#Copyright The Royal Society of Chemistry, 1998 #(Me3S)[Cd2I6]1/2.3I2 data_(1) #------------------------------------------------------------------------------ _audit_creation_date 'Thu Jul 31 23:09:20 1997' _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 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 8.9662(8) _cell_length_b 19.843(2) _cell_length_c 12.896(2) _cell_angle_alpha 90 _cell_angle_beta 92.778(7) _cell_angle_gamma 90 _cell_volume 2291.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 12.2 _cell_measurement_theta_max 18.1 #------------------------------------------------------------------------------ _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 'rectangular' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 3.851 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 1328.69 _chemical_formula_analytical ? _chemical_formula_sum 'C3 H6 Cd I9 S ' _chemical_formula_moiety '?' _exptl_crystal_F_000 2260.00 _exptl_absorpt_coefficient_mu 13.153 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.698 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintillation _diffrn_measurement_device 'CAD4' _diffrn_measurement_method '\w-2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count '120 min' _diffrn_standards_decay_% -4.71 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -18 1 -7 -4 -5 2 -3 -7 _diffrn_reflns_number 5080 _reflns_number_total 4784 _reflns_number_observed 3499 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 4.58 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.24 _diffrn_orient_matrix_UB_11 -0.03841 _diffrn_orient_matrix_UB_12 -0.00420 _diffrn_orient_matrix_UB_13 -0.07374 _diffrn_orient_matrix_UB_21 0.00876 _diffrn_orient_matrix_UB_22 -0.05013 _diffrn_orient_matrix_UB_23 0.00491 _diffrn_orient_matrix_UB_31 -0.10457 _diffrn_orient_matrix_UB_32 -0.00265 _diffrn_orient_matrix_UB_33 0.02356 #------------------------------------------------------------------------------ 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 Cd 0 4 -0.807 1.202 'International Tables' I 0 36 -0.474 1.812 'International Tables' S 0 4 0.125 0.123 'International Tables' C 0 12 0.003 0.002 'International Tables' H 0 24 0.000 0.000 '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 I(1) -0.49401(11) -0.202026(48) 0.416531(76) 1.95(4) Beq ? ? I(2) -0.52167(10) -0.129485(48) 0.747640(75) 1.88(4) Beq ? ? I(3) -0.26486(11) -0.000280(47) 0.507556(80) 1.95(4) Beq ? ? I(4) 0.47349(11) -0.154818(53) 0.073741(80) 2.21(4) Beq ? ? I(5) 0.49019(12) -0.029697(54) 0.163474(83) 2.43(4) Beq ? ? I(6) 0.11055(12) -0.132574(59) -0.045874(83) 2.61(5) Beq ? ? I(7) -0.17176(12) -0.129163(57) -0.135247(87) 2.60(5) Beq ? ? I(8) 0.12962(11) -0.177628(53) 0.638185(82) 2.23(4) Beq ? ? I(9) -0.14627(11) -0.200510(49) 0.546014(79) 1.99(4) Beq ? ? Cd(1) -0.49865(12) -0.092244(53) 0.543647(88) 1.85(5) Beq ? ? S(1) -0.02356(42) -0.10050(20) 0.31495(30) 2.0(2) Beq ? ? C(1) 0.1416(19) -0.1424(11) 0.2795(17) 4(1) Beq ? ? C(2) -0.1606(17) -0.15318(89) 0.2464(14) 3.0(8) Beq ? ? C(3) -0.0273(30) -0.0253(10) 0.2360(15) 5(1) Beq ? ? 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 I(1) 0.0294(5) 0.0193(5) 0.0250(5) 0.0028(4) -0.0012(4) -0.0037(4) I(2) 0.0244(5) 0.0270(5) 0.0201(5) -0.0031(4) -0.0005(4) 0.0030(4) I(3) 0.0227(5) 0.0198(5) 0.0318(6) 0.0006(4) 0.0027(4) 0.0006(4) I(4) 0.0250(5) 0.0324(6) 0.0262(6) 0.0008(4) -0.0006(4) -0.0033(4) I(5) 0.0315(6) 0.0337(6) 0.0270(6) 0.0053(5) 0.0001(4) -0.0045(5) I(6) 0.0277(5) 0.0454(7) 0.0262(6) -0.0040(5) 0.0013(4) 0.0029(5) I(7) 0.0257(5) 0.0372(6) 0.0360(6) -0.0002(4) 0.0041(5) 0.0115(5) I(8) 0.0242(5) 0.0301(6) 0.0303(6) -0.0026(4) 0.0007(4) 0.0019(5) I(9) 0.0255(5) 0.0224(5) 0.0275(6) -0.0008(4) 0.0003(4) 0.0010(4) Cd(1) 0.0308(6) 0.0174(6) 0.0223(6) -0.0003(4) 0.0022(5) 0.0000(5) S(1) 0.028(2) 0.028(2) 0.021(2) 0.000(2) 0.004(2) 0.000(2) C(1) 0.021(9) 0.07(1) 0.07(1) 0.003(9) -0.002(9) -0.02(1) C(2) 0.024(8) 0.04(1) 0.04(1) -0.006(7) -0.005(8) -0.022(9) C(3) 0.13(2) 0.04(1) 0.03(1) -0.02(1) -0.02(1) 0.023(9) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment 'H-atoms not located' _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 0.71139E-7 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3499 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0388 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0592 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.131 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.60 _refine_diff_density_max 1.81 #------------------------------------------------------------------------------ _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 I(1) I(4) 3.510(2) ? ? yes I(1) I(9) 3.465(1) ? ? yes I(1) Cd(1) 2.728(1) ? ? yes I(2) I(5) 3.367(2) ? ? yes I(2) I(7) 3.415(1) ? ? yes I(2) I(8) 3.500(1) ? ? yes I(2) Cd(1) 2.750(2) ? ? yes I(3) Cd(1) 2.835(1) ? ? yes I(3) Cd(1) 2.858(1) ? ? yes I(4) I(5) 2.740(2) ? ? yes I(4) I(6) 3.561(1) ? ? yes I(6) I(7) 2.731(2) ? ? yes I(8) I(9) 2.730(1) ? ? yes Cd(1) Cd(1) 3.830(2) ? ? yes I(9) S(1) 3.788(4) ? ? yes S(1) C(1) 1.78(2) ? ? yes S(1) C(2) 1.81(2) ? ? yes S(1) C(3) 1.80(2) ? ? yes C(1) C(2) 2.73(2) ? ? yes C(1) C(3) 2.81(3) ? ? yes C(2) C(3) 2.81(3) ? ? 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 I(4) I(1) I(9) 80.02(3) ? ? ? yes I(4) I(1) Cd(1) 107.16(4) ? ? ? yes I(9) I(1) Cd(1) 75.11(4) ? ? ? yes I(5) I(2) I(7) 77.74(3) ? ? ? yes I(5) I(2) I(8) 116.86(4) ? ? ? yes I(5) I(2) Cd(1) 93.71(4) ? ? ? yes I(7) I(2) I(8) 164.20(4) ? ? ? yes I(7) I(2) Cd(1) 108.22(4) ? ? ? yes I(8) I(2) Cd(1) 78.14(4) ? ? ? yes Cd(1) I(3) Cd(1) 84.56(4) ? ? ? yes I(1) I(4) I(5) 166.59(5) ? ? ? yes I(1) I(4) I(6) 87.12(3) ? ? ? yes I(5) I(4) I(6) 95.78(4) ? ? ? yes I(2) I(5) I(4) 174.62(5) ? ? ? yes I(4) I(6) I(7) 174.23(5) ? ? ? yes I(2) I(7) I(6) 178.01(5) ? ? ? yes I(2) I(8) I(9) 173.58(5) ? ? ? yes I(1) I(9) I(8) 170.56(4) ? ? ? yes I(1) I(9) S(1) 85.08(6) ? ? ? yes I(8) I(9) S(1) 87.92(7) ? ? ? yes I(1) Cd(1) I(2) 111.37(5) ? ? ? yes I(1) Cd(1) I(3) 112.49(5) ? ? ? yes I(1) Cd(1) I(3) 114.01(5) ? ? ? yes I(2) Cd(1) I(3) 114.86(5) ? ? ? yes I(2) Cd(1) I(3) 107.72(5) ? ? ? yes I(3) Cd(1) I(3) 95.44(4) ? ? ? yes I(9) S(1) C(1) 103.6(8) ? ? ? yes I(9) S(1) C(2) 82.3(6) ? ? ? yes I(9) S(1) C(3) 151.4(9) ? ? ? yes C(1) S(1) C(2) 99.1(8) ? ? ? yes C(1) S(1) C(3) 103(1) ? ? ? yes C(2) S(1) C(3) 102.0(9) ? ? ? yes S(1) C(1) C(2) 40.9(5) ? ? ? yes S(1) C(1) C(3) 38.6(7) ? ? ? yes C(2) C(1) C(3) 60.9(7) ? ? ? yes S(1) C(2) C(1) 40.0(5) ? ? ? yes S(1) C(2) C(3) 38.9(6) ? ? ? yes C(1) C(2) C(3) 61.0(8) ? ? ? yes S(1) C(3) C(1) 37.9(7) ? ? ? yes S(1) C(3) C(2) 39.1(6) ? ? ? yes C(1) C(3) C(2) 58.1(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _public_contact_author ; Lars Bengtsson-Kloo Chemical Center University of Lund P.O. 124 S - 22100 Lund Sweden ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' + 46-46-108157 ' _publ_contact_author_fax ' + 46-46-104439 ' _publ_contact_author_email ' Lars.kloo inorg.lu.se ' loop_ _publ_author_name _publ_author_address 'Per H. Svensson' ; Inorganic Chemistry 1 Center for Chemistry and Chemical Engineering Lund University P.O. Box 124 S-221 00 Lund, Sweden ; 'Lars Bengtsson-Kloo' ; Inorganic Chemistry 1 Center for Chemistry and Chemical Engineering Lund University P.O. Box 124 S-221 00 Lund, Sweden ; 'Per Persson' ; Inorganic Chemistry Umea University S-901 87 Umea, Sweden ; _publ_section_title ; Metal Iodides in Polyiodide Networks - The Structural Chemistry of CdI2 with Excess of Iodine. ; #(Et3S)[Cd2I6]1/2 data_(2) #------------------------------------------------------------------------------ _audit_creation_date 'Fri Aug 1 11:09:28 1997' _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 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 7.885(1) _cell_length_b 13.233(6) _cell_length_c 14.862(3) _cell_angle_alpha 90 _cell_angle_beta 96.05(1) _cell_angle_gamma 90 _cell_volume 1542.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 11.1 _cell_measurement_theta_max 18.1 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'rectangular' _exptl_crystal_colour 'transparent' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 2.637 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 1224.74 _chemical_formula_analytical ? _chemical_formula_sum 'C6 H15 Cd I3 S ' _chemical_compound_source ? _exptl_crystal_F_000 1096.00 _exptl_absorpt_coefficient_mu 7.522 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.654 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintillation _diffrn_measurement_device 'CAD4' _diffrn_measurement_method '\w-2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count '120 min' _diffrn_standards_decay_% 3.78 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -3 3 -1 3 3 -1 -3 3 _diffrn_reflns_number 3067 _reflns_number_total 2873 _reflns_number_observed 1123 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 6.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.97 _diffrn_orient_matrix_UB_11 -0.02178 _diffrn_orient_matrix_UB_12 0.07393 _diffrn_orient_matrix_UB_13 -0.00895 _diffrn_orient_matrix_UB_21 0.02086 _diffrn_orient_matrix_UB_22 0.01081 _diffrn_orient_matrix_UB_23 0.06683 _diffrn_orient_matrix_UB_31 0.12394 _diffrn_orient_matrix_UB_32 0.01118 _diffrn_orient_matrix_UB_33 -0.00546 #------------------------------------------------------------------------------ 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 Cd 0 4 -0.807 1.202 'International Tables' I 0 12 -0.474 1.812 'International Tables' C 0 24 0.003 0.002 'International Tables' S 0 4 0.125 0.123 'International Tables' H 0 60 0.000 0.000 '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 I(1) -0.04680(17) 0.39676(12) 0.253978(81) 4.67(6) Beq ? ? I(2) -0.23592(20) 0.22265(11) -0.002839(97) 5.13(8) Beq ? ? I(3) -0.24106(19) 0.57325(10) -0.00402(11) 5.46(8) Beq ? ? Cd(1) -0.08394(17) 0.39297(13) 0.069801(88) 4.19(7) Beq ? ? S(1) 0.20949(58) 0.17123(37) 0.15848(30) 3.8(2) Beq ? ? C(1a) 0.1590(32) 0.1113(22) 0.2631(17) 5.5(6) Beq ? ? C(1b) 0.3940(94) 0.5613(54) 0.3175(50) 2(1) Beq ? ? C(2) -0.0364(27) 0.0845(17) 0.2543(15) 7(1) Beq ? ? C(3a) 0.4389(39) 0.1932(25) 0.1785(21) 6.5(7) Beq ? ? C(3b) 0.1351(83) 0.6884(55) 0.2387(42) 4(1) Beq ? ? C(4) 0.4667(29) 0.2800(23) 0.2482(17) 9(2) Beq ? ? C(5a) 0.2163(40) 0.0621(22) 0.0836(21) 5.6(7) Beq ? ? C(5b) 0.155(10) 0.6145(66) 0.4163(54) 6.4(8) Beq ? ? C(6) 0.2602(28) 0.1002(20) -0.0114(12) 7(1) Beq ? ? 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 I(1) 0.0660(9) 0.0649(9) 0.0468(8) -0.0068(9) 0.0072(6) -0.0058(9) I(2) 0.071(1) 0.067(1) 0.0560(9) -0.0162(9) 0.0034(8) -0.0061(8) I(3) 0.0567(9) 0.066(1) 0.088(1) 0.0107(8) 0.0267(8) 0.0269(9) Cd(1) 0.0580(9) 0.0532(9) 0.0484(9) -0.0066(9) 0.0076(7) 0.0055(9) S(1) 0.048(3) 0.050(3) 0.049(3) -0.005(3) 0.012(3) 0.000(3) C(2) 0.07(2) 0.09(2) 0.10(2) -0.04(1) 0.03(1) 0.03(1) C(4) 0.06(2) 0.16(3) 0.11(2) -0.04(2) 0.02(1) -0.06(2) C(6) 0.11(2) 0.11(2) 0.04(1) -0.02(2) 0.02(1) 0.00(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment 'H-atoms not found' _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 0.45698E-7 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1123 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0411 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0445 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.311 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.83 _refine_diff_density_max 0.69 #------------------------------------------------------------------------------ _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 I(1) Cd(1) 2.723(2) ? ? yes I(2) Cd(1) 2.722(2) ? ? yes I(3) Cd(1) 2.854(2) ? ? yes I(3) Cd(1) 2.872(2) ? ? yes Cd(1) Cd(1) 3.829(3) ? ? yes S(1) C(1a) 1.83(3) ? ? yes S(1) C(2) 2.77(2) ? ? yes S(1) C(2b) 1.72(7) ? ? yes S(1) C(3b) 1.87(6) ? ? yes S(1) C(3a) 1.83(3) ? ? yes S(1) C(4) 2.72(2) ? ? yes S(1) C(5b) 1.79(8) ? ? yes S(1) C(5a) 1.83(3) ? ? yes S(1) C(6) 2.76(2) ? ? yes C(1a) C(2) 1.57(3) ? ? yes C(1a) C(2b) 1.39(7) ? ? yes C(1a) C(3b) 1.92(7) ? ? yes C(1a) C(3a) 2.87(4) ? ? yes C(1a) C(5b) 3.18(9) ? ? yes C(1a) C(5a) 2.83(4) ? ? yes C(2) C(2b) 1.66(8) ? ? yes C(2b) C(3b) 2.8(1) ? ? yes C(2b) C(3a) 3.16(8) ? ? yes C(2b) C(5b) 2.6(1) ? ? yes C(2b) C(5a) 1.79(8) ? ? yes C(2b) C(6) 3.28(8) ? ? yes C(3b) C(3a) 1.42(7) ? ? yes C(3b) C(4) 1.48(7) ? ? yes C(3b) C(5b) 2.80(10) ? ? yes C(3b) C(5a) 3.24(7) ? ? yes C(3a) C(4) 1.55(4) ? ? yes C(3a) C(5b) 1.84(9) ? ? yes C(3a) C(5a) 2.75(4) ? ? yes C(3a) C(6) 3.26(4) ? ? yes C(5b) C(5a) 1.23(8) ? ? yes C(5b) C(6) 1.51(8) ? ? yes C(5a) C(6) 1.57(3) ? ? 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 Cd(1) I(3) Cd(1) 83.93(6) ? ? ? yes I(1) Cd(1) I(3) 111.56(7) ? ? ? yes I(1) Cd(1) I(3) 109.51(6) ? ? ? yes I(1) Cd(1) I(2) 114.22(7) ? ? ? yes I(3) Cd(1) I(3) 96.07(6) ? ? ? yes I(3) Cd(1) I(2) 112.62(7) ? ? ? yes I(3) Cd(1) I(2) 111.42(7) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _public_contact_author ; Lars Bengtsson-Kloo Chemical Center University of Lund P.O. 124 S - 22100 Lund Sweden ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' + 46-46-108157 ' _publ_contact_author_fax ' + 46-46-104439 ' _publ_contact_author_email ' Lars.kloo inorg.lu.se ' loop_ _publ_author_name _publ_author_address 'Per H. Svensson' ; Inorganic Chemistry 1 Center for Chemistry and Chemical Engineering Lund University P.O. Box 124 S-221 00 Lund, Sweden ; 'Lars Bengtsson-Kloo' ; Inorganic Chemistry 1 Center for Chemistry and Chemical Engineering Lund University P.O. Box 124 S-221 00 Lund, Sweden ; 'Per Persson' ; Inorganic Chemistry Umea University S-901 87 Umea, Sweden ; _publ_section_title ; Metal Iodides in Polyiodide Networks - The Structural Chemistry of CdI2 with Excess of Iodine. ; _publ_section_exptl_refinement ; The carbon atoms closest to the sulfur atom in the cation exhibit a disorder over two distinct positions. H-atoms were not located and not put in calculated positions in the structure. ; #(Me3S)CdI3 data_(3) #------------------------------------------------------------------------------ _audit_creation_date 'Thu Sep 18 16:29:28 1997' _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 SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 8.941(2) _cell_length_b 17.112(3) _cell_length_c 8.388(2) _cell_angle_alpha 90 _cell_angle_beta 105.42(1) _cell_angle_gamma 90 _cell_volume 1237.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 12.3 _cell_measurement_theta_max 17.9 #------------------------------------------------------------------------------ _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 'Rectangular' _exptl_crystal_colour 'Transparent' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 3.061 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 570.29 _chemical_formula_analytical ? _chemical_formula_sum 'C3 H9 Cd I3 S ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1000.00 _exptl_absorpt_coefficient_mu 9.363 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.777 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation' _diffrn_measurement_device 'CAD4' _diffrn_measurement_method '\w-2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count '120 min' _diffrn_standards_decay_% 0.64 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -1 -5 4 5 -3 4 0 -4 _diffrn_reflns_number 4105 _reflns_number_total 3872 _reflns_number_observed 1339 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 4.90 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 30.44 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.06126 _diffrn_orient_matrix_UB_12 -0.04755 _diffrn_orient_matrix_UB_13 -0.04558 _diffrn_orient_matrix_UB_21 -0.09832 _diffrn_orient_matrix_UB_22 0.03029 _diffrn_orient_matrix_UB_23 -0.01511 _diffrn_orient_matrix_UB_31 -0.00417 _diffrn_orient_matrix_UB_32 -0.01502 _diffrn_orient_matrix_UB_33 0.11388 #------------------------------------------------------------------------------ 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 Cd 0 4 -0.807 1.202 'International Tables' I 0 12 -0.474 1.812 'International Tables' S 0 4 0.125 0.123 'International Tables' C 0 12 0.003 0.002 'International Tables' H 0 36 0.000 0.000 '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 I(1) 1.0058(1) 0.28210(6) 0.8399(1) 0 Uij ? ? I(2) 1.2340(1) 0.05247(6) 0.7192(1) 0 Uij ? ? I(3) 1.4581(1) 0.30064(6) 0.6833(1) 0 Uij ? ? Cd(1) 1.2093(2) 0.21019(7) 0.6783(2) 0 Uij ? ? S(1) 0.8144(8) 0.0804(4) 0.8032(9) 0 Uij ? ? S(2) 0.672(2) 0.0406(9) 0.739(2) 0 Uij ? ? C(1) 0.795(3) 0.519(1) 0.294(3) 0 Uij ? ? C(2) 0.720(3) 0.387(1) 0.104(2) 0 Uij ? ? C(3) 0.693(2) 0.3866(10) 0.424(2) 0 Uij ? ? 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 I(1) 0.0691(7) 0.0865(8) 0.0500(6) 0.0027(6) 0.0237(5) -0.0084(6) I(2) 0.117(1) 0.0544(6) 0.0716(8) 0.0015(6) 0.0312(8) 0.0018(5) I(3) 0.0798(9) 0.0762(7) 0.0789(8) -0.0087(6) 0.0365(7) 0.0091(6) Cd(1) 0.0802(9) 0.0604(8) 0.0841(9) -0.0001(7) 0.0388(8) 0.0006(7) S(1) 0.056(5) 0.054(4) 0.076(5) -0.006(4) 0.028(4) -0.004(4) S(2) 0.080(10) 0.11(1) 0.19(2) 0.013(9) 0.03(1) -0.01(1) C(1) 0.24(3) 0.07(1) 0.12(2) 0.00(2) 0.04(2) -0.01(1) C(2) 0.16(2) 0.10(1) 0.07(1) -0.03(1) 0.05(1) -0.01(1) C(3) 0.10(1) 0.11(1) 0.07(1) -0.02(1) 0.04(1) 0.01(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment 'H-atoms not found' _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 3.70811E-7 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1339 _refine_ls_number_parameters 83 _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 0.0450 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.014 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.24 _refine_diff_density_max 2.37 #------------------------------------------------------------------------------ _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 I1 Cd1 2.824(2) ? ? yes I1 Cd1 2.939(2) ? ? yes I2 Cd1 2.722(2) ? ? yes I3 Cd1 2.702(2) ? ? yes Cd1 Cd1 4.410(6) ? ? yes S1 S2 1.42(2) ? ? yes S1 C1 1.72(2) ? ? yes S1 C2 1.76(2) ? ? yes S1 C3 1.76(2) ? ? yes S2 C1 1.49(2) ? ? yes S2 C2 1.81(2) ? ? yes S2 C3 1.96(2) ? ? yes C1 C2 2.76(3) ? ? yes C1 C3 2.78(3) ? ? yes C2 C3 2.76(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 I1 Cd1 I2 114.35(5) ? ? ? yes I1 Cd1 I3 112.09(5) ? ? ? yes I2 Cd1 I3 121.82(6) ? ? ? yes I3 Cd1 I1 106.57(5) ? ? ? yes I2 Cd1 I1 100.07(5) ? ? ? yes I1 Cd1 I1 97.56(5) ? ? ? yes S2 S1 C1 55.8(10) ? ? ? yes S2 S1 C2 68.7(10) ? ? ? yes S2 S1 C3 75.0(9) ? ? ? yes C1 S1 C2 105(1) ? ? ? yes C1 S1 C3 105(1) ? ? ? yes C2 S1 C3 103.4(9) ? ? ? yes S1 S2 C1 72(1) ? ? ? yes S1 S2 C2 64.4(10) ? ? ? yes S1 S2 C3 60.4(8) ? ? ? yes C1 S2 C2 112(1) ? ? ? yes C1 S2 C3 106(1) ? ? ? yes C2 S2 C3 93(1) ? ? ? yes S1 C1 S2 52.0(9) ? ? ? yes S1 C1 C2 37.9(7) ? ? ? yes S1 C1 C3 37.5(6) ? ? ? yes S2 C1 C2 37.4(9) ? ? ? yes S2 C1 C3 42.5(9) ? ? ? yes C2 C1 C3 59.8(7) ? ? ? yes S1 C2 S2 46.9(7) ? ? ? yes S1 C2 C1 37.0(6) ? ? ? yes S1 C2 C3 38.4(5) ? ? ? yes S2 C2 C1 30.0(7) ? ? ? yes S2 C2 C3 45.0(7) ? ? ? yes C1 C2 C3 60.5(7) ? ? ? yes S1 C3 S2 44.6(6) ? ? ? yes S1 C3 C1 36.5(6) ? ? ? yes S1 C3 C2 38.2(6) ? ? ? yes S2 C3 C1 31.0(6) ? ? ? yes S2 C3 C2 41.0(7) ? ? ? yes C1 C3 C2 59.7(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _public_contact_author ; Lars Bengtsson-Kloo Chemical Center University of Lund P.O. 124 S - 22100 Lund Sweden ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' + 46-46-108157 ' _publ_contact_author_fax ' + 46-46-104439 ' _publ_contact_author_email ' Lars.kloo inorg.lu.se ' loop_ _publ_author_name _publ_author_address 'Per H. Svensson' ; Inorganic Chemistry 1 Center for Chemistry and Chemical Engineering Lund University P.O. Box 124 S-221 00 Lund, Sweden ; 'Lars Bengtsson-Kloo' ; Inorganic Chemistry 1 Center for Chemistry and Chemical Engineering Lund University P.O. Box 124 S-221 00 Lund, Sweden ; 'Per Persson' ; Inorganic Chemistry Umea University S-901 87 Umea, Sweden ; _publ_section_title ; Metal Iodides in Polyiodide Networks - The Structural Chemistry of CdI2 with Excess of Iodine. ; _publ_section_exptl_refinement ; The sulfur atom of the cation is disordered over two distinct positions. H-atoms were not located and not put in calculated positions in the structure. ; #(Me3S)CdI3 data_(4) #------------------------------------------------------------------------------ _audit_creation_date 'Thu Sep 18 16:34:46 1997' _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 SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 8.393(1) _cell_length_b 16.714(2) _cell_length_c 17.537(2) _cell_angle_alpha 90 _cell_angle_beta 102.54(1) _cell_angle_gamma 90 _cell_volume 2401.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10.4 _cell_measurement_theta_max 20.1 #------------------------------------------------------------------------------ _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 'Rectangular' _exptl_crystal_colour 'Transparent' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 3.155 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 570.29 _chemical_formula_analytical ? _chemical_formula_sum 'C3 H9 Cd I3 S ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2000.00 _exptl_absorpt_coefficient_mu 9.648 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.545 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintillation _diffrn_measurement_device 'CAD4' _diffrn_measurement_method '\w-2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count '120 min' _diffrn_standards_decay_% -1.82 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -5 -5 -2 -5 -4 -1 4 -7 _diffrn_reflns_number 4682 _reflns_number_total 4422 _reflns_number_observed 3325 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 3.19 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.02801 _diffrn_orient_matrix_UB_12 -0.05755 _diffrn_orient_matrix_UB_13 -0.01153 _diffrn_orient_matrix_UB_21 0.02619 _diffrn_orient_matrix_UB_22 0.00604 _diffrn_orient_matrix_UB_23 -0.05265 _diffrn_orient_matrix_UB_31 0.11588 _diffrn_orient_matrix_UB_32 -0.01527 _diffrn_orient_matrix_UB_33 0.02253 #------------------------------------------------------------------------------ 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 Cd 0 8 -0.807 1.202 'International Tables' I 0 24 -0.474 1.812 'International Tables' C 0 24 0.003 0.002 'International Tables' S 0 8 0.125 0.123 'International Tables' H 0 72 0.000 0.000 '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 I(1) 0.91050(8) 0.19797(4) 0.74393(4) 0 Uij ? ? I(2) 1.27580(9) 0.20029(4) 0.97965(4) 0 Uij ? ? I(3) 1.14884(9) 0.44269(4) 0.84541(4) 0 Uij ? ? I(4) 1.40585(8) 0.25728(4) 0.74419(4) 0 Uij ? ? I(5) 1.66919(9) 0.04031(4) 0.88507(4) 0 Uij ? ? I(6) 1.78714(9) 0.31008(4) 0.96178(4) 0 Uij ? ? Cd(1) 1.17414(10) 0.27901(4) 0.84336(5) 0 Uij ? ? Cd(2) 1.68853(9) 0.19843(4) 0.84913(5) 0 Uij ? ? S(1) 1.3457(4) 0.0275(2) 0.5785(2) 0 Uij ? ? S(2) 1.1592(3) -0.0952(1) 0.8431(2) 0 Uij ? ? C(1) 1.383(2) -0.0085(7) 0.6780(6) 0 Uij ? ? C(2) 1.496(1) 0.1039(6) 0.5817(7) 0 Uij ? ? C(3) 1.166(1) 0.0868(8) 0.5749(8) 0 Uij ? ? C(4) 1.344(1) -0.1337(6) 0.9028(6) 0 Uij ? ? C(5) 1.171(1) 0.0098(6) 0.8690(8) 0 Uij ? ? C(6) 1.008(1) -0.1285(6) 0.8942(6) 0 Uij ? ? 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 I(1) 0.0174(3) 0.0255(3) 0.0255(4) -0.0029(3) 0.0034(3) -0.0007(3) I(2) 0.0257(4) 0.0280(4) 0.0280(4) 0.0034(3) 0.0003(3) 0.0025(3) I(3) 0.0259(4) 0.0221(3) 0.0374(4) -0.0019(3) 0.0056(3) -0.0036(3) I(4) 0.0185(4) 0.0438(4) 0.0271(4) 0.0059(3) 0.0048(3) -0.0001(3) I(5) 0.0297(4) 0.0229(3) 0.0354(4) -0.0016(3) 0.0091(3) -0.0001(3) I(6) 0.0262(4) 0.0251(4) 0.0350(4) 0.0006(3) 0.0039(3) -0.0038(3) Cd(1) 0.0231(4) 0.0242(4) 0.0258(4) 0.0006(3) 0.0019(3) -0.0002(3) Cd(2) 0.0237(4) 0.0243(4) 0.0293(4) 0.0004(3) 0.0041(3) 0.0004(3) S(1) 0.052(2) 0.025(1) 0.027(2) -0.007(1) 0.010(1) -0.001(1) S(2) 0.022(1) 0.026(1) 0.025(1) 0.003(1) 0.000(1) 0.001(1) C(1) 0.055(8) 0.050(7) 0.018(6) 0.004(6) 0.008(6) 0.009(5) C(2) 0.016(6) 0.033(6) 0.059(8) 0.001(5) 0.011(6) 0.004(6) C(3) 0.023(7) 0.053(8) 0.066(9) 0.007(6) 0.001(6) 0.021(7) C(4) 0.021(6) 0.033(6) 0.027(6) 0.009(5) -0.001(5) 0.002(5) C(5) 0.035(7) 0.015(5) 0.062(9) 0.000(5) 0.012(6) -0.002(5) C(6) 0.015(5) 0.037(6) 0.037(7) -0.001(5) 0.008(5) 0.005(5) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment 'H-atoms not found' _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 1.21055E-7 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3325 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0352 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0426 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.792 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.17 _refine_diff_density_max 1.67 #------------------------------------------------------------------------------ _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 I(1) Cd(1) 2.845(1) ? ? yes I(1) Cd(2) 2.892(1) ? ? yes I(2) Cd(1) 2.699(1) ? ? yes I(3) Cd(1) 2.745(1) ? ? yes I(4) Cd(1) 2.899(1) ? ? yes I(4) Cd(2) 2.844(1) ? ? yes I(5) Cd(2) 2.730(1) ? ? yes I(6) Cd(2) 2.713(1) ? ? yes S(1) C(1) 1.81(1) ? ? yes S(1) C(2) 1.79(1) ? ? yes S(1) C(3) 1.80(1) ? ? yes S(2) C(4) 1.79(1) ? ? yes S(2) C(5) 1.81(1) ? ? yes S(2) C(6) 1.79(1) ? ? yes C(1) C(2) 2.83(2) ? ? yes C(1) C(3) 2.77(2) ? ? yes C(2) C(3) 2.76(2) ? ? yes C(4) C(5) 2.80(1) ? ? yes C(4) C(6) 2.79(1) ? ? yes C(5) C(6) 2.77(1) ? ? yes I(2) S(1) 4.858(3) ? ? 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 Cd(1) I(1) Cd(2) 97.51(3) ? ? ? yes Cd(1) I(4) Cd(2) 103.24(3) ? ? ? yes I(1) Cd(1) I(2) 111.40(3) ? ? ? yes I(1) Cd(1) I(3) 115.49(3) ? ? ? yes I(1) Cd(1) I(4) 96.11(3) ? ? ? yes I(2) Cd(1) I(3) 118.99(4) ? ? ? yes I(2) Cd(1) I(4) 110.23(3) ? ? ? yes I(3) Cd(1) I(4) 101.33(3) ? ? ? yes I(1) Cd(2) I(4) 98.66(3) ? ? ? yes I(1) Cd(2) I(5) 102.91(3) ? ? ? yes I(1) Cd(2) I(6) 109.23(3) ? ? ? yes I(4) Cd(2) I(5) 113.65(3) ? ? ? yes I(4) Cd(2) I(6) 108.25(3) ? ? ? yes I(5) Cd(2) I(6) 121.45(4) ? ? ? yes C(1) S(1) C(2) 103.7(6) ? ? ? yes C(1) S(1) C(3) 100.7(6) ? ? ? yes C(2) S(1) C(3) 100.9(5) ? ? ? yes C(4) S(2) C(5) 102.0(5) ? ? ? yes C(4) S(2) C(6) 102.3(5) ? ? ? yes C(5) S(2) C(6) 100.5(5) ? ? ? yes S(1) C(1) C(2) 37.9(4) ? ? ? yes S(1) C(1) C(3) 39.5(4) ? ? ? yes C(2) C(1) C(3) 59.1(4) ? ? ? yes S(1) C(2) C(1) 38.4(4) ? ? ? yes S(1) C(2) C(3) 39.7(4) ? ? ? yes C(1) C(2) C(3) 59.5(4) ? ? ? yes S(1) C(3) C(1) 39.8(4) ? ? ? yes S(1) C(3) C(2) 39.4(3) ? ? ? yes C(1) C(3) C(2) 61.4(4) ? ? ? yes S(2) C(4) C(5) 39.2(3) ? ? ? yes S(2) C(4) C(6) 38.8(3) ? ? ? yes C(5) C(4) C(6) 59.4(4) ? ? ? yes S(2) C(5) C(4) 38.8(3) ? ? ? yes S(2) C(5) C(6) 39.5(3) ? ? ? yes C(4) C(5) C(6) 60.2(4) ? ? ? yes S(2) C(6) C(4) 38.8(3) ? ? ? yes S(2) C(6) C(5) 39.9(3) ? ? ? yes C(4) C(6) C(5) 60.4(4) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _public_contact_author ; Lars Bengtsson-Kloo Chemical Center University of Lund P.O. 124 S - 22100 Lund Sweden ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' + 46-46-108157 ' _publ_contact_author_fax ' + 46-46-104439 ' _publ_contact_author_email ' Lars.kloo inorg.lu.se ' loop_ _publ_author_name _publ_author_address 'Per H. Svensson' ; Inorganic Chemistry 1 Center for Chemistry and Chemical Engineering Lund University P.O. Box 124 S-221 00 Lund, Sweden ; 'Lars Bengtsson-Kloo' ; Inorganic Chemistry 1 Center for Chemistry and Chemical Engineering Lund University P.O. Box 124 S-221 00 Lund, Sweden ; 'Per Persson' ; Inorganic Chemistry Umea University S-901 87 Umea, Sweden ; _publ_section_title ; Metal Iodides in Polyiodide Networks - The Structural Chemistry of CdI2 with Excess of Iodine. ;