#------------------------------------------------------------------------------ #$Date: 2021-10-07 02:10:18 +0300 (Thu, 07 Oct 2021) $ #$Revision: 269805 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708518.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_7708518 loop_ _publ_author_name 'Li, Yi-Lin' 'Hu, Chun-Li' 'Chen, Jin' 'Mao, Jiang-Gao' _publ_section_title ; Two Bismuth Iodate Sulfates with Enhanced Optical Anisotropy ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02514G _journal_year 2021 _chemical_formula_sum 'Bi Cd I O11 S2' _chemical_formula_weight 688.40 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-07-26 deposited with the CCDC. 2021-10-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.226(15) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.777(2) _cell_length_b 6.8491(9) _cell_length_c 9.9835(14) _cell_measurement_reflns_used 2425 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30.0760 _cell_measurement_theta_min 3.6020 _cell_volume 850.5(2) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.3468 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 6764 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.361 _diffrn_reflns_theta_min 3.276 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 27.341 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.42373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 5.376 _exptl_crystal_description Plate _exptl_crystal_F_000 1216 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.426 _refine_diff_density_min -1.794 _refine_diff_density_rms 0.320 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 1736 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0299 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0119P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.0534 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1499 _reflns_number_total 1736 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02514g2.cif _cod_data_source_block 2_CCDC1 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7708518 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; 2.res created by SHELXL-2014/7 TITL 2 in P2(1)/c CELL 0.71073 12.7767 6.8491 9.9835 90.000 103.226 90.000 ZERR 4.00 0.0020 0.0009 0.0014 0.000 0.015 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC O S CD I BI UNIT 44 8 4 4 4 L.S. 4 BOND FMAP 2 PLAN 20 ACTA ISOR 0.003 0.006 O3 OMIT -3 0 2 OMIT 2 0 2 OMIT -8 5 4 WGHT 0.011900 FVAR 0.11217 CD1 3 0.938447 0.791520 0.390066 11.00000 0.00985 0.01340 = 0.01145 -0.00189 0.00245 -0.00093 BI1 5 0.688231 0.233632 0.501792 11.00000 0.00941 0.01481 = 0.01325 -0.00092 0.00252 -0.00114 I1 4 0.474508 0.163694 0.221074 11.00000 0.00834 0.00839 = 0.00977 0.00080 0.00304 0.00135 S1 2 0.884808 0.286868 0.315305 11.00000 0.00715 0.01099 = 0.01012 0.00083 0.00244 0.00233 S2 2 0.753673 0.733785 0.073418 11.00000 0.00746 0.01233 = 0.00850 0.00064 0.00190 0.00059 O1 1 0.572007 0.038747 0.361283 11.00000 0.00585 0.01510 = 0.01360 0.00063 -0.00327 -0.00148 O2 1 0.547676 0.180688 0.090708 11.00000 0.02918 0.01573 = 0.00755 0.00181 0.00928 -0.00396 O3 1 0.432834 -0.109869 0.173196 11.00000 0.00901 0.00630 = 0.01237 -0.00292 -0.00121 -0.00179 O4 1 0.955084 0.134510 0.395659 11.00000 0.01361 0.00878 = 0.01457 0.00116 0.00034 0.00191 O5 1 0.770734 0.234046 0.301967 11.00000 0.01277 0.02280 = 0.01766 0.00594 0.00218 0.00188 O6 1 0.902047 0.296717 0.174597 11.00000 0.00913 0.03173 = 0.01099 0.00319 0.00407 -0.00019 O7 1 0.908222 0.470532 0.389225 11.00000 0.03677 0.00762 = 0.02758 -0.00281 -0.00640 0.00099 O8 1 0.842381 0.817230 0.175762 11.00000 0.02092 0.01960 = 0.01966 -0.00279 -0.00054 -0.00377 O9 1 0.794598 0.621920 -0.029481 11.00000 0.01875 0.01744 = 0.01753 -0.00667 0.01222 -0.00672 O10 1 0.687626 0.595313 0.132118 11.00000 0.01784 0.02548 = 0.02005 0.00230 0.01591 0.00035 O11 1 0.685491 0.893594 0.003654 11.00000 0.02708 0.00848 = 0.02530 0.00539 -0.00274 0.00846 HKLF 4 REM 2 in P2(1)/c REM R1 = 0.0299 for 1499 Fo > 4sig(Fo) and 0.0380 for all 1736 data REM 145 parameters refined using 6 restraints END WGHT 0.0119 0.0000 REM Highest difference peak 1.426, deepest hole -1.794, 1-sigma level 0.320 Q1 1 0.7645 0.2462 0.5129 11.00000 0.05 1.43 Q2 1 0.4746 0.3053 0.2128 11.00000 0.05 1.39 Q3 1 0.8408 0.2718 0.0033 11.00000 0.05 1.17 Q4 1 0.9639 -0.0007 0.2805 11.00000 0.05 1.14 Q5 1 0.6772 1.0513 0.0949 11.00000 0.05 1.06 Q6 1 0.7811 0.1950 0.3807 11.00000 0.05 1.05 Q7 1 0.6861 0.2653 0.1966 11.00000 0.05 0.99 Q8 1 0.6780 0.3529 0.5226 11.00000 0.05 0.98 Q9 1 0.5000 0.0000 0.5000 10.50000 0.05 0.97 Q10 1 0.4134 -0.0346 0.2237 11.00000 0.05 0.96 Q11 1 0.7125 1.0564 -0.0993 11.00000 0.05 0.96 Q12 1 0.7031 0.2297 0.3910 11.00000 0.05 0.92 Q13 1 0.5998 0.6924 0.1405 11.00000 0.05 0.89 Q14 1 0.9291 0.2066 0.3775 11.00000 0.05 0.89 Q15 1 0.4826 0.1878 0.0175 11.00000 0.05 0.89 Q16 1 0.6853 0.1169 0.4551 11.00000 0.05 0.87 Q17 1 0.5442 0.1758 0.4062 11.00000 0.05 0.87 Q18 1 0.9327 0.8979 0.4071 11.00000 0.05 0.86 Q19 1 0.7125 0.2882 0.5999 11.00000 0.05 0.85 Q20 1 0.6664 0.8872 -0.0846 11.00000 0.05 0.84 ; _shelx_res_checksum 23204 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.93845(5) 0.79152(8) 0.39007(6) 0.01157(16) Uani 1 1 d . . . . . Bi1 Bi 0.68823(3) 0.23363(4) 0.50179(3) 0.01250(11) Uani 1 1 d . . . . . I1 I 0.47451(5) 0.16369(7) 0.22107(5) 0.00868(14) Uani 1 1 d . . . . . S1 S 0.88481(18) 0.2869(3) 0.31530(19) 0.0093(4) Uani 1 1 d . . . . . S2 S 0.75367(18) 0.7338(3) 0.07342(19) 0.0094(4) Uani 1 1 d . . . . . O1 O 0.5720(5) 0.0387(7) 0.3613(5) 0.0124(13) Uani 1 1 d . . . . . O2 O 0.5477(5) 0.1807(8) 0.0907(5) 0.0167(14) Uani 1 1 d . . . . . O3 O 0.4328(5) -0.1099(7) 0.1732(5) 0.0098(12) Uani 1 1 d . U . . . O4 O 0.9551(5) 0.1345(7) 0.3957(5) 0.0128(13) Uani 1 1 d . . . . . O5 O 0.7707(5) 0.2340(8) 0.3020(6) 0.0180(14) Uani 1 1 d . . . . . O6 O 0.9020(5) 0.2967(8) 0.1746(5) 0.0170(14) Uani 1 1 d . . . . . O7 O 0.9082(6) 0.4705(8) 0.3892(6) 0.0262(17) Uani 1 1 d . . . . . O8 O 0.8424(5) 0.8172(8) 0.1758(6) 0.0209(15) Uani 1 1 d . . . . . O9 O 0.7946(5) 0.6219(8) -0.0295(5) 0.0166(14) Uani 1 1 d . . . . . O10 O 0.6876(5) 0.5953(8) 0.1321(5) 0.0193(14) Uani 1 1 d . . . . . O11 O 0.6855(5) 0.8936(8) 0.0037(6) 0.0217(16) Uani 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0099(4) 0.0134(3) 0.0115(3) -0.0019(2) 0.0025(3) -0.0009(3) Bi1 0.0094(2) 0.01481(18) 0.01325(17) -0.00092(12) 0.00252(14) -0.00114(13) I1 0.0083(3) 0.0084(3) 0.0098(3) 0.00080(19) 0.0030(2) 0.0014(2) S1 0.0072(13) 0.0110(9) 0.0101(10) 0.0008(8) 0.0024(9) 0.0023(8) S2 0.0075(13) 0.0123(10) 0.0085(9) 0.0006(7) 0.0019(9) 0.0006(8) O1 0.006(3) 0.015(3) 0.014(3) 0.001(2) -0.003(3) -0.001(2) O2 0.029(4) 0.016(3) 0.008(3) 0.002(2) 0.009(3) -0.004(3) O3 0.009(2) 0.006(2) 0.012(2) -0.0029(18) -0.0012(19) -0.0018(19) O4 0.014(4) 0.009(3) 0.015(3) 0.001(2) 0.000(3) 0.002(2) O5 0.013(4) 0.023(3) 0.018(3) 0.006(2) 0.002(3) 0.002(3) O6 0.009(4) 0.032(3) 0.011(3) 0.003(2) 0.004(3) 0.000(3) O7 0.037(5) 0.008(3) 0.028(3) -0.003(2) -0.006(3) 0.001(3) O8 0.021(4) 0.020(3) 0.020(3) -0.003(2) -0.001(3) -0.004(3) O9 0.019(4) 0.017(3) 0.018(3) -0.007(2) 0.012(3) -0.007(3) O10 0.018(4) 0.025(3) 0.020(3) 0.002(3) 0.016(3) 0.000(3) O11 0.027(5) 0.008(3) 0.025(3) 0.005(2) -0.003(3) 0.008(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 '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 _geom_angle_publ_flag O8 Cd1 O7 91.0(2) . . ? O8 Cd1 O9 90.4(2) . 4_576 ? O7 Cd1 O9 96.1(2) . 4_576 ? O8 Cd1 O6 93.4(2) . 2_755 ? O7 Cd1 O6 100.4(2) . 2_755 ? O9 Cd1 O6 163.0(2) 4_576 2_755 ? O8 Cd1 O4 162.51(19) . 3_766 ? O7 Cd1 O4 106.49(19) . 3_766 ? O9 Cd1 O4 88.1(2) 4_576 3_766 ? O6 Cd1 O4 83.3(2) 2_755 3_766 ? O8 Cd1 O4 88.32(19) . 1_565 ? O7 Cd1 O4 174.8(2) . 1_565 ? O9 Cd1 O4 78.8(2) 4_576 1_565 ? O6 Cd1 O4 84.8(2) 2_755 1_565 ? O4 Cd1 O4 74.29(19) 3_766 1_565 ? O1 Bi1 O2 85.9(2) . 4_566 ? O1 Bi1 O3 64.52(18) . 2_655 ? O2 Bi1 O3 73.8(2) 4_566 2_655 ? O1 Bi1 O5 80.7(2) . . ? O2 Bi1 O5 147.81(19) 4_566 . ? O3 Bi1 O5 74.0(2) 2_655 . ? O1 Bi1 O11 126.38(18) . 4_576 ? O2 Bi1 O11 73.9(2) 4_566 4_576 ? O3 Bi1 O11 62.26(17) 2_655 4_576 ? O5 Bi1 O11 90.80(18) . 4_576 ? O1 Bi1 O10 73.71(18) . 4_566 ? O2 Bi1 O10 86.26(19) 4_566 4_566 ? O3 Bi1 O10 134.45(19) 2_655 4_566 ? O5 Bi1 O10 117.21(18) . 4_566 ? O11 Bi1 O10 149.35(17) 4_576 4_566 ? O2 I1 O1 102.0(3) . . ? O2 I1 O3 92.5(2) . . ? O1 I1 O3 80.9(2) . . ? O2 I1 O3 89.4(2) . 2_655 ? O1 I1 O3 75.9(2) . 2_655 ? O3 I1 O3 156.60(14) . 2_655 ? O7 S1 O6 112.7(4) . . ? O7 S1 O5 110.0(4) . . ? O6 S1 O5 106.6(3) . . ? O7 S1 O4 107.7(3) . . ? O6 S1 O4 110.1(3) . . ? O5 S1 O4 109.8(3) . . ? O8 S2 O9 110.5(4) . . ? O8 S2 O11 108.7(3) . . ? O9 S2 O11 108.9(3) . . ? O8 S2 O10 113.4(3) . . ? O9 S2 O10 105.6(3) . . ? O11 S2 O10 109.6(4) . . ? I1 O1 Bi1 115.6(2) . . ? I1 O2 Bi1 155.2(3) . 4_565 ? I1 O3 I1 119.5(3) . 2_645 ? I1 O3 Bi1 135.9(2) . 2_645 ? I1 O3 Bi1 103.98(19) 2_645 2_645 ? S1 O4 Cd1 120.0(3) . 3_766 ? S1 O4 Cd1 130.3(3) . 1_545 ? Cd1 O4 Cd1 105.71(19) 3_766 1_545 ? S1 O5 Bi1 121.6(3) . . ? S1 O6 Cd1 127.5(4) . 2_745 ? S1 O7 Cd1 150.4(4) . . ? S2 O8 Cd1 144.6(4) . . ? S2 O9 Cd1 124.3(3) . 4_575 ? S2 O10 Bi1 106.9(3) . 4_565 ? S2 O11 Bi1 137.7(4) . 4_575 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O8 2.217(6) . ? Cd1 O7 2.232(5) . ? Cd1 O9 2.247(6) 4_576 ? Cd1 O6 2.275(6) 2_755 ? Cd1 O4 2.313(5) 3_766 ? Cd1 O4 2.358(5) 1_565 ? Bi1 O1 2.236(5) . ? Bi1 O2 2.255(6) 4_566 ? Bi1 O3 2.314(5) 2_655 ? Bi1 O5 2.460(6) . ? Bi1 O11 2.554(5) 4_576 ? Bi1 O10 2.603(6) 4_566 ? I1 O2 1.771(6) . ? I1 O1 1.856(5) . ? I1 O3 1.976(5) . ? I1 O3 2.085(5) 2_655 ? S1 O7 1.454(6) . ? S1 O6 1.472(6) . ? S1 O5 1.478(7) . ? S1 O4 1.486(5) . ? S2 O8 1.458(6) . ? S2 O9 1.470(6) . ? S2 O11 1.471(6) . ? S2 O10 1.477(6) . ? O2 Bi1 2.255(6) 4_565 ? O3 I1 2.085(5) 2_645 ? O3 Bi1 2.315(5) 2_645 ? O4 Cd1 2.313(5) 3_766 ? O4 Cd1 2.358(5) 1_545 ? O6 Cd1 2.275(6) 2_745 ? O9 Cd1 2.247(6) 4_575 ? O10 Bi1 2.603(6) 4_565 ? O11 Bi1 2.554(5) 4_575 ?