# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1826 data_BiBr3ccd #------------------------------------------------------------------------------ _audit_creation_date '19100-01-25' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry, University of Southampton Highfield, Southampton SO17 1BJ UK ; _publ_contact_letter ; This is a revised CIF file for [BiBr3{MeS(CH2)3SMe}] included in Dalton manuscript no. 9/09803H. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' _publ_section_exptl_refinement ; Atom C5 shows some disorder which was modelled successfully using partial occupancies, C5 population = 0.6, C5B population = 0.4. Atom C1 is refined i sotropically since it showed non-positive definate TP when anisotropic. This is attributed to the fact that the scattering is heavily dominated by the Bi and Br atoms. ; _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. 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 'Enraf Nonius Kappa CCD Diffractometer Control' _computing_cell_refinement 'Enraf Nonius Kappa CCD 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 12.9497(4) _cell_length_b 11.8967(3) _cell_length_c 18.0227(4) _cell_angle_alpha 90 _cell_angle_beta 102.895(2) _cell_angle_gamma 90 _cell_volume 2706.5(1) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 2.871 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 584.96 _chemical_formula_analytical ? _chemical_formula_sum 'C5 H12 Bi Br3 S2 ' _chemical_formula_moiety 'C5 H12 Bi Br3 S2 ' _chemical_formula_structural '[BiBr3{MeS(CH2)3SMe}]' _chemical_compound_source ? _exptl_crystal_F_000 2096.00 _exptl_absorpt_coefficient_mu 22.151 _exptl_absorpt_correction_type SORTAV #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Enraf Nonius Kappa CCD' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 14331 _reflns_number_total 2873 _reflns_number_gt 2138 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.10175 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 26.38 _diffrn_reflns_reduction_process 'Lp corrections applied' #------------------------------------------------------------------------------ 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 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Br 0 24 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 16 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Bi 0 8 -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) 0.25294(5) 0.09695(5) 0.57157(3) 0.0179(2) 1.000 . Uani d ? Br(1) 0.4027(1) 0.2280(1) 0.4992(1) 0.0275(5) 1.000 . Uani d ? Br(2) 0.4126(1) -0.0450(1) 0.6355(1) 0.0274(5) 1.000 . Uani d ? Br(3) 0.1061(2) -0.0185(1) 0.6255(1) 0.0329(5) 1.000 . Uani d ? S(1) 0.2965(4) -0.2269(4) 0.2099(3) 0.034(1) 1.000 . Uani d ? S(2) 0.2086(4) -0.0211(3) 0.4251(2) 0.023(1) 1.000 . Uani d ? C(1) 0.339(1) -0.082(1) 0.424(1) 0.021(4) 1.000 . Uiso d ? C(2) 0.336(1) -0.166(1) 0.3622(9) 0.023(5) 1.000 . Uani d ? C(3) 0.304(2) -0.117(2) 0.282(1) 0.034(6) 1.000 . Uani d ? C(4) 0.139(2) -0.144(2) 0.447(2) 0.050(7) 1.000 . Uani d ? C(5) 0.181(3) -0.284(3) 0.212(2) 0.041(8) 0.600 . Uiso d ? C(5B) 0.422(4) -0.270(4) 0.220(3) 0.03(1) 0.400 . Uiso d ? H(1) 0.3869 -0.0216 0.4187 0.028 1.000 . Uiso c ? H(2) 0.3673 -0.1166 0.4729 0.028 1.000 . Uiso c ? H(3) 0.4055 -0.1993 0.3674 0.029 1.000 . Uiso c ? H(4) 0.2877 -0.2242 0.3667 0.029 1.000 . Uiso c ? H(5) 0.3546 -0.0605 0.2753 0.044 1.000 . Uiso c ? H(6) 0.2365 -0.0804 0.2762 0.044 1.000 . Uiso c ? H(7) 0.0773 -0.1229 0.4657 0.060 1.000 . Uiso c ? H(8) 0.1151 -0.1900 0.4029 0.060 1.000 . Uiso c ? H(9) 0.1831 -0.1891 0.4855 0.060 1.000 . Uiso c ? H(10) 0.1250 -0.2303 0.1976 0.046 0.600 . Uiso d ? H(11) 0.1660 -0.3453 0.1754 0.046 0.600 . Uiso d ? H(12) 0.1803 -0.3131 0.2605 0.046 0.600 . Uiso d ? H(13) 0.4490 -0.2965 0.2731 0.041 0.400 . Uiso d ? H(14) 0.4295 -0.3277 0.1875 0.041 0.400 . Uiso d ? H(15) 0.4674 -0.2077 0.2144 0.041 0.400 . Uiso d ? Br(1*) 0.0973(1) 0.2720(1) 0.5008(1) 0.0275(5) 1.000 . Uani d ? S(1*) 0.2965(4) 0.2269(4) 0.7099(3) 0.034(1) 1.000 . Uani d ? Bi(1*) 0.24706(5) 0.40305(5) 0.42843(3) 0.0179(2) 1.000 . Uani d ? Bi(1*) 0.25294(5) -0.09695(5) 0.07157(3) 0.0179(2) 1.000 . Uani d ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Bi(1) 0.0212(4) 0.0161(3) 0.0159(4) 0.0010(3) 0.0034(3) 0.0026(2) Br(1) 0.020(1) 0.0257(9) 0.036(1) 0.0015(7) 0.0041(8) 0.0101(8) Br(2) 0.029(1) 0.0281(9) 0.0237(9) 0.0094(8) 0.0038(8) 0.0052(7) Br(3) 0.032(1) 0.030(1) 0.038(1) -0.0054(8) 0.0134(9) 0.0061(8) S(1) 0.058(4) 0.027(2) 0.017(2) 0.006(2) 0.008(2) 0.002(2) S(2) 0.025(2) 0.026(2) 0.017(2) 0.001(2) 0.001(2) 0.000(2) C(2) 0.03(1) 0.020(8) 0.020(9) 0.000(7) 0.012(8) 0.000(7) C(3) 0.05(1) 0.04(1) 0.02(1) -0.004(9) 0.01(1) -0.004(8) C(4) 0.03(1) 0.04(1) 0.08(2) 0.00(1) 0.01(1) 0.00(1) Br(1*) 0.020(1) 0.0257(9) 0.036(1) 0.0015(7) 0.0041(8) 0.0101(8) S(1*) 0.058(4) 0.027(2) 0.017(2) -0.006(2) 0.008(2) -0.002(2) Bi(1*) 0.0212(4) 0.0161(3) 0.0159(4) 0.0010(3) 0.0034(3) 0.0026(2) Bi(1*) 0.0212(4) 0.0161(3) 0.0159(4) -0.0010(3) 0.0034(3) -0.0026(2) #------------------------------------------------------------------------------ _refine_special_details ; See above ; _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)]' _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 2138 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_all 0.0769 _refine_ls_wR_factor_ref 0.0769 _refine_ls_goodness_of_fit_all 1.584 _refine_ls_goodness_of_fit_ref 1.584 _refine_ls_shift/su_max 0.0644 _refine_ls_shift/su_mean 0.0307 _refine_diff_density_min -4.31 _refine_diff_density_max 2.47 #------------------------------------------------------------------------------ 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) Br(1) 3.004(2) . . yes Bi(1) Br(1) 2.980(2) . 7_556 yes Bi(1) Br(2) 2.719(2) . . yes Bi(1) Br(3) 2.697(2) . . yes Bi(1) S(1) 2.880(4) . 4 yes Bi(1) S(2) 2.931(4) . . yes S(1) C(3) 1.83(2) . . yes S(1) C(5) 1.65(3) . . yes S(1) C(5B) 1.68(5) . . yes S(2) C(1) 1.84(2) . . yes S(2) C(4) 1.81(2) . . yes C(1) C(2) 1.50(2) . . yes C(1) H(1) 0.97 . . no C(1) H(2) 0.96 . . no C(2) C(3) 1.53(3) . . yes C(2) H(3) 0.96 . . no C(2) H(4) 0.95 . . no C(3) H(5) 0.97 . . no C(3) H(6) 0.96 . . no C(4) H(7) 0.96 . . no C(4) H(8) 0.96 . . no C(4) H(9) 0.96 . . no C(5) H(10) 0.96 . . no C(5) H(11) 0.97 . . no C(5) H(12) 0.95 . . no C(5B) H(13) 0.99 . . no C(5B) H(14) 0.92 . . no C(5B) H(15) 0.96 . . 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) Bi(1) Br(1) 83.80(5) . . 7_556 yes Br(1) Bi(1) Br(2) 90.16(5) . . . yes Br(1) Bi(1) Br(3) 175.18(6) . . . yes Br(1) Bi(1) S(1) 94.4(1) . . 4 yes Br(1) Bi(1) S(2) 82.73(9) . . . yes Br(1) Bi(1) Br(2) 173.40(5) 7_556 . . yes Br(1) Bi(1) Br(3) 92.64(6) 7_556 . . yes Br(1) Bi(1) S(1) 88.8(1) 7_556 . 4 yes Br(1) Bi(1) S(2) 88.36(9) 7_556 . . yes Br(2) Bi(1) Br(3) 93.54(6) . . . yes Br(2) Bi(1) S(1) 89.0(1) . . 4 yes Br(2) Bi(1) S(2) 93.53(9) . . . yes Br(3) Bi(1) S(1) 88.8(1) . . 4 yes Br(3) Bi(1) S(2) 93.9(1) . . . yes S(1) Bi(1) S(2) 176.1(1) 4 . . yes Bi(1) Br(1) Bi(1) 96.20(5) . . 7_556 yes Bi(1) S(1) C(3) 101.5(6) 4_554 . . yes Bi(1) S(1) C(5) 104(1) 4_554 . . yes Bi(1) S(1) C(5B) 105(2) 4_554 . . yes C(3) S(1) C(5) 101(1) . . . yes C(3) S(1) C(5B) 104(2) . . . yes C(5) S(1) C(5B) 137(2) . . . yes Bi(1) S(2) C(1) 101.5(6) . . . yes Bi(1) S(2) C(4) 101.3(8) . . . yes C(1) S(2) C(4) 100.9(9) . . . yes S(2) C(1) C(2) 114(1) . . . yes S(2) C(1) H(1) 108.8 . . . no S(2) C(1) H(2) 109.0 . . . no C(2) C(1) H(1) 109.1 . . . no C(2) C(1) H(2) 109.2 . . . no H(1) C(1) H(2) 107.0 . . . no C(1) C(2) C(3) 114(1) . . . yes C(1) C(2) H(3) 109.6 . . . no C(1) C(2) H(4) 109.1 . . . no C(3) C(2) H(3) 107.5 . . . no C(3) C(2) H(4) 108.1 . . . no H(3) C(2) H(4) 108.6 . . . no S(1) C(3) C(2) 111(1) . . . yes S(1) C(3) H(5) 110.1 . . . no S(1) C(3) H(6) 110.4 . . . no C(2) C(3) H(5) 109.3 . . . no C(2) C(3) H(6) 108.9 . . . no H(5) C(3) H(6) 107.2 . . . no S(2) C(4) H(7) 110.8 . . . no S(2) C(4) H(8) 111.1 . . . no S(2) C(4) H(9) 111.3 . . . no H(7) C(4) H(8) 107.5 . . . no H(7) C(4) H(9) 107.8 . . . no H(8) C(4) H(9) 108.3 . . . no S(1) C(5) H(10) 110.6 . . . no S(1) C(5) H(11) 110.2 . . . no S(1) C(5) H(12) 111.3 . . . no H(10) C(5) H(11) 107.3 . . . no H(10) C(5) H(12) 108.8 . . . no H(11) C(5) H(12) 108.4 . . . no S(1) C(5B) H(13) 108.8 . . . no S(1) C(5B) H(14) 113.2 . . . no S(1) C(5B) H(15) 110.4 . . . no H(13) C(5B) H(14) 108.3 . . . no H(13) C(5B) H(15) 104.8 . . . no H(14) C(5B) H(15) 110.9 . . . 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(5B) C(5B) 2.1(1) . 2_655 no #------------------------------------------------------------------------------ data_bibr3_[(BiBr3)n(MeS(CH2)2S #------------------------------------------------------------------------------ _audit_creation_date '19100-01-10' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UK ; _publ_contact_letter ; CIF file for [BiBr3{MeSe(CH2)2SeMe}2] ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 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 13.040(1) _cell_length_b 14.493(2) _cell_length_c 9.883(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1867.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150.1 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 17.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 2.465 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 693.18 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H20 Bi Br3 S4 ' _chemical_formula_moiety 'C8 H20 Bi Br3 S4 ' _chemical_formula_structural [BiBr3{MeSe(CH2)2SeMe}2] _chemical_compound_source ? _exptl_crystal_F_000 1280.00 _exptl_absorpt_coefficient_mu 16.285 _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 0.807 _exptl_special_details ; The scan width was (0.79+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 150.1 _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_% -0.04 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -2 -3 -1 -3 -3 1 -2 -3 _diffrn_reflns_number 1907 _reflns_number_total 1907 _reflns_number_gt 1548 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.06558 _diffrn_orient_matrix_UB_12 -0.02007 _diffrn_orient_matrix_UB_13 -0.04341 _diffrn_orient_matrix_UB_21 -0.01534 _diffrn_orient_matrix_UB_22 -0.06547 _diffrn_orient_matrix_UB_23 0.02474 _diffrn_orient_matrix_UB_31 -0.03667 _diffrn_orient_matrix_UB_32 -0.00851 _diffrn_orient_matrix_UB_33 -0.08798 #------------------------------------------------------------------------------ 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 32 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 80 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 16 0.110 0.124 ;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) ; 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) -0.02396(4) -0.49510(3) -0.04408(5) 0.0183(1) 1.000 . Uani d ? Br(1) 0.0726(1) -0.4326(1) -0.2816(1) 0.0310(4) 1.000 . Uani d ? Br(2) 0.1195(1) -0.6312(1) 0.0338(2) 0.0379(5) 1.000 . Uani d ? Br(3) -0.1853(1) -0.3690(1) -0.0512(2) 0.0350(4) 1.000 . Uani d ? S(1) 0.1210(3) -0.3534(3) 0.0567(5) 0.033(1) 1.000 . Uani d ? S(2) -0.0615(3) -0.4608(3) 0.2605(4) 0.035(1) 1.000 . Uani d ? S(3) -0.1579(3) -0.6421(2) 0.0770(3) 0.0231(9) 1.000 . Uani d ? S(4) -0.1031(3) -0.6068(2) -0.2664(3) 0.0239(9) 1.000 . Uani d ? C(1) 0.248(1) -0.392(1) -0.001(2) 0.042(5) 1.000 . Uani d ? C(2) 0.135(1) -0.378(1) 0.238(2) 0.053(4) 1.000 . Uani d ? C(3) 0.027(2) -0.368(1) 0.302(1) 0.046(4) 1.000 . Uani d ? C(4) -0.014(1) -0.560(1) 0.360(1) 0.049(5) 1.000 . Uani d ? C(5) -0.290(1) -0.609(1) 0.073(1) 0.033(4) 1.000 . Uani d ? C(6) -0.153(1) -0.7275(9) -0.056(1) 0.028(4) 1.000 . Uani d ? C(7) -0.186(1) -0.6935(9) -0.194(1) 0.026(4) 1.000 . Uani d ? C(8) 0.009(1) -0.6778(9) -0.306(1) 0.030(4) 1.000 . Uani d ? H(1) 0.2559 -0.4559 0.0187 0.051 1.000 . Uiso c ? H(2) 0.2537 -0.3826 -0.0957 0.051 1.000 . Uiso c ? H(3) 0.2996 -0.3579 0.0446 0.051 1.000 . Uiso c ? H(4) 0.1602 -0.4394 0.2509 0.063 1.000 . Uiso c ? H(5) 0.1814 -0.3357 0.2786 0.063 1.000 . Uiso c ? H(6) -0.0014 -0.3118 0.2718 0.056 1.000 . Uiso c ? H(7) 0.0351 -0.3667 0.3977 0.056 1.000 . Uiso c ? H(8) -0.0566 -0.6117 0.3446 0.059 1.000 . Uiso c ? H(9) 0.0543 -0.5738 0.3330 0.059 1.000 . Uiso c ? H(10) -0.0147 -0.5444 0.4534 0.059 1.000 . Uiso c ? H(11) -0.3025 -0.5628 0.1392 0.040 1.000 . Uiso c ? H(12) -0.3064 -0.5850 -0.0143 0.040 1.000 . Uiso c ? H(13) -0.3321 -0.6611 0.0907 0.040 1.000 . Uiso c ? H(14) -0.0847 -0.7492 -0.0632 0.034 1.000 . Uiso c ? H(15) -0.1970 -0.7772 -0.0316 0.034 1.000 . Uiso c ? H(16) -0.2528 -0.6681 -0.1857 0.031 1.000 . Uiso c ? H(17) -0.1877 -0.7449 -0.2535 0.031 1.000 . Uiso c ? H(18) 0.0336 -0.7056 -0.2258 0.036 1.000 . Uiso c ? H(19) -0.0106 -0.7245 -0.3689 0.036 1.000 . Uiso c ? H(20) 0.0605 -0.6402 -0.3449 0.036 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) 0.0243(2) 0.0157(2) 0.0148(2) 0.0013(3) 0.0003(2) -0.0002(3) Br(1) 0.0472(9) 0.0241(7) 0.0218(7) -0.0090(7) 0.0091(8) 0.0007(6) Br(2) 0.0346(9) 0.0321(8) 0.047(1) 0.0121(7) -0.006(1) 0.0012(9) Br(3) 0.0391(9) 0.0349(8) 0.0309(8) 0.0158(7) 0.0048(9) 0.0067(8) S(1) 0.034(2) 0.027(2) 0.037(2) -0.006(2) -0.009(2) -0.003(2) S(2) 0.054(3) 0.037(2) 0.015(2) 0.004(2) -0.005(2) -0.004(2) S(3) 0.033(2) 0.022(2) 0.014(2) -0.003(2) 0.002(2) 0.002(1) S(4) 0.038(2) 0.020(2) 0.013(2) -0.001(2) 0.000(2) 0.001(1) C(1) 0.030(6) 0.05(1) 0.04(1) 0.003(7) -0.012(6) 0.009(8) C(2) 0.067(9) 0.06(1) 0.035(4) -0.01(1) -0.040(8) -0.025(8) C(3) 0.08(1) 0.036(8) 0.022(8) -0.014(7) -0.013(9) -0.010(7) C(4) 0.08(1) 0.047(9) 0.015(7) 0.001(9) -0.023(9) 0.014(6) C(5) 0.031(4) 0.040(9) 0.028(9) -0.005(7) 0.005(7) -0.008(7) C(6) 0.034(8) 0.022(7) 0.029(6) -0.005(6) 0.005(7) -0.011(4) C(7) 0.031(8) 0.019(7) 0.029(7) -0.003(5) 0.006(6) -0.011(5) C(8) 0.039(8) 0.023(7) 0.028(7) -0.004(5) 0.015(7) -0.002(6) #------------------------------------------------------------------------------ _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) + 0.00001|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 1548 _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 0.0354 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0436 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.919 _refine_ls_shift/su_max 0.0162 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -2.43 _refine_diff_density_max 1.57 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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) Br(1) 2.813(2) . . yes Bi(1) Br(2) 2.826(2) . . yes Bi(1) Br(3) 2.787(2) . . yes Bi(1) S(1) 2.963(5) . . yes Bi(1) S(2) 3.090(5) . . yes Bi(1) S(3) 3.004(5) . . yes Bi(1) S(4) 2.918(5) . . yes S(1) C(1) 1.84(2) . . yes S(1) C(2) 1.84(2) . . yes S(2) C(3) 1.82(2) . . yes S(2) C(4) 1.85(2) . . yes S(3) C(5) 1.79(2) . . yes S(3) C(6) 1.81(2) . . yes S(4) C(7) 1.81(2) . . yes S(4) C(8) 1.83(2) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(1) H(3) 0.94 . . no C(2) C(3) 1.55(3) . . yes C(2) H(4) 0.98 . . no C(2) H(5) 0.97 . . no C(3) H(6) 0.94 . . no C(3) H(7) 0.94 . . no C(4) H(8) 0.94 . . no C(4) H(9) 0.95 . . no C(4) H(10) 0.95 . . no C(5) H(11) 0.94 . . no C(5) H(12) 0.95 . . no C(5) H(13) 0.95 . . no C(6) C(7) 1.51(3) . . yes C(6) H(14) 0.95 . . no C(6) H(15) 0.95 . . no C(7) H(16) 0.95 . . no C(7) H(17) 0.95 . . no C(8) H(18) 0.95 . . no C(8) H(19) 0.95 . . no C(8) H(20) 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) Bi(1) Br(2) 98.96(7) . . . yes Br(1) Bi(1) Br(3) 96.07(7) . . . yes Br(1) Bi(1) S(1) 76.8(1) . . . yes Br(1) Bi(1) S(2) 146.3(1) . . . yes Br(1) Bi(1) S(3) 145.2(1) . . . yes Br(1) Bi(1) S(4) 73.1(1) . . . yes Br(2) Bi(1) Br(3) 164.63(7) . . . yes Br(2) Bi(1) S(1) 88.3(1) . . . yes Br(2) Bi(1) S(2) 87.2(1) . . . yes Br(2) Bi(1) S(3) 77.4(1) . . . yes Br(2) Bi(1) S(4) 93.0(1) . . . yes Br(3) Bi(1) S(1) 92.1(1) . . . yes Br(3) Bi(1) S(2) 78.4(1) . . . yes Br(3) Bi(1) S(3) 92.1(1) . . . yes Br(3) Bi(1) S(4) 94.5(1) . . . yes S(1) Bi(1) S(2) 70.3(2) . . . yes S(1) Bi(1) S(3) 136.8(2) . . . yes S(1) Bi(1) S(4) 149.7(2) . . . yes S(2) Bi(1) S(3) 68.5(1) . . . yes S(2) Bi(1) S(4) 140.1(1) . . . yes S(3) Bi(1) S(4) 72.6(1) . . . yes Bi(1) S(1) C(1) 105.0(8) . . . yes Bi(1) S(1) C(2) 104.8(8) . . . yes C(1) S(1) C(2) 99(1) . . . yes Bi(1) S(2) C(3) 103.8(7) . . . yes Bi(1) S(2) C(4) 109.9(7) . . . yes C(3) S(2) C(4) 104(1) . . . yes Bi(1) S(3) C(5) 111.0(7) . . . yes Bi(1) S(3) C(6) 100.1(6) . . . yes C(5) S(3) C(6) 101.4(9) . . . yes Bi(1) S(4) C(7) 107.3(6) . . . yes Bi(1) S(4) C(8) 101.1(7) . . . yes C(7) S(4) C(8) 99.8(9) . . . yes S(1) C(1) H(1) 108.9 . . . no S(1) C(1) H(2) 109.1 . . . no S(1) C(1) H(3) 109.3 . . . no H(1) C(1) H(2) 109.6 . . . no H(1) C(1) H(3) 109.8 . . . no H(2) C(1) H(3) 110.2 . . . no S(1) C(2) C(3) 107(2) . . . yes S(1) C(2) H(4) 110.4 . . . no S(1) C(2) H(5) 111.2 . . . no C(3) C(2) H(4) 111.1 . . . no C(3) C(2) H(5) 112.2 . . . no H(4) C(2) H(5) 105.4 . . . no S(2) C(3) C(2) 115(2) . . . yes S(2) C(3) H(6) 109.4 . . . no S(2) C(3) H(7) 109.4 . . . no C(2) C(3) H(6) 105.4 . . . no C(2) C(3) H(7) 107.3 . . . no H(6) C(3) H(7) 110.5 . . . no S(2) C(4) H(8) 109.6 . . . no S(2) C(4) H(9) 109.1 . . . no S(2) C(4) H(10) 109.1 . . . no H(8) C(4) H(9) 110.0 . . . no H(8) C(4) H(10) 109.9 . . . no H(9) C(4) H(10) 109.2 . . . no S(3) C(5) H(11) 109.3 . . . no S(3) C(5) H(12) 108.8 . . . no S(3) C(5) H(13) 109.1 . . . no H(11) C(5) H(12) 109.9 . . . no H(11) C(5) H(13) 110.2 . . . no H(12) C(5) H(13) 109.4 . . . no S(3) C(6) C(7) 115(1) . . . yes S(3) C(6) H(14) 107.9 . . . no S(3) C(6) H(15) 107.9 . . . no C(7) C(6) H(14) 108.2 . . . no C(7) C(6) H(15) 108.4 . . . no H(14) C(6) H(15) 109.2 . . . no S(4) C(7) C(6) 115(1) . . . yes S(4) C(7) H(16) 108.1 . . . no S(4) C(7) H(17) 108.4 . . . no C(6) C(7) H(16) 108.0 . . . no C(6) C(7) H(17) 108.3 . . . no H(16) C(7) H(17) 109.4 . . . no S(4) C(8) H(18) 109.4 . . . no S(4) C(8) H(19) 109.6 . . . no S(4) C(8) H(20) 109.3 . . . no H(18) C(8) H(19) 109.7 . . . no H(18) C(8) H(20) 109.2 . . . no H(19) C(8) H(20) 109.6 . . . 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 Br(1) C(6) 3.54(2) . 4_554 no Br(2) H(15) 2.7378 . 3_535 no S(1) H(19) 3.0073 . 4_554 no S(2) H(12) 2.8922 . 2_445 no S(4) H(11) 2.9094 . 2_444 no C(1) H(20) 2.9696 . 2_545 no C(6) H(7) 2.9725 . 4_545 no C(8) H(3) 2.9518 . 2_544 no H(2) H(17) 2.6363 . 4_554 no H(2) H(9) 2.6794 . 2_544 no H(3) H(20) 2.1280 . 2_545 no H(5) H(15) 2.6369 . 4 no H(7) H(14) 2.4394 . 4 no H(10) H(20) 2.6218 . 1_556 no data_bibr3ph_[BiBr3{PhS(CH2)2SPh}] #------------------------------------------------------------------------------ _audit_creation_date '19100-01-10' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UK ; _publ_contact_letter ; CIF file for [Bi2Br6{PhS(CH2)2SPh}] ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 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. 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 9.267(3) _cell_length_b 6.981(2) _cell_length_c 18.340(5) _cell_angle_alpha 90 _cell_angle_beta 93.94(2) _cell_angle_gamma 90 _cell_volume 1183.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150.1 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 7.0 _cell_measurement_theta_max 8.9 #------------------------------------------------------------------------------ _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 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 3.209 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1143.77 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H14 Bi2 Br6 S2 ' _chemical_formula_moiety 'C14 H14 Bi2 Br6 S2 ' _chemical_formula_structural '[Bi2Br6{PhS(CH2)2SPh}]' _chemical_compound_source ? _exptl_crystal_F_000 1012.00 _exptl_absorpt_coefficient_mu 25.153 _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 0.535 _exptl_special_details ; The scan width was (1.52+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 150.1 _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_% 0.63 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -1 6 0 -1 6 -2 -2 2 _diffrn_reflns_number 2419 _reflns_number_total 2277 _reflns_number_gt 1212 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.09317 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05806 _diffrn_orient_matrix_UB_12 0.01009 _diffrn_orient_matrix_UB_13 0.04383 _diffrn_orient_matrix_UB_21 -0.06864 _diffrn_orient_matrix_UB_22 0.08930 _diffrn_orient_matrix_UB_23 -0.02730 _diffrn_orient_matrix_UB_31 -0.06015 _diffrn_orient_matrix_UB_32 -0.11155 _diffrn_orient_matrix_UB_33 -0.01790 #------------------------------------------------------------------------------ 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 28 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 28 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 4 0.110 0.124 ;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) ; 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) 0.92682(9) 0.2489(2) 0.43818(4) 0.0142(2) 1.000 . Uani d ? Br(1) 0.9128(3) 0.4002(4) 0.3086(1) 0.0225(7) 1.000 . Uani d ? Br(2) 1.1952(2) 0.3969(4) 0.4794(1) 0.0196(6) 1.000 . Uani d ? Br(3) 1.0454(3) -0.0806(4) 0.3948(1) 0.0209(7) 1.000 . Uani d ? S(1) 0.6287(6) 0.060(1) 0.4051(3) 0.020(2) 1.000 . Uani d ? C(1) 0.569(2) 0.060(3) 0.499(1) 0.010(6) 1.000 . Uani d ? C(2) 0.510(2) 0.227(4) 0.363(1) 0.012(6) 1.000 . Uani d ? C(3) 0.527(3) 0.431(4) 0.376(1) 0.023(7) 1.000 . Uani d ? C(4) 0.432(3) 0.560(4) 0.341(1) 0.026(8) 1.000 . Uani d ? C(5) 0.319(3) 0.492(4) 0.293(1) 0.024(7) 1.000 . Uani d ? C(6) 0.303(3) 0.297(3) 0.281(1) 0.018(7) 1.000 . Uani d ? C(7) 0.394(2) 0.167(3) 0.315(1) 0.015(6) 1.000 . Uani d ? H(1) 0.5479 0.1887 0.5147 0.011 1.000 . Uiso c ? H(2) 0.6418 0.0088 0.5330 0.011 1.000 . Uiso c ? H(3) 0.6027 0.4758 0.4093 0.028 1.000 . Uiso c ? H(4) 0.4452 0.6935 0.3489 0.031 1.000 . Uiso c ? H(5) 0.2525 0.5799 0.2694 0.028 1.000 . Uiso c ? H(6) 0.2271 0.2529 0.2473 0.022 1.000 . Uiso c ? H(7) 0.3784 0.0346 0.3060 0.018 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) 0.0141(4) 0.0139(4) 0.0146(4) -0.0034(6) 0.0010(3) -0.0025(6) Br(1) 0.023(1) 0.026(2) 0.018(1) -0.003(1) 0.000(1) 0.008(1) Br(2) 0.013(1) 0.023(1) 0.023(1) -0.002(1) -0.0001(9) -0.006(1) Br(3) 0.029(1) 0.018(1) 0.017(1) 0.001(1) 0.0039(9) 0.000(1) S(1) 0.014(3) 0.028(4) 0.018(3) -0.003(3) 0.001(2) -0.002(3) C(1) 0.00(1) 0.01(1) 0.02(1) 0.00(1) -0.001(9) 0.00(1) C(2) 0.02(1) 0.01(1) 0.01(1) -0.01(1) 0.012(8) -0.01(1) C(3) 0.02(1) 0.03(2) 0.02(1) -0.01(1) -0.01(1) 0.00(1) C(4) 0.06(2) 0.01(2) 0.01(1) -0.02(1) 0.01(1) -0.01(1) C(5) 0.02(1) 0.04(2) 0.02(1) 0.02(1) -0.01(1) 0.00(1) C(6) 0.02(1) 0.01(2) 0.03(1) -0.01(1) 0.00(1) 0.00(1) C(7) 0.01(1) 0.02(1) 0.02(1) -0.01(1) 0.00(1) 0.00(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) + 0.00002|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 1212 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0485 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.940 _refine_ls_shift/su_max 0.0110 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.72 _refine_diff_density_max 3.11 #------------------------------------------------------------------------------ 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) Br(1) 2.596(2) . . yes Bi(1) Br(2) 2.751(2) . . yes Bi(1) Br(2) 3.149(3) . 3_766 yes Bi(1) Br(3) 2.693(3) . . yes Bi(1) Br(3) 3.274(2) . 3_756 yes Bi(1) S(1) 3.082(6) . . yes S(1) C(1) 1.84(2) . . yes S(1) C(2) 1.75(2) . . yes C(1) C(1) 1.53(4) . 3_656 yes C(1) H(1) 0.97 . . no C(1) H(2) 0.96 . . no C(2) C(3) 1.45(4) . . yes C(2) C(7) 1.41(3) . . yes C(3) C(4) 1.39(4) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.40(3) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.39(3) . . yes C(5) H(5) 0.95 . . no C(6) C(7) 1.36(3) . . yes C(6) H(6) 0.95 . . no C(7) H(7) 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) Bi(1) Br(2) 94.94(8) . . . yes Br(1) Bi(1) Br(2) 97.04(8) . . 3_766 yes Br(1) Bi(1) Br(3) 94.19(8) . . . yes Br(1) Bi(1) Br(3) 176.62(8) . . 3_756 yes Br(1) Bi(1) S(1) 90.3(1) . . . yes Br(2) Bi(1) Br(2) 85.46(8) . . 3_766 yes Br(2) Bi(1) Br(3) 91.29(8) . . . yes Br(2) Bi(1) Br(3) 82.31(7) . . 3_756 yes Br(2) Bi(1) S(1) 174.7(1) . . . yes Br(2) Bi(1) Br(3) 168.53(7) 3_766 . . yes Br(2) Bi(1) Br(3) 80.82(6) 3_766 . 3_756 yes Br(2) Bi(1) S(1) 94.8(1) 3_766 . . yes Br(3) Bi(1) Br(3) 87.85(7) . . 3_756 yes Br(3) Bi(1) S(1) 87.5(1) . . . yes Br(3) Bi(1) S(1) 92.4(1) 3_756 . . yes Bi(1) Br(2) Bi(1) 94.54(8) . . 3_766 yes Bi(1) Br(3) Bi(1) 92.15(7) . . 3_756 yes Bi(1) S(1) C(1) 98.1(6) . . . yes Bi(1) S(1) C(2) 109.4(8) . . . yes C(1) S(1) C(2) 101.4(9) . . . yes S(1) C(1) C(1) 109(2) . . 3_656 yes S(1) C(1) H(1) 110.9 . . . no S(1) C(1) H(2) 111.4 . . . no C(1) C(1) H(1) 108.5 3_656 . . no C(1) C(1) H(2) 109.3 3_656 . . no H(1) C(1) H(2) 107.4 . . . no S(1) C(2) C(3) 121(2) . . . yes S(1) C(2) C(7) 121(2) . . . yes C(3) C(2) C(7) 118(2) . . . yes C(2) C(3) C(4) 120(2) . . . yes C(2) C(3) H(3) 119.7 . . . no C(4) C(3) H(3) 120.0 . . . no C(3) C(4) C(5) 120(2) . . . yes C(3) C(4) H(4) 119.6 . . . no C(5) C(4) H(4) 120.8 . . . no C(4) C(5) C(6) 120(2) . . . yes C(4) C(5) H(5) 120.0 . . . no C(6) C(5) H(5) 119.9 . . . no C(5) C(6) C(7) 122(2) . . . yes C(5) C(6) H(6) 119.5 . . . no C(7) C(6) H(6) 118.9 . . . no C(2) C(7) C(6) 121(2) . . . yes C(2) C(7) H(7) 119.6 . . . no C(6) C(7) H(7) 119.4 . . . 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(4) C(7) 3.45(3) . 2_655 no #------------------------------------------------------------------------------ data_bibr3sec3_[BiBr3(MeSe(CH2)3SeMe}] #------------------------------------------------------------------------------ _audit_creation_date '19100-01-10' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UK ; _publ_contact_letter ; This is the CIF file for [BiBr3{MeSe(CH2)3SeMe}] included in Dalton paper number 9/09803H. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' _publ_section_exptl_refinement ; Aton C5 shows a high TP, however attempts to split this into alternative positions with partial occupancies were not successful. Some of the C atoms gave npd TP's when refined anisotropically, since the scattering is dominate by the Bi, Br and Se atoms, hence the C atoms were refined isotropically. ; _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. 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 13.013(2) _cell_length_b 12.012(2) _cell_length_c 18.305(4) _cell_angle_alpha 90 _cell_angle_beta 103.64(2) _cell_angle_gamma 90 _cell_volume 2780.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _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 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'column' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 3.243 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 678.76 _chemical_formula_analytical ? _chemical_formula_sum 'C5 H12 Bi Br3 Se2 ' _chemical_formula_moiety 'C5 H12 Bi Br3 Se2 ' _chemical_formula_structural '[BiBr3{MeSe(CH2)3SeMe}]' _chemical_compound_source ? _exptl_crystal_F_000 2384.00 _exptl_absorpt_coefficient_mu 26.499 _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 0.441 _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_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_% -1.55 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 3 -2 -3 3 -1 2 4 -3 _diffrn_reflns_number 2998 _reflns_number_total 2998 _reflns_number_gt 1056 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 22.46 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01624 _diffrn_orient_matrix_UB_12 0.07743 _diffrn_orient_matrix_UB_13 0.01396 _diffrn_orient_matrix_UB_21 0.06592 _diffrn_orient_matrix_UB_22 0.02745 _diffrn_orient_matrix_UB_23 -0.01316 _diffrn_orient_matrix_UB_31 -0.04055 _diffrn_orient_matrix_UB_32 0.01351 _diffrn_orient_matrix_UB_33 -0.05284 #------------------------------------------------------------------------------ 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 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Se 0 16 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Br 0 24 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Bi 0 8 -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) 0.75177(7) 0.09853(6) 0.57066(5) 0.0204(3) 1.000 . Uani d ? Br(1) 0.9110(2) -0.0435(2) 0.6340(1) 0.0303(7) 1.000 . Uani d ? Br(2) 0.6066(2) -0.0145(2) 0.6262(1) 0.0368(8) 1.000 . Uani d ? Br(3) 0.9005(2) 0.2247(2) 0.4989(1) 0.0291(7) 1.000 . Uani d ? Se(1) 0.7007(2) -0.0177(2) 0.4196(1) 0.0260(7) 1.000 . Uani d ? Se(2) 0.8061(3) -0.2391(2) 0.2084(1) 0.051(1) 1.000 . Uani d ? C(1) 0.634(2) -0.147(2) 0.448(1) 0.054(8) 1.000 . Uiso d ? C(2) 0.841(2) -0.082(2) 0.425(1) 0.019(5) 1.000 . Uiso d ? C(3) 0.838(2) -0.168(2) 0.363(1) 0.029(6) 1.000 . Uiso d ? C(4) 0.814(2) -0.121(2) 0.284(1) 0.032(6) 1.000 . Uiso d ? C(5) 0.672(4) -0.288(3) 0.209(2) 0.16(2) 1.000 . Uiso d ? H(1) 0.5616 -0.1330 0.4484 0.056 1.000 . Uiso c ? H(2) 0.6346 -0.2078 0.4134 0.056 1.000 . Uiso c ? H(3) 0.6695 -0.1728 0.4971 0.056 1.000 . Uiso c ? H(4) 0.8890 -0.0248 0.4198 0.022 1.000 . Uiso c ? H(5) 0.8660 -0.1169 0.4732 0.022 1.000 . Uiso c ? H(6) 0.9047 -0.2067 0.3717 0.030 1.000 . Uiso c ? H(7) 0.7848 -0.2239 0.3656 0.030 1.000 . Uiso c ? H(8) 0.8671 -0.0677 0.2805 0.036 1.000 . Uiso c ? H(9) 0.7470 -0.0815 0.2753 0.036 1.000 . Uiso c ? H(10) 0.6179 -0.2272 0.1959 0.148 1.000 . Uiso c ? H(11) 0.6459 -0.3474 0.1765 0.148 1.000 . Uiso c ? H(12) 0.6650 -0.3104 0.2598 0.148 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) 0.0204(6) 0.0206(5) 0.0204(5) 0.0006(4) 0.0052(4) 0.0026(4) Br(1) 0.029(2) 0.033(1) 0.028(1) 0.009(1) 0.007(1) 0.007(1) Br(2) 0.031(2) 0.036(1) 0.045(2) -0.006(1) 0.014(1) 0.010(1) Br(3) 0.019(2) 0.030(1) 0.038(1) 0.001(1) 0.006(1) 0.011(1) Se(1) 0.024(2) 0.026(1) 0.026(1) 0.002(1) 0.001(1) 0.001(1) Se(2) 0.094(3) 0.033(1) 0.025(2) 0.014(1) 0.012(2) -0.001(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) + 0.00000|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 1056 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all - _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_all - _refine_ls_wR_factor_ref 0.0382 _refine_ls_goodness_of_fit_all - _refine_ls_goodness_of_fit_ref 1.657 _refine_ls_shift/su_max 1.4620 _refine_ls_shift/su_mean 0.0480 _refine_diff_density_min -0.89 _refine_diff_density_max 1.39 #------------------------------------------------------------------------------ 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) Br(1) 2.723(2) . . yes Bi(1) Br(2) 2.711(3) . . yes Bi(1) Br(3) 2.994(2) . . yes Bi(1) Br(3) 2.978(2) . 7_656 yes Bi(1) Se(1) 3.028(2) . . yes Bi(1) Se(2) 2.978(2) . 4 yes Se(1) C(1) 1.91(3) . . yes Se(1) C(2) 1.96(2) . . yes Se(2) C(4) 1.97(2) . . yes Se(2) C(5) 1.84(5) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.97 . . no C(1) H(3) 0.96 . . no C(2) C(3) 1.53(3) . . yes C(2) H(4) 0.94 . . no C(2) H(5) 0.97 . . no C(3) C(4) 1.51(3) . . yes C(3) H(6) 0.96 . . no C(3) H(7) 0.98 . . no C(4) H(8) 0.96 . . no C(4) H(9) 0.97 . . no C(5) H(10) 1.01 . . no C(5) H(11) 0.94 . . no C(5) H(12) 1.00 . . 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) Bi(1) Br(2) 93.11(8) . . . yes Br(1) Bi(1) Br(3) 89.89(7) . . . yes Br(1) Bi(1) Br(3) 172.59(8) . . 7_656 yes Br(1) Bi(1) Se(1) 94.67(7) . . . yes Br(1) Bi(1) Se(2) 89.41(8) . . 4 yes Br(2) Bi(1) Br(3) 175.91(8) . . . yes Br(2) Bi(1) Br(3) 93.74(7) . . 7_656 yes Br(2) Bi(1) Se(1) 95.10(7) . . . yes Br(2) Bi(1) Se(2) 90.79(8) . . 4 yes Br(3) Bi(1) Br(3) 83.42(7) . . 7_656 yes Br(3) Bi(1) Se(1) 81.87(6) . . . yes Br(3) Bi(1) Se(2) 92.03(7) . . 4 yes Br(3) Bi(1) Se(1) 87.56(6) 7_656 . . yes Br(3) Bi(1) Se(2) 87.65(7) 7_656 . 4 yes Se(1) Bi(1) Se(2) 172.64(7) . . 4 yes Bi(1) Br(3) Bi(1) 96.58(7) . . 7_656 yes Bi(1) Se(1) C(1) 98.0(7) . . . yes Bi(1) Se(1) C(2) 97.7(6) . . . yes C(1) Se(1) C(2) 99(1) . . . yes Bi(1) Se(2) C(4) 98.7(6) 4_554 . . yes Bi(1) Se(2) C(5) 99(1) 4_554 . . yes C(4) Se(2) C(5) 97(2) . . . yes Se(1) C(1) H(1) 111.8 . . . no Se(1) C(1) H(2) 110.8 . . . no Se(1) C(1) H(3) 111.7 . . . no H(1) C(1) H(2) 107.1 . . . no H(1) C(1) H(3) 108.4 . . . no H(2) C(1) H(3) 106.8 . . . no Se(1) C(2) C(3) 112(1) . . . yes Se(1) C(2) H(4) 110.1 . . . no Se(1) C(2) H(5) 109.0 . . . no C(3) C(2) H(4) 108.4 . . . no C(3) C(2) H(5) 108.9 . . . no H(4) C(2) H(5) 108.5 . . . no C(2) C(3) C(4) 115(2) . . . yes C(2) C(3) H(6) 109.9 . . . no C(2) C(3) H(7) 108.5 . . . no C(4) C(3) H(6) 108.8 . . . no C(4) C(3) H(7) 108.1 . . . no H(6) C(3) H(7) 106.4 . . . no Se(2) C(4) C(3) 112(1) . . . yes Se(2) C(4) H(8) 110.5 . . . no Se(2) C(4) H(9) 110.2 . . . no C(3) C(4) H(8) 108.7 . . . no C(3) C(4) H(9) 108.8 . . . no H(8) C(4) H(9) 106.8 . . . no Se(2) C(5) H(10) 112.1 . . . no Se(2) C(5) H(11) 116.6 . . . no Se(2) C(5) H(12) 113.0 . . . no H(10) C(5) H(11) 105.6 . . . no H(10) C(5) H(12) 101.3 . . . no H(11) C(5) H(12) 106.9 . . . no data_bi4cl4 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Jun 16 14:23:20 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 8.653(6) _cell_length_b 12.024(5) _cell_length_c 12.600(6) _cell_angle_alpha 90 _cell_angle_beta 107.70(5) _cell_angle_gamma 90 _cell_volume 1248(1) _cell_formula_units_Z 4 _cell_measurement_temperature 150.1 _cell_measurement_reflns_used 25 _cell_measurement_2theta_min 41.3 _cell_measurement_2theta_max 49.7 #------------------------------------------------------------------------------ _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 'yellow' _exptl_crystal_size_max 0.470 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.900 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 545.41 _chemical_formula_analytical ? _chemical_formula_sum 'C5 H12 Bi Cl3 Se2 ' _chemical_formula_moiety 'C5 H12 Bi Cl3 Se2 ' _chemical_formula_structural '[BiCl3(MeSeCH2CH2CH2SeMe]' _chemical_compound_source ? _exptl_crystal_F_000 976.00 _exptl_absorpt_coefficient_mu 20.511 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.433 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150.1 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.32 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 3 3 1 0 4 0 -1 4 _diffrn_reflns_number 2476 _reflns_number_total 2317 _reflns_number_observed 1721 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0681 _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 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.02181 _diffrn_orient_matrix_UB_12 0.06661 _diffrn_orient_matrix_UB_13 0.04077 _diffrn_orient_matrix_UB_21 -0.07986 _diffrn_orient_matrix_UB_22 -0.04402 _diffrn_orient_matrix_UB_23 0.02580 _diffrn_orient_matrix_UB_31 0.08868 _diffrn_orient_matrix_UB_32 -0.02326 _diffrn_orient_matrix_UB_33 0.06791 #------------------------------------------------------------------------------ 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 0.003 0.002 'International Tables' H 0 48 0.000 0.000 'International Tables' Cl 0 12 0.148 0.159 'International Tables' Se 0 8 -0.093 2.226 'International Tables' Bi 0 4 -4.108 10.257 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Bi(1) 0.35911(6) 0.14675(5) 0.94133(5) 0.0163(2) Uij ? ? Se(1) 0.6095(2) 0.2743(1) 1.1216(1) 0.0196(4) Uij ? ? Se(2) 0.1459(2) 0.0082(1) 0.7579(1) 0.0217(4) Uij ? ? Cl(1) 0.3736(4) 0.2942(3) 0.7988(3) 0.023(1) Uij ? ? Cl(2) 0.1063(5) 0.2424(4) 0.9645(3) 0.030(1) Uij ? ? Cl(3) 0.6345(5) 0.0394(3) 0.9131(3) 0.027(1) Uij ? ? C(1) 0.472(2) 0.404(1) 1.117(1) 0.023(4) Uij ? ? C(2) 0.733(2) 0.334(1) 1.026(1) 0.028(5) Uij ? ? C(3) 0.856(2) 0.422(1) 1.085(1) 0.025(4) Uij ? ? C(4) -0.005(2) 0.124(1) 0.683(1) 0.025(5) Uij ? ? C(5) 0.008(2) -0.056(2) 0.840(2) 0.042(6) Uij ? ? H(1) 0.4088 0.4199 1.0423 0.0274 Uiso ? ? H(2) 0.4017 0.3920 1.1609 0.0274 Uiso ? ? H(3) 0.5382 0.4682 1.1458 0.0274 Uiso ? ? H(4) 0.6592 0.3658 0.9596 0.0355 Uiso ? ? H(5) 0.7897 0.2744 1.0027 0.0355 Uiso ? ? H(6) 0.8014 0.4784 1.1136 0.0310 Uiso ? ? H(7) 0.9026 0.4565 1.0330 0.0310 Uiso ? ? H(8) 0.0521 0.1791 0.6538 0.0306 Uiso ? ? H(9) -0.0503 0.1591 0.7339 0.0306 Uiso ? ? H(10) -0.0920 -0.0819 0.7903 0.0502 Uiso ? ? H(11) -0.0162 -0.0012 0.8884 0.0502 Uiso ? ? H(12) 0.0615 -0.1170 0.8853 0.0502 Uiso ? ? 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) 0.0167(3) 0.0152(3) 0.0169(3) 0.0005(3) 0.0051(2) 0.0007(3) Se(1) 0.0206(8) 0.0213(8) 0.0182(8) -0.0004(7) 0.0078(7) 0.0024(7) Se(2) 0.0190(8) 0.0224(9) 0.0235(9) 0.0017(7) 0.0059(7) -0.0010(7) Cl(1) 0.027(2) 0.022(2) 0.019(2) -0.001(2) 0.008(2) 0.004(2) Cl(2) 0.028(2) 0.041(3) 0.025(2) 0.003(2) 0.014(2) -0.008(2) Cl(3) 0.033(2) 0.031(2) 0.021(2) 0.008(2) 0.013(2) 0.007(2) C(1) 0.013(7) 0.030(9) 0.022(9) 0.011(7) 0.000(7) -0.007(8) C(2) 0.033(9) 0.028(10) 0.028(10) -0.010(8) 0.015(8) 0.000(8) C(3) 0.033(9) 0.024(9) 0.019(9) 0.009(8) 0.009(8) 0.010(8) C(4) 0.033(9) 0.022(9) 0.024(9) 0.000(7) 0.016(8) 0.011(7) C(5) 0.034(10) 0.04(1) 0.05(1) -0.011(9) 0.021(10) 0.02(1) Cl(3*) 0.033(2) 0.031(2) 0.021(2) 0.008(2) 0.013(2) 0.007(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _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 1721 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0451 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0489 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.470 _refine_ls_shift/esd_max 0.0090 _refine_ls_shift/esd_mean ? _refine_diff_density_min -2.58 _refine_diff_density_max 3.65 #------------------------------------------------------------------------------ _geom_special_details ? 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) Se(1) 3.036(2) ? ? yes Bi(1) Se(2) 2.988(2) ? ? yes Bi(1) Cl(1) 2.554(4) ? ? yes Bi(1) Cl(2) 2.566(4) ? ? yes Bi(1) Cl(3) 2.826(4) ? ? yes Bi(1) Cl(3*) 2.884(4) ? ? yes Se(1) C(1) 1.95(1) ? ? yes Se(1) C(2) 1.97(1) ? ? yes Se(2) C(4) 1.94(2) ? ? yes Se(2) C(5) 1.95(2) ? ? yes C(2) C(3) 1.53(2) ? ? yes C(3) C(4) 1.54(2) ? ? yes #------------------------------------------------------------------------------ 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) Bi(1) Se(2) 173.19(4) ? ? ? yes Se(1) Bi(1) Cl(1) 89.95(9) ? ? ? yes Se(1) Bi(1) Cl(2) 97.3(1) ? ? ? yes Se(1) Bi(1) Cl(3) 83.56(10) ? ? ? yes Se(1) Bi(1) Cl(3*) 92.57(9) ? ? ? yes Se(2) Bi(1) Cl(1) 89.65(9) ? ? ? yes Se(2) Bi(1) Cl(2) 89.5(1) ? ? ? yes Se(2) Bi(1) Cl(3) 89.65(10) ? ? ? yes Se(2) Bi(1) Cl(3*) 86.97(9) ? ? ? yes Cl(1) Bi(1) Cl(2) 89.7(1) ? ? ? yes Cl(1) Bi(1) Cl(3) 90.3(1) ? ? ? yes Cl(1) Bi(1) Cl(3*) 172.2(1) ? ? ? yes Cl(2) Bi(1) Cl(3) 179.1(1) ? ? ? yes Cl(2) Bi(1) Cl(3*) 97.3(1) ? ? ? yes Cl(3) Bi(1) Cl(3*) 82.6(1) ? ? ? yes Bi(1) Se(1) C(1) 95.3(5) ? ? ? yes Bi(1) Se(1) C(2) 97.0(5) ? ? ? yes C(1) Se(1) C(2) 97.3(7) ? ? ? yes Bi(1) Se(2) C(4) 98.2(5) ? ? ? yes Bi(1) Se(2) C(5) 98.4(6) ? ? ? yes C(4) Se(2) C(5) 96.6(7) ? ? ? yes Bi(1) Cl(3) Bi(1) 97.4(1) ? ? ? yes Se(1) C(2) C(3) 112(1) ? ? ? yes C(2) C(3) C(4) 113(1) ? ? ? yes Se(2) C(4) C(3) 112(1) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_contact_author ; Dr Gillian Reid Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; CIF file for [BiCl3{MeSe(CH2)3SeMe}]. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' loop_ __publ_section_experimental ; Largest peaks of unassigned electron density adjacent to Bi. ; data_abbi1_BiCl3_+_se3-tripod #------------------------------------------------------------------------------ _audit_creation_date 'Wed Jun 16 14:03:14 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 11.402(7) _cell_length_b 16.919(5) _cell_length_c 11.893(6) _cell_angle_alpha 90 _cell_angle_beta 99.23(4) _cell_angle_gamma 90 _cell_volume 2264(1) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 18 _cell_measurement_2theta_min 13.9 _cell_measurement_2theta_max 17.2 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _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, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.040 _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 666.45 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H18 Bi Cl3 Se3 ' _chemical_formula_moiety 'C8 H18 Bi Cl3 Se3 ' _chemical_formula_structural '[BiCl3(MeC(CH2SeMe)3]' _chemical_compound_source ? _exptl_crystal_F_000 1208.00 _exptl_absorpt_coefficient_mu 12.928 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.254 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.53 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 6 0 0 5 2 2 5 0 _diffrn_reflns_number 4352 _reflns_number_total 4136 _reflns_number_observed 1880 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0884 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.07359 _diffrn_orient_matrix_UB_12 0.03249 _diffrn_orient_matrix_UB_13 0.02044 _diffrn_orient_matrix_UB_21 -0.00643 _diffrn_orient_matrix_UB_22 0.01755 _diffrn_orient_matrix_UB_23 -0.08105 _diffrn_orient_matrix_UB_31 -0.04937 _diffrn_orient_matrix_UB_32 0.04615 _diffrn_orient_matrix_UB_33 0.01643 #------------------------------------------------------------------------------ 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 32 0.003 0.002 'International Tables' H 0 72 0.000 0.000 'International Tables' Se 0 12 -0.093 2.226 'International Tables' Bi 0 4 -4.108 10.257 'International Tables' Cl 0 12 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Bi(1) 0.1095(1) 0.04207(7) 0.3660(1) 0.0305(4) Uij ? ? Se(1) 0.1980(3) -0.0840(2) 0.2285(4) 0.040(1) Uij ? ? Se(2) 0.4644(3) -0.2848(2) 0.5895(4) 0.043(1) Uij ? ? Se(4) 0.2555(3) -0.0656(2) 0.5555(4) 0.036(1) Uij ? ? Cl(1) 0.3158(8) 0.1039(5) 0.3451(10) 0.050(3) Uij ? ? Cl(2) 0.001(1) 0.0799(6) 0.1688(10) 0.063(4) Uij ? ? Cl(3) -0.0605(7) -0.0726(5) 0.3843(9) 0.038(3) Uij ? ? C(1) 0.376(3) -0.107(2) 0.469(3) 0.04(1) Uij ? ? C(2) 0.339(3) -0.185(2) 0.401(3) 0.04(1) Uij ? ? C(3) 0.210(3) -0.173(2) 0.334(3) 0.04(1) Uij ? ? C(4) 0.430(3) -0.205(2) 0.331(3) 0.04(1) Uij ? ? C(5) 0.359(3) 0.014(2) 0.641(3) 0.05(1) Uij ? ? C(6) 0.324(3) -0.255(2) 0.481(4) 0.05(1) Uij ? ? C(7) 0.053(3) -0.123(2) 0.140(3) 0.05(1) Uij ? ? C(8) 0.435(4) -0.227(2) 0.722(4) 0.06(2) Uij ? ? H(1) 0.3911 -0.0674 0.4165 0.0420 UiSO ? ? H(2) 0.4464 -0.1170 0.5215 0.0420 UiSO ? ? H(3) 0.1570 -0.1645 0.3869 0.0451 UiSO ? ? H(4) 0.1868 -0.2200 0.2916 0.0451 UiSO ? ? H(5) 0.4060 -0.2510 0.2873 0.0533 UiSO ? ? H(6) 0.4381 -0.1622 0.2806 0.0533 UiSO ? ? H(7) 0.5034 -0.2144 0.3784 0.0533 UiSO ? ? H(8) 0.4259 -0.0116 0.6833 0.0581 UiSO ? ? H(9) 0.3844 0.0502 0.5891 0.0581 UiSO ? ? H(10) 0.3160 0.0410 0.6910 0.0581 UiSO ? ? H(11) 0.3007 -0.2998 0.4348 0.0599 UiSO ? ? H(12) 0.2632 -0.2418 0.5235 0.0599 UiSO ? ? H(13) -0.0060 -0.1288 0.1883 0.0633 UiSO ? ? H(14) 0.0251 -0.0867 0.0810 0.0633 UiSO ? ? H(15) 0.0669 -0.1728 0.1081 0.0633 UiSO ? ? H(16) 0.4983 -0.2350 0.7830 0.0697 UiSO ? ? H(17) 0.4283 -0.1719 0.7046 0.0697 UiSO ? ? H(18) 0.3626 -0.2446 0.7440 0.0697 UiSO ? ? 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) 0.0290(7) 0.0184(6) 0.0442(9) -0.0008(7) 0.0057(6) 0.0004(8) Se(1) 0.048(2) 0.026(2) 0.050(3) 0.005(2) 0.017(2) 0.002(2) Se(2) 0.038(2) 0.020(2) 0.069(4) -0.002(2) 0.001(2) 0.003(2) Se(4) 0.030(2) 0.021(2) 0.057(3) 0.000(1) 0.006(2) -0.002(2) Cl(1) 0.035(6) 0.036(5) 0.080(9) -0.006(4) 0.012(6) 0.006(6) Cl(2) 0.093(9) 0.029(5) 0.059(9) 0.006(6) -0.014(7) -0.004(5) Cl(3) 0.031(5) 0.027(5) 0.056(7) -0.009(4) 0.011(5) -0.007(5) C(1) 0.02(2) 0.02(2) 0.06(3) -0.01(1) 0.01(2) 0.00(2) C(2) 0.06(3) 0.03(2) 0.02(3) -0.01(2) 0.00(2) 0.00(2) C(3) 0.08(3) 0.02(2) 0.02(2) 0.01(2) 0.01(2) 0.00(2) C(4) 0.03(2) 0.05(2) 0.06(3) 0.00(2) 0.01(2) 0.01(2) C(5) 0.06(3) 0.06(3) 0.03(3) 0.01(2) 0.00(2) 0.00(2) C(6) 0.03(2) 0.02(2) 0.11(4) 0.00(2) 0.02(2) -0.01(2) C(7) 0.07(3) 0.04(2) 0.04(3) -0.01(2) -0.01(2) -0.01(2) C(8) 0.07(3) 0.03(2) 0.07(4) -0.02(2) 0.00(3) 0.01(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _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 1880 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0598 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0877 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.568 _refine_ls_shift/esd_max 0.0070 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.34 _refine_diff_density_max 3.45 #------------------------------------------------------------------------------ _geom_special_details ? 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) Se(1) 2.962(4) ? ? yes Bi(1) Se(2*) 3.117(4) ? ? yes Bi(1) Se(4) 3.156(4) ? ? yes Bi(1) Cl(1) 2.622(9) ? ? yes Bi(1) Cl(2) 2.55(1) ? ? yes Bi(1) Cl(3) 2.776(8) ? ? yes Bi(1*) Cl(3) 3.151(10) ? ? yes Se(1) C(3) 1.95(3) ? ? yes Se(1) C(7) 1.93(4) ? ? yes Se(2) C(6) 1.95(4) ? ? yes Se(2) C(8) 1.93(5) ? ? yes Se(4) C(1) 1.97(3) ? ? yes Se(4) C(5) 1.96(4) ? ? yes C(1) C(2) 1.57(5) ? ? yes C(2) C(3) 1.57(5) ? ? yes C(2) C(4) 1.47(5) ? ? yes C(2) C(6) 1.55(5) ? ? yes #------------------------------------------------------------------------------ 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) Bi(1) Se(2*) 153.6(1) ? ? ? yes Se(1) Bi(1) Se(4) 78.0(1) ? ? ? yes Se(1) Bi(1) Cl(1) 81.1(2) ? ? ? yes Se(1) Bi(1) Cl(2) 80.3(3) ? ? ? yes Se(1) Bi(1) Cl(3) 81.0(2) ? ? ? yes Se(1) Bi(1) Cl(3*) 140.0(2) ? ? ? yes Se(2) Bi(1) Se(4) 123.2(1) ? ? ? yes Se(2) Bi(1) Cl(1) 85.0(2) ? ? ? yes Se(2) Bi(1) Cl(2) 79.4(2) ? ? ? yes Se(2) Bi(1) Cl(3) 115.6(2) ? ? ? yes Se(2) Bi(1) Cl(3*) 65.9(2) ? ? ? yes Se(4) Bi(1) Cl(1) 85.4(2) ? ? ? yes Se(4) Bi(1) Cl(2) 157.5(2) ? ? ? yes Se(4) Bi(1) Cl(3) 80.5(2) ? ? ? yes Se(4) Bi(1) Cl(3*) 64.8(2) ? ? ? yes Cl(1) Bi(1) Cl(2) 97.1(4) ? ? ? yes Cl(1) Bi(1) Cl(3) 159.2(3) ? ? ? yes Cl(1) Bi(1) Cl(3*) 108.8(3) ? ? ? yes Cl(2) Bi(1) Cl(3) 90.3(3) ? ? ? yes Cl(2) Bi(1) Cl(3*) 133.7(3) ? ? ? yes Cl(3) Bi(1) Cl(3*) 79.0(3) ? ? ? yes Bi(1) Se(1) C(3) 101.4(10) ? ? ? yes Bi(1) Se(1) C(7) 101(1) ? ? ? yes C(3) Se(1) C(7) 92(1) ? ? ? yes Bi(1) Se(2) C(6) 98.0(10) ? ? ? yes Bi(1) Se(2) C(8) 104(1) ? ? ? yes C(6) Se(2) C(8) 100(1) ? ? ? yes Bi(1) Se(4) C(1) 99(1) ? ? ? yes Bi(1) Se(4) C(5) 100(1) ? ? ? yes C(1) Se(4) C(5) 95(1) ? ? ? yes Bi(1) Cl(3) Bi(1) 101.0(3) ? ? ? yes Se(4) C(1) C(2) 114(2) ? ? ? yes C(1) C(2) C(3) 108(2) ? ? ? yes C(1) C(2) C(4) 109(2) ? ? ? yes C(1) C(2) C(6) 112(3) ? ? ? yes C(3) C(2) C(4) 115(3) ? ? ? yes C(3) C(2) C(6) 103(2) ? ? ? yes C(4) C(2) C(6) 109(3) ? ? ? yes Se(1) C(3) C(2) 112(2) ? ? ? yes Se(2) C(6) C(2) 116(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_contact_author ; DR GILLIAN REID DEPARTMENT OF CHEMISTRY UNIVERSITY OF SOUTHAMPTON HIGHFIELD SOUTHAMPTON SO17 1BJ ; _publ_contact_letter ; CIF file for [BiCl3{MeC(CH2SeMe)3}] ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' _publ_section_experimental ; Largest unassinged electron density adjacent to Bi. ; data_bii3se3_BiI3_+_MeC(CH2SeMe)3 #------------------------------------------------------------------------------ _audit_creation_date '19100-01-25' _audit_creation_method 'by teXsan v1.8' #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UK ; _publ_contact_letter ; This is the CIF file for [Bi2I6{MeC(CH2SeMe)3}2] included as a footnote in Dalton manuscript no. 9/09803H. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 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 10.59(1) _cell_length_b 8.717(4) _cell_length_c 21.40(1) _cell_angle_alpha 90 _cell_angle_beta 97.93(6) _cell_angle_gamma 90 _cell_volume 1956(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 14 _cell_measurement_theta_min 7.1 _cell_measurement_theta_max 11.7 #------------------------------------------------------------------------------ _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 'red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 3.194 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 940.80 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H18 Bi I3 Se3 ' _chemical_formula_moiety 'C8 H18 Bi I3 Se3 ' _chemical_formula_structural '[Bi2I6{MeC(CH2SeMe)3}2]' _chemical_compound_source 'recrystallisation from MeCN' _exptl_crystal_F_000 1640.00 _exptl_absorpt_coefficient_mu 19.295 _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 0.352 _exptl_special_details ; The scan width was (1.47+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 ; Rather poor quality crystals, weakly diffracting. Bi, I and Se atoms refined anisotropically. ; _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_% -1.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 0 12 -3 0 6 -2 1 11 _diffrn_reflns_number 3029 _reflns_number_total 2961 _reflns_number_gt 700 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.12563 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06456 _diffrn_orient_matrix_UB_12 0.08319 _diffrn_orient_matrix_UB_13 0.00188 _diffrn_orient_matrix_UB_21 -0.06138 _diffrn_orient_matrix_UB_22 -0.05661 _diffrn_orient_matrix_UB_23 -0.03152 _diffrn_orient_matrix_UB_31 -0.03401 _diffrn_orient_matrix_UB_32 -0.05508 _diffrn_orient_matrix_UB_33 0.03507 #------------------------------------------------------------------------------ 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 32 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 72 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Se 0 12 -0.178 2.223 ;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) 0.0587(4) 0.5244(4) 0.1006(2) 0.022(1) 1.000 . Uani d ? I(1) 0.2003(8) 0.3408(7) 0.2011(3) 0.034(3) 1.000 . Uani d ? I(2) 0.0394(8) 0.2356(6) 0.0125(3) 0.039(3) 1.000 . Uani d ? I(3) -0.1878(8) 0.5184(8) 0.1469(3) 0.046(3) 1.000 . Uani d ? Se(1) 0.132(1) 0.797(1) 0.1802(4) 0.028(4) 1.000 . Uani d ? Se(2) 0.324(1) 0.606(1) 0.0538(5) 0.040(4) 1.000 . Uani d ? Se(3) 0.624(1) 0.925(1) 0.0892(6) 0.062(5) 1.000 . Uani d ? C(1) 0.42(1) 0.91(1) 0.205(4) 0.05(3) 1.000 . Uiso d ? C(2) 0.381(9) 0.864(8) 0.136(4) 0.01(2) 1.000 . Uiso d ? C(3) 0.22(1) 0.90(1) 0.121(4) 0.05(3) 1.000 . Uiso d ? C(4) 0.412(9) 0.694(9) 0.130(4) 0.03(3) 1.000 . Uiso d ? C(5) 0.44(1) 0.966(9) 0.088(4) 0.03(3) 1.000 . Uiso d ? C(6) 0.00(1) 0.93(1) 0.158(4) 0.05(3) 1.000 . Uiso d ? C(7) 0.43(1) 0.40(1) 0.065(5) 0.09(4) 1.000 . Uiso d ? C(8) 0.69(1) 1.13(1) 0.128(6) 0.11(5) 1.000 . Uiso d ? H(1) 0.3852 0.8474 0.2331 0.046 1.000 . Uiso c ? H(2) 0.5168 0.8932 0.2149 0.046 1.000 . Uiso c ? H(3) 0.4094 1.0149 0.2136 0.046 1.000 . Uiso c ? H(4) 0.1890 0.8767 0.0768 0.031 1.000 . Uiso c ? H(5) 0.2066 1.0164 0.1221 0.031 1.000 . Uiso c ? H(6) 0.3934 0.6358 0.1646 0.026 1.000 . Uiso c ? H(7) 0.5044 0.6807 0.1280 0.026 1.000 . Uiso c ? H(8) 0.4125 1.0779 0.0962 0.038 1.000 . Uiso c ? H(9) 0.3814 0.9514 0.0453 0.038 1.000 . Uiso c ? H(10) 0.0222 1.0312 0.1638 0.031 1.000 . Uiso c ? H(11) -0.0311 0.9160 0.1114 0.031 1.000 . Uiso c ? H(12) -0.0722 0.9044 0.1781 0.031 1.000 . Uiso c ? H(13) 0.4160 0.3465 0.1086 0.077 1.000 . Uiso c ? H(14) 0.4024 0.3195 0.0363 0.077 1.000 . Uiso c ? H(15) 0.5189 0.4085 0.0702 0.077 1.000 . Uiso c ? H(16) 0.7854 1.1237 0.1325 0.084 1.000 . Uiso c ? H(17) 0.6642 1.2088 0.1010 0.084 1.000 . Uiso c ? H(18) 0.6679 1.1399 0.1681 0.084 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) 0.028(4) 0.020(2) 0.020(2) 0.000(3) 0.003(2) -0.002(2) I(1) 0.041(7) 0.039(5) 0.021(5) 0.007(4) -0.002(4) 0.005(3) I(2) 0.068(8) 0.028(4) 0.017(4) 0.004(4) -0.007(4) 0.000(3) I(3) 0.044(7) 0.039(5) 0.055(5) -0.002(4) 0.013(5) 0.001(4) Se(1) 0.03(1) 0.034(6) 0.020(6) 0.002(6) -0.002(6) -0.004(6) Se(2) 0.05(1) 0.024(6) 0.055(9) 0.000(6) 0.021(7) -0.008(6) Se(3) 0.05(1) 0.060(9) 0.08(1) 0.001(8) 0.019(8) -0.003(8) #------------------------------------------------------------------------------ _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 700 _refine_ls_number_parameters 96 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_all 0.0742 _refine_ls_wR_factor_ref 0.0742 _refine_ls_goodness_of_fit_all 2.471 _refine_ls_goodness_of_fit_ref 2.471 _refine_ls_shift/su_max 0.0238 _refine_ls_shift/su_mean 0.0049 _refine_diff_density_min -2.33 _refine_diff_density_max 2.20 #------------------------------------------------------------------------------ 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) 2.923(7) . . yes Bi(1) I(2) 3.133(7) . . yes Bi(1) I(2) 3.260(7) . 3_565 yes Bi(1) I(3) 2.917(9) . . yes Bi(1) Se(1) 2.96(1) . . yes Bi(1) Se(2) 3.19(1) . . yes Se(1) C(3) 1.93(9) . . yes Se(1) C(6) 1.8(1) . . yes Se(2) C(4) 1.92(9) . . yes Se(2) C(7) 2.1(1) . . yes Se(3) C(5) 2.0(1) . . yes Se(3) C(8) 2.0(1) . . yes C(1) C(2) 1.5(1) . . yes C(1) H(1) 0.93 . . no C(1) H(2) 0.97 . . no C(1) H(3) 0.98 . . no C(2) C(3) 1.7(1) . . yes C(2) C(4) 1.53(9) . . yes C(2) C(5) 1.5(1) . . yes C(3) H(4) 1.00 . . no C(3) H(5) 1.01 . . no C(4) H(6) 0.94 . . no C(4) H(7) 0.99 . . no C(5) H(8) 1.03 . . no C(5) H(9) 1.02 . . no C(6) H(10) 0.93 . . no C(6) H(11) 1.02 . . no C(6) H(12) 0.96 . . no C(7) H(13) 1.06 . . no C(7) H(14) 0.92 . . no C(7) H(15) 0.98 . . no C(8) H(16) 1.02 . . no C(8) H(17) 0.94 . . no C(8) H(18) 0.92 . . 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) 89.3(2) . . . yes I(1) Bi(1) I(2) 167.5(3) . . 3_565 yes I(1) Bi(1) I(3) 97.5(2) . . . yes I(1) Bi(1) Se(1) 87.0(2) . . . yes I(1) Bi(1) Se(2) 88.3(3) . . . yes I(2) Bi(1) I(2) 94.6(2) . . 3_565 yes I(2) Bi(1) I(3) 101.6(3) . . . yes I(2) Bi(1) Se(1) 168.3(3) . . . yes I(2) Bi(1) Se(2) 88.7(3) . . . yes I(2) Bi(1) I(3) 93.3(3) 3_565 . . yes I(2) Bi(1) Se(1) 86.8(2) 3_565 . . yes I(2) Bi(1) Se(2) 80.0(3) 3_565 . . yes I(3) Bi(1) Se(1) 89.9(3) . . . yes I(3) Bi(1) Se(2) 168.2(3) . . . yes Se(1) Bi(1) Se(2) 80.1(3) . . . yes Bi(1) I(2) Bi(1) 85.4(2) . . 3_565 yes Bi(1) Se(1) C(3) 97(3) . . . yes Bi(1) Se(1) C(6) 103(3) . . . yes C(3) Se(1) C(6) 88(4) . . . yes Bi(1) Se(2) C(4) 100(3) . . . yes Bi(1) Se(2) C(7) 103(3) . . . yes C(4) Se(2) C(7) 94(4) . . . yes C(5) Se(3) C(8) 97(4) . . . yes C(2) C(1) H(1) 112.5 . . . no C(2) C(1) H(2) 109.4 . . . no C(2) C(1) H(3) 111.8 . . . no H(1) C(1) H(2) 108.8 . . . no H(1) C(1) H(3) 108.6 . . . no H(2) C(1) H(3) 105.4 . . . no C(1) C(2) C(3) 107(7) . . . yes C(1) C(2) C(4) 106(7) . . . yes C(1) C(2) C(5) 115(7) . . . yes C(3) C(2) C(4) 113(7) . . . yes C(3) C(2) C(5) 103(7) . . . yes C(4) C(2) C(5) 113(7) . . . yes Se(1) C(3) C(2) 111(6) . . . yes Se(1) C(3) H(4) 111.5 . . . no Se(1) C(3) H(5) 110.6 . . . no C(2) C(3) H(4) 111.1 . . . no C(2) C(3) H(5) 111.1 . . . no H(4) C(3) H(5) 101.0 . . . no Se(2) C(4) C(2) 112(6) . . . yes Se(2) C(4) H(6) 108.8 . . . no Se(2) C(4) H(7) 106.7 . . . no C(2) C(4) H(6) 112.8 . . . no C(2) C(4) H(7) 109.6 . . . no H(6) C(4) H(7) 106.7 . . . no Se(3) C(5) C(2) 111(6) . . . yes Se(3) C(5) H(8) 116.4 . . . no Se(3) C(5) H(9) 116.8 . . . no C(2) C(5) H(8) 106.8 . . . no C(2) C(5) H(9) 106.5 . . . no H(8) C(5) H(9) 98.0 . . . no Se(1) C(6) H(10) 114.8 . . . no Se(1) C(6) H(11) 109.7 . . . no Se(1) C(6) H(12) 112.7 . . . no H(10) C(6) H(11) 105.5 . . . no H(10) C(6) H(12) 110.1 . . . no H(11) C(6) H(12) 103.2 . . . no Se(2) C(7) H(13) 110.1 . . . no Se(2) C(7) H(14) 117.8 . . . no Se(2) C(7) H(15) 114.4 . . . no H(13) C(7) H(14) 103.4 . . . no H(13) C(7) H(15) 99.3 . . . no H(14) C(7) H(15) 109.6 . . . no Se(3) C(8) H(16) 108.1 . . . no Se(3) C(8) H(17) 112.1 . . . no Se(3) C(8) H(18) 113.4 . . . no H(16) C(8) H(17) 104.2 . . . no H(16) C(8) H(18) 105.8 . . . no H(17) C(8) H(18) 112.5 . . . no