#------------------------------------------------------------------------------ #$Date: 2021-10-07 02:10:18 +0300 (Thu, 07 Oct 2021) $ #$Revision: 269805 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708517.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_7708517 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 I O7 S' _chemical_formula_weight 479.94 _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 ; 2021-07-25 deposited with the CCDC. 2021-10-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 105.168(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.4355(2) _cell_length_b 6.9168(2) _cell_length_c 8.3374(2) _cell_measurement_reflns_used 6149 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 33.1390 _cell_measurement_theta_min 2.9180 _cell_volume 525.17(2) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_unetI/netI 0.0185 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 5685 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.101 _diffrn_reflns_theta_min 3.699 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 39.827 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.27195 _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 'clear light colourless' _exptl_crystal_density_diffrn 6.070 _exptl_crystal_description block _exptl_crystal_F_000 832 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.364 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.252 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 91 _refine_ls_number_reflns 1159 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.115 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0215 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+4.6072P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.0493 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1132 _reflns_number_total 1159 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02514g2.cif _cod_data_source_block 2 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7708517 _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 9.4355 6.9168 8.3374 90.000 105.168 90.000 ZERR 4.00 0.0002 0.0002 0.0002 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC O S I BI UNIT 28 4 4 4 L.S. 4 BOND FMAP 2 PLAN 20 ACTA TEMP 20 OMIT 1 0 0 OMIT 0 0 6 WGHT 0.023100 4.607200 FVAR 0.15066 BI1 4 0.699180 0.140496 0.979867 11.00000 0.01641 0.01253 = 0.01598 0.00025 0.00288 0.00305 I1 3 1.030547 0.210327 1.369513 11.00000 0.00857 0.00909 = 0.00795 -0.00023 0.00234 -0.00060 S1 2 0.394503 0.168738 0.690066 11.00000 0.00817 0.00806 = 0.00624 0.00158 -0.00027 -0.00074 O1 1 0.837447 0.278361 1.281323 11.00000 0.00380 0.01640 = 0.01971 -0.00477 0.00272 0.00075 O2 1 1.101942 0.455448 1.392282 11.00000 0.01049 0.00946 = 0.01358 0.00038 -0.00198 -0.00590 O3 1 1.006151 0.174892 1.575458 11.00000 0.03932 0.01796 = 0.01316 -0.00380 0.01665 -0.00490 O4 1 0.410437 0.099161 0.863707 11.00000 0.01827 0.01415 = 0.00814 0.00181 0.00305 0.00008 O5 1 0.547130 0.198335 0.680668 11.00000 0.00948 0.01609 = 0.01920 0.00655 0.00596 0.00276 O6 1 0.314748 0.354531 0.673471 11.00000 0.01360 0.01152 = 0.01606 0.00364 0.00170 0.00417 O7 1 0.313090 0.031069 0.566024 11.00000 0.02024 0.01642 = 0.01355 -0.00432 -0.00021 -0.00961 HKLF 4 REM 2 in P2(1)/c REM R1 = 0.0215 for 1132 Fo > 4sig(Fo) and 0.0223 for all 1159 data REM 91 parameters refined using 0 restraints END WGHT 0.0231 4.6076 REM Highest difference peak 1.364, deepest hole -1.234, 1-sigma level 0.252 Q1 1 0.7871 0.1538 0.9863 11.00000 0.05 1.36 Q2 1 0.7267 0.1359 1.0718 11.00000 0.05 0.98 Q3 1 1.1148 0.3877 1.6017 11.00000 0.05 0.89 Q4 1 0.4322 0.1910 0.9138 11.00000 0.05 0.84 Q5 1 0.6169 0.1777 0.9816 11.00000 0.05 0.83 Q6 1 0.1670 0.3091 0.5498 11.00000 0.05 0.82 Q7 1 0.7283 0.0188 0.9740 11.00000 0.05 0.81 Q8 1 0.4553 0.0566 0.4391 11.00000 0.05 0.79 Q9 1 1.1230 0.3156 1.3965 11.00000 0.05 0.79 Q10 1 0.9252 0.2370 1.3554 11.00000 0.05 0.76 Q11 1 0.2855 0.3715 0.5801 11.00000 0.05 0.75 Q12 1 0.9540 0.1244 1.3605 11.00000 0.05 0.73 Q13 1 0.3757 0.2748 0.6807 11.00000 0.05 0.70 Q14 1 0.8799 0.2167 1.2350 11.00000 0.05 0.69 Q15 1 1.1797 0.1618 1.6753 11.00000 0.05 0.68 Q16 1 1.0164 0.3471 1.3838 11.00000 0.05 0.68 Q17 1 0.7821 0.2112 1.2990 11.00000 0.05 0.65 Q18 1 0.4445 0.0039 0.5610 11.00000 0.05 0.63 Q19 1 1.0067 0.2019 1.2586 11.00000 0.05 0.63 Q20 1 1.1871 0.3986 1.4722 11.00000 0.05 0.63 ; _shelx_res_checksum 74415 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 Bi1 Bi 0.69918(3) 0.14050(4) 0.97987(3) 0.01523(9) Uani 1 1 d . . . . . I1 I 1.03055(4) 0.21033(6) 1.36951(5) 0.00850(11) Uani 1 1 d . . . . . S1 S 0.39450(16) 0.1687(2) 0.69007(18) 0.0079(3) Uani 1 1 d . . . . . O1 O 0.8374(5) 0.2784(7) 1.2813(6) 0.0134(10) Uani 1 1 d . . . . . O2 O 1.1019(5) 0.4554(6) 1.3923(6) 0.0121(9) Uani 1 1 d . . . . . O3 O 1.0062(6) 0.1749(8) 1.5755(6) 0.0216(11) Uani 1 1 d . . . . . O4 O 0.4104(5) 0.0992(7) 0.8637(6) 0.0136(9) Uani 1 1 d . . . . . O5 O 0.5471(5) 0.1983(7) 0.6807(6) 0.0145(10) Uani 1 1 d . . . . . O6 O 0.3147(5) 0.3545(6) 0.6735(6) 0.0141(10) Uani 1 1 d . . . . . O7 O 0.3131(5) 0.0311(7) 0.5660(6) 0.0176(10) 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 Bi1 0.01641(14) 0.01253(15) 0.01598(15) 0.00025(10) 0.00288(10) 0.00305(9) I1 0.00857(19) 0.0091(2) 0.00795(19) -0.00023(14) 0.00234(14) -0.00060(13) S1 0.0082(7) 0.0081(7) 0.0062(7) 0.0016(5) -0.0003(5) -0.0007(5) O1 0.004(2) 0.016(2) 0.020(2) -0.0048(19) 0.0027(18) 0.0008(17) O2 0.010(2) 0.009(2) 0.014(2) 0.0004(18) -0.0020(18) -0.0059(16) O3 0.039(3) 0.018(3) 0.013(3) -0.004(2) 0.017(2) -0.005(2) O4 0.018(2) 0.014(2) 0.008(2) 0.0018(18) 0.0031(18) 0.0001(18) O5 0.009(2) 0.016(2) 0.019(3) 0.007(2) 0.0060(19) 0.0028(18) O6 0.014(2) 0.012(2) 0.016(2) 0.0036(18) 0.0017(19) 0.0042(17) O7 0.020(2) 0.016(3) 0.014(2) -0.004(2) -0.0002(19) -0.0096(19) 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' 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 O2 Bi1 O6 72.79(16) 2_747 2_646 ? O2 Bi1 O1 85.73(16) 2_747 4_565 ? O6 Bi1 O1 77.65(16) 2_646 4_565 ? O2 Bi1 O4 77.68(16) 2_747 3_657 ? O6 Bi1 O4 75.66(16) 2_646 3_657 ? O1 Bi1 O4 151.74(16) 4_565 3_657 ? O2 Bi1 O5 136.21(16) 2_747 . ? O6 Bi1 O5 70.31(16) 2_646 . ? O1 Bi1 O5 64.14(14) 4_565 . ? O4 Bi1 O5 114.17(15) 3_657 . ? O2 Bi1 O4 138.27(16) 2_747 . ? O6 Bi1 O4 78.71(15) 2_646 . ? O1 Bi1 O4 117.34(14) 4_565 . ? O4 Bi1 O4 66.00(17) 3_657 . ? O5 Bi1 O4 53.32(14) . . ? O2 Bi1 O1 67.96(15) 2_747 . ? O6 Bi1 O1 139.07(15) 2_646 . ? O1 Bi1 O1 109.88(14) 4_565 . ? O4 Bi1 O1 85.01(15) 3_657 . ? O5 Bi1 O1 150.07(15) . . ? O4 Bi1 O1 125.45(13) . . ? O2 Bi1 O5 116.32(16) 2_747 4_566 ? O6 Bi1 O5 136.16(15) 2_646 4_566 ? O1 Bi1 O5 142.32(16) 4_565 4_566 ? O4 Bi1 O5 65.92(15) 3_657 4_566 ? O5 Bi1 O5 106.54(14) . 4_566 ? O4 Bi1 O5 67.16(14) . 4_566 ? O1 Bi1 O5 58.83(13) . 4_566 ? O2 Bi1 O7 128.19(15) 2_747 2_656 ? O6 Bi1 O7 140.04(16) 2_646 2_656 ? O1 Bi1 O7 71.68(15) 4_565 2_656 ? O4 Bi1 O7 136.34(15) 3_657 2_656 ? O5 Bi1 O7 73.52(15) . 2_656 ? O4 Bi1 O7 93.07(14) . 2_656 ? O1 Bi1 O7 76.82(15) . 2_656 ? O5 Bi1 O7 70.71(15) 4_566 2_656 ? O3 I1 O2 99.4(2) . . ? O3 I1 O1 93.2(2) . . ? O2 I1 O1 96.0(2) . . ? O7 S1 O5 113.0(3) . . ? O7 S1 O6 109.8(3) . . ? O5 S1 O6 110.8(3) . . ? O7 S1 O4 112.0(3) . . ? O5 S1 O4 104.1(3) . . ? O6 S1 O4 106.9(3) . . ? I1 O1 Bi1 116.1(2) . 4_566 ? I1 O1 Bi1 118.1(2) . . ? Bi1 O1 Bi1 120.29(17) 4_566 . ? I1 O2 Bi1 143.8(2) . 2_757 ? S1 O4 Bi1 140.3(3) . 3_657 ? S1 O4 Bi1 98.7(2) . . ? Bi1 O4 Bi1 114.00(17) 3_657 . ? S1 O5 Bi1 103.4(2) . . ? S1 O5 Bi1 140.4(3) . 4_565 ? Bi1 O5 Bi1 114.40(17) . 4_565 ? S1 O6 Bi1 137.8(3) . 2_656 ? S1 O7 Bi1 137.5(3) . 2_646 ? 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 Bi1 O2 2.291(4) 2_747 ? Bi1 O6 2.340(5) 2_646 ? Bi1 O1 2.426(5) 4_565 ? Bi1 O4 2.495(5) 3_657 ? Bi1 O5 2.563(5) . ? Bi1 O4 2.657(5) . ? Bi1 O1 2.686(5) . ? Bi1 O5 2.713(5) 4_566 ? Bi1 O7 2.727(5) 2_656 ? I1 O3 1.808(5) . ? I1 O2 1.816(4) . ? I1 O1 1.839(4) . ? S1 O7 1.467(5) . ? S1 O5 1.477(5) . ? S1 O6 1.477(5) . ? S1 O4 1.495(5) . ? O1 Bi1 2.426(4) 4_566 ? O2 Bi1 2.291(4) 2_757 ? O4 Bi1 2.495(5) 3_657 ? O5 Bi1 2.713(5) 4_565 ? O6 Bi1 2.340(5) 2_656 ? O7 Bi1 2.727(5) 2_646 ?