.04560 _diffrn_orient_matrix_UB_33 -0.02622 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 40 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 64 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; As 0 8 -0.030 2.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 24 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Sb 0 8 -0.816 1.546 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Sb(1) 0.31294(7) -0.19265(4) 0.30580(4) 0.0166(2) 1.000 . Uani d ? Sb(2) 0.17807(8) 0.05439(4) 0.19263(4) 0.0196(2) 1.000 . Uani d ? As(1) 0.5817(1) -0.10875(6) 0.36720(6) 0.0158(3) 1.000 . Uani d ? As(2) 0.3655(1) -0.27395(6) 0.44827(6) 0.0157(3) 1.000 . Uani d ? Cl(1) 0.5163(3) -0.3097(2) 0.2721(2) 0.0286(7) 1.000 . Uani d ? Cl(2) 0.1865(3) -0.0683(2) 0.3824(2) 0.0290(7) 1.000 . Uani d ? Cl(3) 0.4041(3) -0.0604(2) 0.1747(1) 0.0240(6) 1.000 . Uani d ? Cl(4) 0.1729(3) 0.1013(2) 0.0590(2) 0.0343(8) 1.000 . Uani d ? Cl(5) -0.0075(3) -0.0636(2) 0.1581(2) 0.0328(8) 1.000 . Uani d ? Cl(6) -0.0525(4) 0.1673(2) 0.2031(2) 0.0453(9) 1.000 . Uani d ? C(1) 0.567(1) 0.0181(7) 0.3891(7) 0.032(3) 1.000 . Uani d ? C(2) 0.760(1) -0.1189(8) 0.3094(7) 0.031(3) 1.000 . Uani d ? C(3) 0.655(1) -0.1632(6) 0.4706(5) 0.019(2) 1.000 . Uani d ? C(4) 0.802(1) -0.1350(6) 0.5124(6) 0.020(3) 1.000 . Uani d ? C(5) 0.859(1) -0.1710(7) 0.5858(6) 0.023(3) 1.000 . Uani d ? C(6) 0.772(1) -0.2351(7) 0.6202(6) 0.023(3) 1.000 . Uani d ? C(7) 0.626(1) -0.2641(7) 0.5795(6) 0.022(3) 1.000 . Uani d ? C(8) 0.566(1) -0.2283(6) 0.5031(6) 0.019(3) 1.000 . Uani d ? C(9) 0.383(1) -0.4033(7) 0.4464(6) 0.026(3) 1.000 . Uani d ? C(10) 0.209(1) -0.2497(7) 0.5180(6) 0.028(3) 1.000 . Uani d ? H(1) 0.4934 0.0275 0.4252 0.038 1.000 . Uiso c ? H(2) 0.5326 0.0495 0.3404 0.038 1.000 . Uiso c ? H(3) 0.6693 0.0399 0.4126 0.038 1.000 . Uiso c ? H(4) 0.7328 -0.0926 0.2577 0.038 1.000 . Uiso c ? H(5) 0.8495 -0.0883 0.3380 0.038 1.000 . Uiso c ? H(6) 0.7857 -0.1806 0.3039 0.038 1.000 . Uiso c ? H(7) 0.8621 -0.0906 0.4897 0.024 1.000 . Uiso c ? H(8) 0.9594 -0.1518 0.6135 0.028 1.000 . Uiso c ? H(9) 0.8122 -0.2592 0.6716 0.027 1.000 . Uiso c ? H(10) 0.5658 -0.3080 0.6030 0.026 1.000 . Uiso c ? H(11) 0.2824 -0.4287 0.4260 0.032 1.000 . Uiso c ? H(12) 0.4176 -0.4249 0.4993 0.032 1.000 . Uiso c ? H(13) 0.4587 -0.4201 0.4129 0.032 1.000 . Uiso c ? H(14) 0.2454 -0.2736 0.5698 0.033 1.000 . Uiso c ? H(15) 0.1945 -0.1865 0.5218 0.033 1.000 . Uiso c ? H(16) 0.1105 -0.2771 0.4964 0.033 1.000 . Uiso c ? 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 Sb(1) 0.0188(4) 0.0153(3) 0.0155(4) -0.0007(2) 0.0017(3) 0.0005(2) Sb(2) 0.0221(4) 0.0173(4) 0.0194(4) 0.0022(3) 0.0030(3) -0.0001(3) As(1) 0.0179(5) 0.0156(5) 0.0145(5) -0.0029(4) 0.0042(4) 0.0015(4) As(2) 0.0178(5) 0.0153(5) 0.0150(5) -0.0014(4) 0.0059(4) 0.0005(4) Cl(1) 0.040(2) 0.022(1) 0.027(1) 0.004(1) 0.014(1) -0.002(1) Cl(2) 0.024(1) 0.024(1) 0.040(2) 0.006(1) 0.006(1) -0.004(1) Cl(3) 0.027(1) 0.024(1) 0.023(1) 0.007(1) 0.010(1) 0.005(1) Cl(4) 0.036(2) 0.041(2) 0.027(1) 0.003(1) 0.006(1) 0.016(1) Cl(5) 0.034(2) 0.032(1) 0.033(2) -0.012(1) 0.007(1) -0.001(1) Cl(6) 0.037(2) 0.054(2) 0.041(2) 0.025(1) -0.009(1) -0.019(1) C(1) 0.048(7) 0.013(5) 0.032(6) -0.006(5) 0.001(5) 0.002(5) C(2) 0.025(6) 0.047(7) 0.025(6) -0.006(5) 0.013(5) -0.002(5) C(3) 0.032(6) 0.018(5) 0.009(4) 0.007(4) 0.007(4) -0.001(4) C(4) 0.016(5) 0.022(5) 0.024(5) -0.006(4) 0.005(4) -0.001(4) C(5) 0.019(5) 0.030(6) 0.019(5) -0.002(4) -0.003(4) -0.008(4) C(6) 0.026(6) 0.032(6) 0.011(5) 0.009(4) 0.003(4) 0.002(4) C(7) 0.020(5) 0.023(5) 0.022(5) -0.004(4) 0.005(4) 0.002(4) C(8) 0.033(6) 0.011(4) 0.015(5) 0.004(4) 0.011(4) -0.002(4) C(9) 0.033(6) 0.022(5) 0.024(6) 0.003(4) 0.007(5) 0.007(4) C(10) 0.026(6) 0.034(6) 0.027(6) -0.003(5) 0.017(5) 0.000(5) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00007|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 3231 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_all 0.0655 _refine_ls_wR_factor_ref 0.0655 _refine_ls_goodness_of_fit_all 3.188 _refine_ls_goodness_of_fit_ref 3.188 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -2.40 _refine_diff_density_max 1.40 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb(1) As(1) 2.663(1) . . yes Sb(1) As(2) 2.664(1) . . yes Sb(1) Cl(1) 2.573(2) . . yes Sb(1) Cl(2) 2.580(2) . . yes Sb(1) Cl(3) 3.141(2) . . yes Sb(1) Cl(6) 3.020(3) . 2_545 yes Sb(2) Cl(3) 2.618(2) . . yes Sb(2) Cl(4) 2.352(3) . . yes Sb(2) Cl(5) 2.366(3) . . yes Sb(2) Cl(6) 2.603(3) . . yes As(1) C(1) 1.93(1) . . yes As(1) C(2) 1.93(1) . . yes As(1) C(3) 1.936(9) . . yes As(2) C(8) 1.93(1) . . yes As(2) C(9) 1.93(1) . . yes As(2) C(10) 1.939(9) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.95 . . no C(2) H(4) 0.95 . . no C(2) H(5) 0.95 . . no C(2) H(6) 0.95 . . no C(3) C(4) 1.39(1) . . yes C(3) C(8) 1.39(1) . . yes C(4) C(5) 1.37(1) . . yes C(4) H(7) 0.95 . . no C(5) C(6) 1.39(1) . . yes C(5) H(8) 0.95 . . no C(6) C(7) 1.39(1) . . yes C(6) H(9) 0.95 . . no C(7) C(8) 1.41(1) . . yes C(7) H(10) 0.95 . . no C(9) H(11) 0.95 . . no C(9) H(12) 0.95 . . no C(9) H(13) 0.95 . . no C(10) H(14) 0.95 . . no C(10) H(15) 0.95 . . no C(10) H(16) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag As(1) Sb(1) As(2) 81.23(3) . . . yes As(1) Sb(1) Cl(1) 80.69(7) . . . yes As(1) Sb(1) Cl(2) 82.45(6) . . . yes As(1) Sb(1) Cl(3) 72.06(5) . . . yes As(1) Sb(1) Cl(6) 156.49(6) . . 2_545 yes As(2) Sb(1) Cl(1) 82.51(6) . . . yes As(2) Sb(1) Cl(2) 84.07(7) . . . yes As(2) Sb(1) Cl(3) 153.21(6) . . . yes As(2) Sb(1) Cl(6*) 75.65(6) . . 2_545 yes Cl(1) Sb(1) Cl(2) 159.84(9) . . . yes Cl(1) Sb(1) Cl(3) 91.08(7) . . . yes Cl(1) Sb(1) Cl(6*) 92.04(9) . . 2_545 yes Cl(2) Sb(1) Cl(3) 94.17(7) . . . yes Cl(2) Sb(1) Cl(6*) 99.14(9) . . 2_545 yes Cl(3) Sb(1) Cl(6*) 130.77(8) . . 2_545 yes Cl(3) Sb(2) Cl(4) 89.27(9) . . . yes Cl(3) Sb(2) Cl(5) 87.83(9) . . . yes Cl(3) Sb(2) Cl(6) 177.20(9) . . . yes Cl(4) Sb(2) Cl(5) 94.1(1) . . . yes Cl(4) Sb(2) Cl(6) 88.4(1) . . . yes Cl(5) Sb(2) Cl(6) 90.8(1) . . . yes Sb(1) As(1) C(1) 117.1(4) . . . yes Sb(1) As(1) C(2) 117.3(3) . . . yes Sb(1) As(1) C(3) 107.0(3) . . . yes C(1) As(1) C(2) 104.5(5) . . . yes C(1) As(1) C(3) 104.8(4) . . . yes C(2) As(1) C(3) 104.7(5) . . . yes Sb(1) As(2) C(8) 106.6(3) . . . yes Sb(1) As(2) C(9) 116.0(3) . . . yes Sb(1) As(2) C(10) 115.4(3) . . . yes C(8) As(2) C(9) 107.0(4) . . . yes C(8) As(2) C(10) 106.3(4) . . . yes C(9) As(2) C(10) 105.0(4) . . . yes Sb(1) Cl(3) Sb(2) 93.45(7) . . . yes Sb(1*) Cl(6) Sb(2) 172.5(1) 2 . . yes As(1) C(3) C(4) 117.9(7) . . . yes As(1) C(3) C(8) 121.8(8) . . . yes C(4) C(3) C(8) 120.4(9) . . . yes C(3) C(4) C(5) 120.2(9) . . . yes C(4) C(5) C(6) 120.7(9) . . . yes C(5) C(6) C(7) 119.8(9) . . . yes C(6) C(7) C(8) 120.0(9) . . . yes As(2) C(8) C(3) 123.2(8) . . . yes As(2) C(8) C(7) 118.0(7) . . . yes C(3) C(8) C(7) 118.8(9) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Sb(2) Cl(1) 3.267(3) . 2_655 no #------------------------------------------------------------------------------