# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 182/1865 data_General #============================================================================== _audit_creation_date '2000-10-03' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_requested_journal ' J. Chem. Soc., Chem. Commun.' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for the structure of [SbBr3{MeS(CH2)3SMe}] included in manuscript number B007805K. ; _publ_contact_author_phone ' 023 80 593609 ' _publ_contact_author_fax ' 023 80 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== _publ_section_references ; Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. (1997). ; #============================================================================== data__sbbrsc3_SbBr3_+_MeS(CH2)3Me #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SHELX97 (Sheldrick, 1997) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 14.105(2) _cell_length_b 9.446(1) _cell_length_c 9.781(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1303.2(3) _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 8.8 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' '1/2-x,1/2+y,1/2+z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ? _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.537 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 497.73 _chemical_formula_analytical ? _chemical_formula_sum 'C5 H12 Br3 S2 Sb ' _chemical_formula_moiety 'C5 H12 Br3 S2 Sb ' _chemical_formula_structural [SbBr3{MeS(CH2)3SMe}] _chemical_compound_source ? _exptl_crystal_F_000 920.00 _exptl_absorpt_coefficient_mu 11.611 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.795 _exptl_special_details ; The scan width was (1.15+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. ; #============================================================================== # EXPERIMENTAL DATA _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 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.60 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -2 3 1 -1 3 1 1 3 _diffrn_reflns_number 1364 _reflns_number_total 1364 _reflns_number_gt 1022 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.080 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.04004 _diffrn_orient_matrix_UB_12 0.06910 _diffrn_orient_matrix_UB_13 0.05164 _diffrn_orient_matrix_UB_21 0.03828 _diffrn_orient_matrix_UB_22 0.01807 _diffrn_orient_matrix_UB_23 -0.08426 _diffrn_orient_matrix_UB_31 -0.04425 _diffrn_orient_matrix_UB_32 0.07815 _diffrn_orient_matrix_UB_33 -0.02617 #------------------------------------------------------------------------------ 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 20 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 8 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Sb 0 4 -0.816 1.546 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Br 0 12 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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) 0.09880(6) 0.13476(9) 0.9613 0.0177(2) 1.000 . Uani d ? Br(1) 0.2132(1) 0.2960(2) 0.8283(2) 0.0261(4) 1.000 . Uani d ? Br(2) 0.1716(1) 0.1809(2) 1.1904(2) 0.0286(4) 1.000 . Uani d ? Br(3) 0.2013(1) -0.0862(2) 0.9174(2) 0.0320(4) 1.000 . Uani d ? S(1) 0.0389(3) 0.0680(4) 0.6426(4) 0.0223(9) 1.000 . Uani d ? S(2) 0.0038(3) 0.5760(4) 0.5252(4) 0.027(1) 1.000 . Uani d ? C(1) 0.148(1) 0.014(2) 0.558(2) 0.031(4) 1.000 . Uani d ? C(2) 0.020(1) 0.243(1) 0.566(2) 0.026(3) 1.000 . Uani d ? C(3) -0.052(1) 0.324(1) 0.651(1) 0.021(4) 1.000 . Uani d ? C(4) -0.089(1) 0.457(2) 0.585(2) 0.028(4) 1.000 . Uani d ? C(5) 0.061(1) 0.616(2) 0.686(2) 0.052(6) 1.000 . Uani d ? H(1) 0.1938 -0.0072 0.6261 0.042 1.000 . Uiso c ? H(2) 0.1362 -0.0634 0.5024 0.042 1.000 . Uiso c ? H(3) 0.1704 0.0927 0.5049 0.042 1.000 . Uiso c ? H(4) 0.0784 0.2940 0.5643 0.032 1.000 . Uiso c ? H(5) -0.0027 0.2326 0.4751 0.032 1.000 . Uiso c ? H(6) -0.1041 0.2631 0.6684 0.024 1.000 . Uiso c ? H(7) -0.0231 0.3505 0.7344 0.024 1.000 . Uiso c ? H(8) -0.1291 0.5083 0.6403 0.035 1.000 . Uiso c ? H(9) -0.1244 0.4312 0.5004 0.035 1.000 . Uiso c ? H(10) 0.0219 0.5876 0.7590 0.054 1.000 . Uiso c ? H(11) 0.1203 0.5709 0.6901 0.054 1.000 . Uiso c ? H(12) 0.0705 0.7173 0.6914 0.054 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) 0.0207(4) 0.0167(4) 0.0157(4) 0.0009(4) 0.0016(4) -0.0007(4) Br(1) 0.0250(8) 0.0272(7) 0.0262(8) -0.0082(7) 0.0066(7) -0.0009(7) Br(2) 0.0341(8) 0.0301(8) 0.0214(7) -0.0004(7) -0.0079(7) -0.0008(7) Br(3) 0.0359(9) 0.0254(8) 0.0348(9) 0.0121(7) 0.0077(7) 0.0004(7) S(1) 0.024(2) 0.022(2) 0.021(2) 0.001(2) 0.001(2) -0.002(2) S(2) 0.024(2) 0.030(2) 0.026(2) 0.004(2) -0.000(2) 0.008(2) C(1) 0.029(7) 0.038(9) 0.027(9) 0.006(7) 0.012(6) -0.001(8) C(2) 0.030(8) 0.020(5) 0.029(7) -0.003(6) 0.006(7) -0.002(5) C(3) 0.031(8) 0.022(7) 0.011(7) -0.007(6) -0.001(6) -0.001(5) C(4) 0.034(8) 0.017(7) 0.031(9) -0.000(5) 0.006(7) -0.003(6) C(5) 0.08(1) 0.028(9) 0.04(1) -0.001(9) -0.05(1) -0.015(9) #============================================================================== # REFINEMENT DATA _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) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1022 _refine_ls_number_parameters 99 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_all 0.0490 _refine_ls_wR_factor_ref 0.0490 _refine_ls_goodness_of_fit_all 2.054 _refine_ls_goodness_of_fit_ref 2.050 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min -1.68 _refine_diff_density_max 1.17 #============================================================================== # MOLECULAR GEOMETRY 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 SB1 BR1 2.572(2) . . ? SB1 BR2 2.503(2) . . ? SB1 BR3 2.575(2) . . ? SB1 S1 3.291(5) . . ? SB1 S1* 3.253(5) . . ? SB1 S2* 3.155(5) . . ? S1 C1 1.81(2) . . ? S1 C2 1.83(2) . . ? S2 C4 1.82(2) . . ? S2 C5 1.81(2) . . ? C1 H1 0.95(2) . . ? C1 H2 0.95(2) . . ? C1 H3 0.95(2) . . ? C2 C3 1.52(3) . . ? C2 H4 0.95(2) . . ? C2 H5 0.95(2) . . ? C3 C4 1.51(3) . . ? C3 H6 0.95(2) . . ? C3 H7 0.95(2) . . ? C4 H8 0.95(2) . . ? C4 H9 0.95(2) . . ? C5 H10 0.95(3) . . ? C5 H11 0.95(3) . . ? C5 H12 0.95(2) . . ? #------------------------------------------------------------------------------ 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 BR1 SB1 BR2 95.29(8) . . . ? BR1 SB1 BR3 92.49(8) . . . ? BR1 SB1 S1 78.2(1) . . . ? BR1 SB1 S1* 177.2(1) . . . ? BR1 SB1 S2* 82.8(1) . . . ? BR2 SB1 BR3 93.44(9) . . . ? BR2 SB1 S1 170.6(1) . . . ? BR2 SB1 S1* 81.9(1) . . . ? BR2 SB1 S2* 82.0(1) . . . ? BR3 SB1 S1 80.3(1) . . . ? BR3 SB1 S1* 87.1(1) . . . ? BR3 SB1 S2* 173.1(1) . . . ? S1 SB1 S1* 104.49(7) . . . ? S1 SB1 S2* 103.6(1) . . . ? S1* SB1 S2* 97.4(1) 2 2 2 ? SB1 S1 SB1* 141.5(2) . . . ? SB1 S1 C1 105.5(8) . . . ? SB1 S1 C2 104.4(7) . . . ? SB1 S1* C1* 95.2(8) 2_554 2_554 2_554 ? SB1 S1* C2* 103.0(7) 2_554 2_554 2_554 ? C1 S1 C2 101(1) . . . ? SB1 S2* C4* 105.6(7) 2_564 2_564 2_564 ? SB1 S2* C5* 101.3(8) 2_564 2_564 2_564 ? C4 S2 C5 100(1) . . . ? S1 C1 H1 109(2) . . . ? S1 C1 H2 109(2) . . . ? S1 C1 H3 109(2) . . . ? H1 C1 H2 109(2) . . . ? H1 C1 H3 109(2) . . . ? H2 C1 H3 109(2) . . . ? S1 C2 C3 109(1) . . . ? S1 C2 H4 110(2) . . . ? S1 C2 H5 110(2) . . . ? C3 C2 H4 110(2) . . . ? C3 C2 H5 110(2) . . . ? H4 C2 H5 109(2) . . . ? C2 C3 C4 115(2) . . . ? C2 C3 H6 108(2) . . . ? C2 C3 H7 108(2) . . . ? C4 C3 H6 108(2) . . . ? C4 C3 H7 108(2) . . . ? H6 C3 H7 109(2) . . . ? S2 C4 C3 114(2) . . . ? S2 C4 H8 108(2) . . . ? S2 C4 H9 108(2) . . . ? C3 C4 H8 108(2) . . . ? C3 C4 H9 108(2) . . . ? H8 C4 H9 109(2) . . . ? S2 C5 H10 109(2) . . . ? S2 C5 H11 109(2) . . . ? S2 C5 H12 109(2) . . . ? H10 C5 H11 109(3) . . . ? H10 C5 H12 109(3) . . . ? H11 C5 H12 109(3) . . . ? #------------------------------------------------------------------------------ data_sbbr3se4_(SbBr3)2[16aneSe4] #------------------------------------------------------------------------------ _audit_creation_date '19100-09-27' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Soc., Chem. Commun.' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry, University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for the structure of [(SbBr3)2([16]aneSe4)] included in manuscript number B007805K. ; _publ_contact_author_phone ' 023 80 593609 ' _publ_contact_author_fax ' 023 80 593781 ' _publ_contact_author_email ' gr@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. ; #------------------------------------------------------------------------------ _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 10.276(2) _cell_length_b 13.540(3) _cell_length_c 10.755(2) _cell_angle_alpha 90 _cell_angle_beta 113.71(1) _cell_angle_gamma 90 _cell_volume 1370.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150.2 _cell_measurement_reflns_used 14 _cell_measurement_theta_min 7.0 _cell_measurement_theta_max 8.7 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _publ_section_exptl_prep ? _exptl_crystal_description 'rhomboid' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 2.926 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 603.54 _chemical_formula_analytical ? _chemical_formula_sum 'C6 H12 Br3 Sb Se2 ' _chemical_formula_moiety 'C6 H12 Br3 Sb Se2 ' _chemical_formula_structural [(SbBr3)2([16]aneSe4)] _chemical_compound_source ? _exptl_crystal_F_000 1088.00 _exptl_absorpt_coefficient_mu 16.058 _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 0.527 _exptl_special_details ; The scan width was (1.26+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_special_details ? _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_% 0.66 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -3 0 -1 -2 -3 -3 0 -1 _diffrn_reflns_number 2681 _reflns_number_total 2536 _reflns_number_gt 1724 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.16079 _diffrn_reflns_av_sigmaI/netI 0.090 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.08279 _diffrn_orient_matrix_UB_12 -0.01092 _diffrn_orient_matrix_UB_13 -0.08849 _diffrn_orient_matrix_UB_21 0.06657 _diffrn_orient_matrix_UB_22 -0.00978 _diffrn_orient_matrix_UB_23 -0.04585 _diffrn_orient_matrix_UB_31 0.00349 _diffrn_orient_matrix_UB_32 -0.07238 _diffrn_orient_matrix_UB_33 0.01955 #------------------------------------------------------------------------------ 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 24 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Se 0 8 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Br 0 12 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Sb 0 4 -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) 0.05524(7) -0.43921(5) 0.20889(8) 0.0130(2) 1.000 . Uani d ? Br(1) 0.0770(1) -0.62142(8) 0.1200(1) 0.0206(3) 1.000 . Uani d ? Br(2) 0.1654(1) -0.49846(8) 0.4532(1) 0.0192(3) 1.000 . Uani d ? Br(3) -0.2035(1) -0.4706(1) 0.1848(1) 0.0266(3) 1.000 . Uani d ? Se(1) 0.0633(1) -0.24647(8) 0.3473(1) 0.0179(3) 1.000 . Uani d ? Se(2) 0.1260(1) 0.12013(8) 0.2379(1) 0.0187(3) 1.000 . Uani d ? C(1) -0.050(1) -0.1692(8) 0.184(1) 0.018(3) 1.000 . Uani d ? C(2) 0.034(1) -0.0792(8) 0.170(1) 0.015(3) 1.000 . Uani d ? C(3) 0.062(1) -0.0054(8) 0.283(1) 0.019(3) 1.000 . Uani d ? C(4) 0.170(1) 0.1914(8) 0.410(1) 0.022(3) 1.000 . Uani d ? C(5) 0.047(1) 0.1936(9) 0.456(1) 0.022(3) 1.000 . Uani d ? C(6) 0.077(1) 0.261(1) 0.575(1) 0.033(4) 1.000 . Uani d ? H(1) -0.0761 -0.2097 0.1050 0.019 1.000 . Uiso c ? H(2) -0.1366 -0.1471 0.1903 0.019 1.000 . Uiso c ? H(3) 0.1213 -0.0995 0.1698 0.017 1.000 . Uiso c ? H(4) -0.0201 -0.0459 0.0847 0.017 1.000 . Uiso c ? H(5) 0.1308 -0.0308 0.3651 0.021 1.000 . Uiso c ? H(6) -0.0252 0.0056 0.2962 0.021 1.000 . Uiso c ? H(7) 0.2517 0.1635 0.4815 0.021 1.000 . Uiso c ? H(8) 0.1935 0.2600 0.4006 0.021 1.000 . Uiso c ? H(9) -0.0399 0.2126 0.3836 0.027 1.000 . Uiso c ? H(10) 0.0320 0.1274 0.4843 0.027 1.000 . Uiso c ? H(11) 0.0757 0.3275 0.5418 0.038 1.000 . Uiso c ? H(12) 0.1702 0.2475 0.6400 0.038 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) 0.0129(4) 0.0137(4) 0.0129(4) 0.0016(3) 0.0058(3) 0.0010(3) Br(1) 0.0231(6) 0.0162(6) 0.0192(6) 0.0027(5) 0.0052(5) -0.0010(5) Br(2) 0.0187(6) 0.0217(7) 0.0148(6) -0.0022(5) 0.0044(5) 0.0037(5) Br(3) 0.0129(6) 0.0423(8) 0.0231(7) -0.0012(5) 0.0057(5) -0.0044(6) Se(1) 0.0231(6) 0.0127(6) 0.0200(6) -0.0012(5) 0.0108(5) -0.0001(5) Se(2) 0.0256(6) 0.0126(6) 0.0218(7) -0.0009(5) 0.0138(5) 0.0001(5) C(1) 0.014(5) 0.016(6) 0.016(6) -0.003(5) -0.005(5) 0.004(5) C(2) 0.014(5) 0.023(7) 0.005(5) -0.001(5) 0.001(4) -0.004(5) C(3) 0.028(6) 0.014(6) 0.016(6) 0.008(5) 0.010(5) 0.007(5) C(4) 0.023(7) 0.011(6) 0.026(7) -0.002(5) 0.005(5) -0.007(6) C(5) 0.017(6) 0.016(6) 0.032(8) -0.001(5) 0.008(5) -0.008(6) C(6) 0.044(8) 0.034(8) 0.035(8) -0.019(7) 0.031(7) -0.010(7) #------------------------------------------------------------------------------ _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) + 0.00000|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 1724 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_all 0.0388 _refine_ls_wR_factor_ref 0.0388 _refine_ls_goodness_of_fit_all 1.610 _refine_ls_goodness_of_fit_ref 1.610 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.08 _refine_diff_density_max 1.08 #------------------------------------------------------------------------------ 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) Br(1) 2.687(1) . . yes Sb(1) Br(2) 2.537(1) . . yes Sb(1) Br(3) 2.601(1) . . yes Sb(1) Se(1) 2.989(1) . . yes Sb(1) Se(2) 3.193(1) . 2_545 yes Se(1) C(1) 1.97(1) . . yes Se(1) C(6) 1.95(1) . 3_556 yes Se(2) C(3) 1.95(1) . . yes Se(2) C(4) 1.97(1) . . yes C(1) C(2) 1.53(1) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.96 . . no C(2) C(3) 1.51(2) . . yes C(2) H(3) 0.94 . . no C(2) H(4) 0.98 . . no C(3) H(5) 0.95 . . no C(3) H(6) 0.97 . . no C(4) C(5) 1.52(2) . . yes C(4) H(7) 0.96 . . no C(4) H(8) 0.98 . . no C(5) C(6) 1.50(2) . . yes C(5) H(9) 0.96 . . no C(5) H(10) 0.98 . . no C(6) H(11) 0.96 . . no C(6) H(12) 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 Br(1) Sb(1) Br(2) 90.67(4) . . . yes Br(1) Sb(1) Br(3) 92.43(4) . . . yes Br(1) Sb(1) Se(1) 171.51(4) . . . yes Br(1) Sb(1) Se(2) 93.94(4) . . 2_545 yes Br(2) Sb(1) Br(3) 93.67(4) . . . yes Br(2) Sb(1) Se(1) 81.31(4) . . . yes Br(2) Sb(1) Se(2) 84.02(4) . . 2_545 yes Br(3) Sb(1) Se(1) 90.83(4) . . . yes Br(3) Sb(1) Se(2) 173.24(5) . . 2_545 yes Se(1) Sb(1) Se(2) 82.55(3) . . 2_545 yes Sb(1) Se(1) C(1) 97.6(3) . . . yes Sb(1) Se(1) C(6) 104.3(4) . . 3_556 yes C(1) Se(1) C(6) 99.4(5) . . 3_556 yes Sb(1) Se(2) C(3) 99.2(3) 2 . . yes Sb(1) Se(2) C(4) 97.2(3) 2 . . yes C(3) Se(2) C(4) 99.4(5) . . . yes Se(1) C(1) C(2) 110.5(7) . . . yes Se(1) C(1) H(1) 109.9 . . . no Se(1) C(1) H(2) 109.4 . . . no C(2) C(1) H(1) 109.8 . . . no C(2) C(1) H(2) 109.3 . . . no H(1) C(1) H(2) 107.9 . . . no C(1) C(2) C(3) 112.6(9) . . . yes C(1) C(2) H(3) 110.2 . . . no C(1) C(2) H(4) 109.3 . . . no C(3) C(2) H(3) 108.9 . . . no C(3) C(2) H(4) 107.8 . . . no H(3) C(2) H(4) 107.9 . . . no Se(2) C(3) C(2) 110.6(8) . . . yes Se(2) C(3) H(5) 110.3 . . . no Se(2) C(3) H(6) 108.9 . . . no C(2) C(3) H(5) 109.8 . . . no C(2) C(3) H(6) 109.2 . . . no H(5) C(3) H(6) 107.9 . . . no Se(2) C(4) C(5) 114.1(8) . . . yes Se(2) C(4) H(7) 110.6 . . . no Se(2) C(4) H(8) 109.8 . . . no C(5) C(4) H(7) 108.8 . . . no C(5) C(4) H(8) 106.9 . . . no H(7) C(4) H(8) 106.4 . . . no C(4) C(5) C(6) 112.0(9) . . . yes C(4) C(5) H(9) 111.4 . . . no C(4) C(5) H(10) 109.9 . . . no C(6) C(5) H(9) 109.4 . . . no C(6) C(5) H(10) 107.5 . . . no H(9) C(5) H(10) 106.5 . . . no Se(1) C(6) C(5) 111.7(8) 3_556 . . yes Se(1) C(6) H(11) 110.5 3_556 . . no Se(1) C(6) H(12) 111.2 3_556 . . no C(5) C(6) H(11) 106.8 . . . no C(5) C(6) H(12) 108.0 . . . no H(11) C(6) H(12) 108.5 . . . 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 Sb(1) Br(1) 3.342(1) . 3_545 no #------------------------------------------------------------------------------ data_sbclsec3_SbCl3{MeSe(CH2)3SeMe} #------------------------------------------------------------------------------ _audit_creation_date '19100-09-27' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Soc., Chem. Commun.' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO171BJ ; _publ_contact_letter ; This is the CIF file for the structure of [SbCl3{MeSe(CH2)3SeMe}] included in manuscript number B007805K. ; _publ_contact_author_phone ' 023 80 593609 ' _publ_contact_author_fax ' 023 80 593781 ' _publ_contact_author_email ' gr@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. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 9.622(5) _cell_length_b 12.882(3) _cell_length_c 10.376(4) _cell_angle_alpha 90 _cell_angle_beta 101.89(4) _cell_angle_gamma 90 _cell_volume 1258.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 23.6 _cell_measurement_theta_max 25.0 #------------------------------------------------------------------------------ _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 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.33 _exptl_crystal_density_diffrn 2.418 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 458.18 _chemical_formula_analytical ? _chemical_formula_sum 'C5 H12 Cl3 Sb Se2 ' _chemical_formula_moiety '?' _chemical_formula_structural [SbCl3{MeSe(CH2)3SeMe}] _chemical_compound_source ? _exptl_crystal_F_000 848.00 _exptl_absorpt_coefficient_mu 8.559 _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 0.536 _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(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_% -0.41 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -4 1 -3 -2 1 -2 -3 2 _diffrn_reflns_number 2489 _reflns_number_total 2344 _reflns_number_gt 1934 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.07376 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.08203 _diffrn_orient_matrix_UB_12 -0.04458 _diffrn_orient_matrix_UB_13 0.01050 _diffrn_orient_matrix_UB_21 0.06495 _diffrn_orient_matrix_UB_22 -0.04321 _diffrn_orient_matrix_UB_23 0.06660 _diffrn_orient_matrix_UB_31 -0.01824 _diffrn_orient_matrix_UB_32 0.04660 _diffrn_orient_matrix_UB_33 0.07179 #------------------------------------------------------------------------------ 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 20 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Se 0 8 -0.178 2.223 ;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) ; Sb 0 4 -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) 0.60528(8) 0.64648(6) 0.08717(8) 0.0130(2) 1.000 . Uani d ? Se(1) 0.2913(1) 0.71857(9) -0.0512(1) 0.0183(3) 1.000 . Uani d ? Se(2) 0.1659(1) 1.17055(9) -0.0760(1) 0.0207(3) 1.000 . Uani d ? Cl(1) 0.5706(3) 0.7480(2) 0.2705(3) 0.0170(7) 1.000 . Uani d ? Cl(2) 0.4676(3) 0.5079(2) 0.1637(3) 0.0223(8) 1.000 . Uani d ? Cl(3) 0.8217(3) 0.5655(2) 0.2056(4) 0.033(1) 1.000 . Uani d ? C(1) 0.185(1) 0.692(1) 0.085(2) 0.040(5) 1.000 . Uani d ? C(2) 0.340(1) 0.8652(9) -0.012(1) 0.022(3) 1.000 . Uani d ? C(3) 0.219(1) 0.9441(9) -0.056(1) 0.019(3) 1.000 . Uani d ? C(4) 0.291(1) 1.0512(8) -0.036(1) 0.019(3) 1.000 . Uani d ? C(5) 0.097(1) 1.149(1) -0.262(1) 0.032(4) 1.000 . Uani d ? H(1) 0.1066 0.7385 0.0747 0.047 1.000 . Uiso c ? H(2) 0.1506 0.6225 0.0774 0.047 1.000 . Uiso c ? H(3) 0.2445 0.7018 0.1689 0.047 1.000 . Uiso c ? H(4) 0.3715 0.8716 0.0811 0.026 1.000 . Uiso c ? H(5) 0.4161 0.8828 -0.0537 0.026 1.000 . Uiso c ? H(6) 0.1490 0.9375 -0.0044 0.023 1.000 . Uiso c ? H(7) 0.1766 0.9340 -0.1465 0.023 1.000 . Uiso c ? H(8) 0.3372 1.0562 0.0542 0.022 1.000 . Uiso c ? H(9) 0.3587 1.0548 -0.0899 0.022 1.000 . Uiso c ? H(10) 0.0327 1.2026 -0.2968 0.038 1.000 . Uiso c ? H(11) 0.0490 1.0837 -0.2758 0.038 1.000 . Uiso c ? H(12) 0.1744 1.1486 -0.3058 0.038 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) 0.0203(4) 0.0030(4) 0.0162(4) 0.0016(3) 0.0044(3) -0.0001(3) Se(1) 0.0232(7) 0.0089(6) 0.0216(7) 0.0006(5) 0.0021(5) 0.0001(5) Se(2) 0.0200(7) 0.0087(6) 0.0337(8) 0.0022(5) 0.0062(6) 0.0025(5) Cl(1) 0.027(2) 0.008(1) 0.017(2) 0.001(1) 0.005(1) -0.003(1) Cl(2) 0.038(2) 0.007(1) 0.024(2) -0.007(1) 0.012(1) 0.000(1) Cl(3) 0.028(2) 0.021(2) 0.046(2) 0.013(1) 0.002(2) 0.008(2) C(1) 0.032(8) 0.029(8) 0.06(1) 0.010(7) 0.016(7) 0.017(8) C(2) 0.020(6) 0.009(6) 0.032(8) -0.001(5) -0.003(6) 0.002(5) C(3) 0.016(6) 0.010(6) 0.033(8) -0.001(5) 0.007(5) 0.002(5) C(4) 0.018(6) 0.008(6) 0.031(8) 0.002(5) 0.008(5) 0.003(5) C(5) 0.026(7) 0.023(7) 0.036(9) -0.011(6) -0.015(6) 0.006(6) #------------------------------------------------------------------------------ _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) + 0.00000|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 1934 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 4.7975 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_all 4.8389 _refine_ls_wR_factor_ref 0.0524 _refine_ls_goodness_of_fit_all 457.910 _refine_ls_goodness_of_fit_ref 4.320 _refine_ls_shift/su_max 0.1860 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -2.01 _refine_diff_density_max 1.42 #------------------------------------------------------------------------------ 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) Se(1) 3.204(2) . . yes Sb(1) Se(2) 3.244(2) . 3_675 yes Sb(1) Cl(1) 2.388(3) . . yes Sb(1) Cl(2) 2.451(3) . . yes Sb(1) Cl(3) 2.424(3) . . yes Se(1) C(1) 1.94(1) . . yes Se(1) C(2) 1.97(1) . . yes Se(2) C(4) 1.94(1) . . yes Se(2) C(5) 1.93(1) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.95 . . no C(2) C(3) 1.55(1) . . yes C(2) H(4) 0.95 . . no C(2) H(5) 0.95 . . no C(3) C(4) 1.54(1) . . yes C(3) H(6) 0.95 . . no C(3) H(7) 0.95 . . no C(4) H(8) 0.95 . . no C(4) H(9) 0.95 . . no C(5) H(10) 0.95 . . no C(5) H(11) 0.95 . . no C(5) H(12) 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 Se(1) Sb(1) Se(2) 110.96(4) . . 3_675 yes Se(1) Sb(1) Cl(1) 85.69(7) . . . yes Se(1) Sb(1) Cl(2) 80.43(8) . . . yes Se(1) Sb(1) Cl(3) 169.70(9) . . . yes Se(2) Sb(1) Cl(1) 80.66(7) 3_675 . . yes Se(2) Sb(1) Cl(2) 163.15(8) 3_675 . . yes Se(2) Sb(1) Cl(3) 79.18(9) 3_675 . . yes Cl(1) Sb(1) Cl(2) 88.1(1) . . . yes Cl(1) Sb(1) Cl(3) 94.5(1) . . . yes Cl(2) Sb(1) Cl(3) 89.3(1) . . . yes Sb(1) Se(1) C(1) 102.3(4) . . . yes Sb(1) Se(1) C(2) 91.2(3) . . . yes C(1) Se(1) C(2) 99.1(6) . . . yes Sb(1) Se(2) C(4) 100.9(3) 3_675 . . yes Sb(1) Se(2) C(5) 99.6(4) 3_675 . . yes C(4) Se(2) C(5) 99.8(5) . . . yes Se(1) C(1) H(1) 109.3 . . . no Se(1) C(1) H(2) 109.2 . . . no Se(1) C(1) H(3) 109.3 . . . no H(1) C(1) H(2) 109.6 . . . no H(1) C(1) H(3) 109.7 . . . no H(2) C(1) H(3) 109.7 . . . no Se(1) C(2) C(3) 115.7(8) . . . yes Se(1) C(2) H(4) 107.9 . . . no Se(1) C(2) H(5) 107.9 . . . no C(3) C(2) H(4) 107.9 . . . no C(3) C(2) H(5) 107.9 . . . no H(4) C(2) H(5) 109.5 . . . no C(2) C(3) C(4) 105.1(9) . . . yes C(2) C(3) H(6) 110.6 . . . no C(2) C(3) H(7) 110.6 . . . no C(4) C(3) H(6) 110.5 . . . no C(4) C(3) H(7) 110.5 . . . no H(6) C(3) H(7) 109.5 . . . no Se(2) C(4) C(3) 116.3(8) . . . yes Se(2) C(4) H(8) 107.7 . . . no Se(2) C(4) H(9) 107.7 . . . no C(3) C(4) H(8) 107.8 . . . no C(3) C(4) H(9) 107.7 . . . no H(8) C(4) H(9) 109.5 . . . no Se(2) C(5) H(10) 109.3 . . . no Se(2) C(5) H(11) 109.3 . . . no Se(2) C(5) H(12) 109.4 . . . no H(10) C(5) H(11) 109.5 . . . no H(10) C(5) H(12) 109.6 . . . no H(11) C(5) H(12) 109.7 . . . 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 Sb(1) Cl(2) 3.236(3) . 3_665 no Sb(1) Cl(1) 3.508(3) . 4_564 no Se(1) Cl(1) 3.589(3) . 4_564 no Cl(1) Cl(2) 3.452(4) . 2_655 no Cl(2) Cl(2) 3.583(6) . 3_665 no #------------------------------------------------------------------------------