#------------------------------------------------------------------------------ #$Date: 2012-03-26 00:38:57 +0200 (Mon, 26 Mar 2012) $ #$Revision: 47574 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/14/4001492.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4001492 loop_ _publ_author_name 'Wang, Lei' 'Hung, Yi-Chung' 'Hwu, Shiou-Jyh' 'Koo, Hyun-Joo' 'Whangbo, M.-H.' _publ_section_title ; Synthesis, Structure, and Properties of a New Family of Mixed-Framework Chalcohalide Semiconductors:  CdSbS2X (X = Cl, Br), CdBiS2X (X = Cl, Br), and CdBiSe2X (X = Br, I) ; _journal_issue 5 _journal_name_full 'Chemistry of Materials' _journal_page_first 1219 _journal_volume 18 _journal_year 2006 _chemical_formula_moiety 'Br Cd S2 Sb' _chemical_formula_sum 'Br Cd S2 Sb' _chemical_formula_weight 378.18 _chemical_name_systematic ; ? ; _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 91.11(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 12.938(3) _cell_length_b 3.9310(8) _cell_length_c 9.6610(19) _cell_measurement_reflns_used 1664 _cell_measurement_temperature 293.15 _cell_measurement_theta_max 26.0212 _cell_measurement_theta_min 3.1484 _cell_volume 491.26(18) _computing_cell_refinement 'CrystalClear (Rigaku/MSC, 1999)' _computing_data_collection 'CrystalClear (Rigaku/MSC, 1999)' _computing_data_reduction 'CrystalClear (Rigaku/MSC, 1999)' _computing_molecular_graphics 'SHELXTL (Bruker-AXS, 1999)' _computing_publication_material 'SHELXTL (Bruker-AXS, 1999)' _computing_structure_refinement 'SHELXTL (Bruker-AXS, 1999)' _computing_structure_solution 'SHELXTL (Bruker-AXS, 1999)' _diffrn_ambient_temperature 293.15 _diffrn_detector_area_resol_mean 14.6199 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; scan: Number of images: 360 Slice: -90.0000 - 90.0000 Image width: 0.5000 Exp time: 10.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 28.0022 2theta: -0.0875 scan: Number of images: 120 Slice: -30.0000 - 30.0000 Image width: 0.5000 Exp time: 10.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 28.0022 2theta: -0.0875 ; _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_measurement_device_details ; AFC8: Eulerian 3-circle ; _diffrn_measurement_device_type 'Rigaku AFC8S' _diffrn_measurement_method '\w scans' _diffrn_radiation_detector CCD _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2284 _diffrn_reflns_theta_full 26.02 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_min 3.15 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 18.617 _exptl_absorpt_correction_T_max 0.6635 _exptl_absorpt_correction_T_min 0.0681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB, CrystalClear' _exptl_crystal_colour 'Dark red' _exptl_crystal_density_diffrn 5.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Needle _exptl_crystal_F_000 664 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.792 _refine_diff_density_min -1.152 _refine_diff_density_rms 0.267 _refine_ls_extinction_coef 0.0101(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 555 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.153 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0254 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.3013P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.0551 _reflns_number_gt 520 _reflns_number_total 555 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cm0522230si20051006_033637.cif _[local]_cod_data_source_block CdSbS2Br_LW2-83-3a-new _[local]_cod_cif_authors_sg_H-M 'C 2/m' _cod_original_cell_volume 491.24(17) _cod_database_code 4001492 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Sb Sb 0.28673(4) 1.0000 0.68815(4) 0.0183(2) Uani 1 2 d S Cd1 Cd 0.5000 0.5000 1.0000 0.0191(2) Uani 1 4 d S Cd2 Cd 0.5000 0.5000 0.5000 0.0214(2) Uani 1 4 d S Br Br 0.36487(6) 0.0000 1.07589(7) 0.0209(2) Uani 1 2 d S S1 S 0.35424(14) 1.0000 0.45029(16) 0.0129(4) Uani 1 2 d S S2 S 0.41539(14) 0.5000 0.74123(17) 0.0144(4) Uani 1 2 d S loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb 0.0192(3) 0.0190(3) 0.0169(3) 0.000 0.00592(19) 0.000 Cd1 0.0221(4) 0.0141(4) 0.0213(4) 0.000 -0.0001(3) 0.000 Cd2 0.0186(4) 0.0182(4) 0.0278(4) 0.000 0.0095(3) 0.000 Br 0.0201(4) 0.0156(4) 0.0274(4) 0.000 0.0075(3) 0.000 S1 0.0129(8) 0.0126(8) 0.0134(7) 0.000 0.0010(6) 0.000 S2 0.0152(8) 0.0133(8) 0.0146(7) 0.000 -0.0020(6) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_3 S1 Sb S2 86.99(5) . 1_565 S1 Sb S2 86.99(5) . . S2 Sb S2 97.22(6) 1_565 . S2 Cd1 S2 180.0 5_667 . S2 Cd1 Br 89.91(3) 5_667 5_667 S2 Cd1 Br 90.09(3) . 5_667 S2 Cd1 Br 90.09(3) 5_667 . S2 Cd1 Br 89.91(3) . . Br Cd1 Br 180.0 5_667 . S2 Cd1 Br 89.91(3) 5_667 5_657 S2 Cd1 Br 90.09(3) . 5_657 Br Cd1 Br 91.68(3) 5_667 5_657 Br Cd1 Br 88.32(3) . 5_657 S2 Cd1 Br 90.09(3) 5_667 1_565 S2 Cd1 Br 89.91(3) . 1_565 Br Cd1 Br 88.32(3) 5_667 1_565 Br Cd1 Br 91.68(3) . 1_565 Br Cd1 Br 180.00(3) 5_657 1_565 S2 Cd2 S2 180.000(1) 5_666 . S2 Cd2 S1 81.81(5) 5_666 5_676 S2 Cd2 S1 98.19(5) . 5_676 S2 Cd2 S1 98.19(5) 5_666 1_545 S2 Cd2 S1 81.81(5) . 1_545 S1 Cd2 S1 180.0 5_676 1_545 S2 Cd2 S1 81.81(5) 5_666 5_666 S2 Cd2 S1 98.19(5) . 5_666 S1 Cd2 S1 90.84(6) 5_676 5_666 S1 Cd2 S1 89.16(6) 1_545 5_666 S2 Cd2 S1 98.19(5) 5_666 . S2 Cd2 S1 81.81(5) . . S1 Cd2 S1 89.16(6) 5_676 . S1 Cd2 S1 90.84(6) 1_545 . S1 Cd2 S1 180.0 5_666 . Cd1 Br Cd1 91.68(3) 1_545 . Sb S1 Cd2 95.20(5) . 1_565 Sb S1 Cd2 95.20(5) . . Cd2 S1 Cd2 90.84(6) 1_565 . Cd2 S2 Sb 95.84(5) . 1_545 Cd2 S2 Sb 95.84(5) . . Sb S2 Sb 97.22(6) 1_545 . Cd2 S2 Cd1 131.22(7) . . Sb S2 Cd1 115.11(5) 1_545 . Sb S2 Cd1 115.11(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sb S1 2.4741(17) . Sb S2 2.6199(13) 1_565 Sb S2 2.6199(13) . Cd1 S2 2.7096(18) 5_667 Cd1 S2 2.7096(18) . Cd1 Br 2.7398(7) 5_667 Cd1 Br 2.7398(7) . Cd1 Br 2.7398(7) 5_657 Cd1 Br 2.7398(7) 1_565 Cd2 S2 2.5939(17) 5_666 Cd2 S2 2.5939(17) . Cd2 S1 2.7596(13) 5_676 Cd2 S1 2.7596(13) 1_545 Cd2 S1 2.7596(13) 5_666 Cd2 S1 2.7596(13) . Br Cd1 2.7398(7) 1_545 S1 Cd2 2.7596(13) 1_565 S2 Sb 2.6199(13) 1_545