#------------------------------------------------------------------------------ #$Date: 2012-03-26 00:38:57 +0200 (Mon, 26 Mar 2012) $ #$Revision: 47574 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/14/4001491.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_4001491 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 'Cd Cl S2 Sb' _chemical_formula_sum 'Cd Cl S2 Sb' _chemical_formula_weight 333.72 _chemical_name_systematic ; ? ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.5850(19) _cell_length_b 3.9910(8) _cell_length_c 12.443(3) _cell_measurement_reflns_used 3072 _cell_measurement_temperature 293.15 _cell_measurement_theta_max 26.3714 _cell_measurement_theta_min 2.6799 _cell_volume 475.99(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 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_details ; scan: Number of images: 360 Slice: -90.0000 - 90.0000 Image width: 0.5000 Exp time: 20.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 27.1619 2theta: -0.0840 scan: Number of images: 120 Slice: -30.0000 - 30.0000 Image width: 0.5000 Exp time: 20.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 27.1619 2theta: -0.0840 ; _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 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 4286 _diffrn_reflns_theta_full 26.35 _diffrn_reflns_theta_max 26.35 _diffrn_reflns_theta_min 2.68 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.380 _exptl_absorpt_correction_T_max 0.7718 _exptl_absorpt_correction_T_min 0.1052 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB, CrystalClear' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 4.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Needle _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.677 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.181 _refine_ls_extinction_coef 0.0146(7) _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 1.135 _refine_ls_matrix_type full _refine_ls_number_parameters 32 _refine_ls_number_reflns 546 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.135 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0201 _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^)+(0.0180P)^2^+1.1715P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0431 _reflns_number_gt 508 _reflns_number_total 546 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cm0522230si20051006_033637.cif _[local]_cod_data_source_block CdSbS2CL_LW2-83-1a-new _[local]_cod_cif_authors_sg_H-M Pnma _cod_original_cell_volume 475.99(16) _cod_database_code 4001491 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' 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 0.68609(5) 1.2500 0.46636(3) 0.01836(16) Uani 1 2 d S Cd Cd 1.00108(5) 0.7500 0.27053(4) 0.01892(17) Uani 1 2 d S S2 S 0.74185(16) 0.7500 0.33195(12) 0.0139(3) Uani 1 2 d S S1 S 0.44993(16) 1.2500 0.38898(12) 0.0142(3) Uani 1 2 d S Cl Cl 1.07295(18) 0.2500 0.39474(13) 0.0217(3) 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 0.0156(2) 0.0207(3) 0.0188(2) 0.000 -0.00373(16) 0.000 Cd 0.0180(3) 0.0188(3) 0.0199(3) 0.000 0.00386(19) 0.000 S2 0.0131(7) 0.0143(7) 0.0143(7) 0.000 0.0010(6) 0.000 S1 0.0129(7) 0.0151(7) 0.0146(7) 0.000 -0.0007(6) 0.000 Cl 0.0275(9) 0.0187(7) 0.0190(7) 0.000 -0.0054(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' Cl Cl 0.1484 0.1585 '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 86.49(4) . . S1 Sb S2 86.49(4) . 1_565 S2 Sb S2 97.31(5) . 1_565 S2 Cd Cl 94.47(5) . 1_565 S2 Cd Cl 94.47(5) . . Cl Cd Cl 99.41(6) 1_565 . S2 Cd S2 168.17(3) . 6_656 Cl Cd S2 93.17(5) 1_565 6_656 Cl Cd S2 93.17(5) . 6_656 S2 Cd S1 92.30(4) . 6_646 Cl Cd S1 171.24(5) 1_565 6_646 Cl Cd S1 85.58(4) . 6_646 S2 Cd S1 79.29(4) 6_656 6_646 S2 Cd S1 92.30(4) . 6_656 Cl Cd S1 85.58(4) 1_565 6_656 Cl Cd S1 171.24(5) . 6_656 S2 Cd S1 79.29(4) 6_656 6_656 S1 Cd S1 88.61(5) 6_646 6_656 Cd S2 Cd 133.98(6) . 6_556 Cd S2 Sb 112.16(4) . . Cd S2 Sb 97.37(4) 6_556 . Cd S2 Sb 112.16(4) . 1_545 Cd S2 Sb 97.37(4) 6_556 1_545 Sb S2 Sb 97.31(5) . 1_545 Sb S1 Cd 96.55(4) . 6_556 Sb S1 Cd 96.55(4) . 6_566 Cd S1 Cd 88.61(5) 6_556 6_566 Cd Cl Cd 99.41(6) 1_545 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sb S1 2.4598(16) . Sb S2 2.6580(11) . Sb S2 2.6580(11) 1_565 Cd S2 2.5996(17) . Cd Cl 2.6163(11) 1_565 Cd Cl 2.6163(11) . Cd S2 2.6366(17) 6_656 Cd S1 2.8569(12) 6_646 Cd S1 2.8569(12) 6_656 S2 Cd 2.6366(17) 6_556 S2 Sb 2.6580(11) 1_545 S1 Cd 2.8569(12) 6_556 S1 Cd 2.8569(12) 6_566 Cl Cd 2.6163(11) 1_545