#------------------------------------------------------------------------------ #$Date: 2020-08-11 05:15:58 +0300 (Tue, 11 Aug 2020) $ #$Revision: 255230 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/50/7705079.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_7705079 loop_ _publ_author_name 'Li, Yanhua' 'Song, Xuedan' 'Liu, Yan' 'Guo, Yongkang' 'Sun, Yu' 'Ji, Min' 'Zhong-Lu, You' 'An, Yonglin' _publ_section_title ; Syntheses, structures, and photocatalytic properties of open-framework Ag-Sn-S compounds ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02513E _journal_year 2020 _chemical_formula_sum 'Ag K S3 Sn' _chemical_formula_weight 361.84 _space_group_crystal_system orthorhombic _space_group_IT_number 43 _space_group_name_Hall 'F 2 -2d' _space_group_name_H-M_alt 'F d d 2' _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2019-11-13 deposited with the CCDC. 2020-08-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 9.9233(7) _cell_length_b 30.274(2) _cell_length_c 8.5537(6) _cell_measurement_reflns_used 4224 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 28.36 _cell_measurement_theta_min 2.69 _cell_volume 2569.7(3) _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_unetI/netI 0.0408 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 4224 _diffrn_reflns_point_group_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.361 _diffrn_reflns_theta_min 2.691 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 8.416 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS-2014/5 _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 3.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2624 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.948 _refine_diff_density_min -2.062 _refine_diff_density_rms 0.299 _refine_ls_abs_structure_details ; Flack x determined using 610 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_extinction_coef 0.00056(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)' _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 57 _refine_ls_number_reflns 1563 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.189 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0449 _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1340 _refine_ls_wR_factor_ref 0.1540 _reflns_Friedel_coverage 0.815 _reflns_Friedel_fraction_full 0.967 _reflns_Friedel_fraction_max 0.930 _reflns_number_gt 1466 _reflns_number_total 1563 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02513e2.cif _cod_data_source_block 1 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 7705079 _shelx_shelxl_version_number 2017/1 _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_estimated_absorpt_t_min 0.4657 _shelx_estimated_absorpt_t_max 0.7457 _shelx_res_file ; TITL 20190919a_0m_a.res in Fdd2 1.res created by SHELXL-2017/1 at 10:03:07 on 19-Sep-2019 REM Old TITL 20190919a_0m in F2dd #43 REM SHELXT solution in Fdd2 REM R1 0.076, Rweak 0.013, Alpha 0.001, Orientation a'=b, b'=c, c'=a REM Flack x = 0.046 ( 0.034 ) from Parsons' quotients REM Formula found by SHELXT: K Ag Sn S3 CELL 0.71073 9.9233 30.2736 8.5537 90 90 90 ZERR 16 0.0007 0.002 0.0006 0 0 0 LATT -4 SYMM -X,-Y,+Z SYMM 0.25+X,0.25-Y,0.25+Z SYMM 0.25-X,0.25+Y,0.25+Z SFAC K Ag Sn S UNIT 16 16 16 48 ACTA L.S. 4 0 0 PLAN 20 TEMP 0 list 4 fmap 2 53 REM REM REM WGHT 0.100000 EXTI 0.000563 FVAR 0.08833 SN1 3 0.451697 0.336415 0.532354 11.00000 0.02013 0.01913 = 0.02393 -0.00055 0.00244 -0.00121 AG1 2 0.250000 0.250000 0.708388 10.50000 0.02632 0.05244 = 0.04727 0.00000 0.00000 -0.01448 AG2 2 0.250000 0.250000 0.339755 10.50000 0.05536 0.02090 = 0.04577 0.00000 0.00000 -0.00734 K1 1 0.225265 0.430275 0.292298 11.00000 0.03948 0.02797 = 0.02801 0.00227 0.00150 -0.00286 S1 4 0.477604 0.275084 0.701423 11.00000 0.02550 0.02292 = 0.02602 0.00266 0.00031 -0.00199 S2 4 0.275281 0.328961 0.352144 11.00000 0.02861 0.02257 = 0.02744 -0.00104 -0.00633 -0.00453 S3 4 0.423910 0.408258 0.658153 11.00000 0.02269 0.02782 = 0.03809 -0.00686 0.00843 -0.00327 HKLF 4 REM 20190919a_0m_a.res in Fdd2 REM R1 = 0.0449 for 1466 Fo > 4sig(Fo) and 0.0483 for all 1563 data REM 57 parameters refined using 1 restraints END WGHT 0.0402 138.5401 REM Highest difference peak 1.948, deepest hole -2.062, 1-sigma level 0.299 Q1 1 0.4054 0.3075 0.4752 11.00000 0.05 1.47 Q2 1 0.5052 0.3072 0.5795 11.00000 0.05 1.32 Q3 1 0.1958 0.4084 0.2756 11.00000 0.05 1.25 Q4 1 0.2479 0.4304 0.3508 11.00000 0.05 1.21 Q5 1 0.4194 0.3404 0.4000 11.00000 0.05 1.17 Q6 1 0.5076 0.3185 0.4638 11.00000 0.05 1.15 Q7 1 0.3014 0.4096 0.2647 11.00000 0.05 1.09 Q8 1 0.1491 0.2501 0.8490 11.00000 0.05 1.09 Q9 1 0.1451 0.4190 0.2063 11.00000 0.05 1.08 Q10 1 0.4061 0.4124 0.7847 11.00000 0.05 1.08 Q11 1 0.3034 0.4108 0.6405 11.00000 0.05 1.06 Q12 1 0.4052 0.3630 0.5969 11.00000 0.05 1.02 Q13 1 0.4246 0.3712 0.5927 11.00000 0.05 1.02 Q14 1 0.4413 0.3736 0.4722 11.00000 0.05 1.01 Q15 1 0.1768 0.2711 0.4086 11.00000 0.05 1.00 Q16 1 0.5074 0.3355 0.6528 11.00000 0.05 0.99 Q17 1 0.4072 0.3639 0.4762 11.00000 0.05 0.93 Q18 1 0.3967 0.3175 0.5921 11.00000 0.05 0.93 Q19 1 0.4022 0.2598 0.2877 11.00000 0.05 0.92 Q20 1 0.3176 0.2719 0.7759 11.00000 0.05 0.91 ; _shelx_res_checksum 5671 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' 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 Sn1 Sn 0.45170(11) 0.33641(3) 0.53235(11) 0.0211(4) Uani 1 1 d . . . . . Ag1 Ag 0.250000 0.250000 0.7084(3) 0.0420(6) Uani 1 2 d S T P . . Ag2 Ag 0.250000 0.250000 0.3398(3) 0.0407(6) Uani 1 2 d S T P . . K1 K 0.2253(4) 0.43027(13) 0.2923(5) 0.0318(9) Uani 1 1 d . . . . . S1 S 0.4776(4) 0.27508(13) 0.7014(5) 0.0248(8) Uani 1 1 d . . . . . S2 S 0.2753(5) 0.32896(13) 0.3521(5) 0.0262(9) Uani 1 1 d . . . . . S3 S 0.4239(5) 0.40826(14) 0.6582(6) 0.0295(9) 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 Sn1 0.0201(5) 0.0191(5) 0.0239(5) -0.0005(4) 0.0024(4) -0.0012(4) Ag1 0.0263(11) 0.0524(14) 0.0473(12) 0.000 0.000 -0.0145(9) Ag2 0.0554(15) 0.0209(9) 0.0458(13) 0.000 0.000 -0.0073(9) K1 0.039(2) 0.0280(16) 0.0280(18) 0.0023(16) 0.0015(18) -0.0029(15) S1 0.0255(18) 0.0229(19) 0.0260(19) 0.0027(15) 0.0003(15) -0.0020(15) S2 0.029(2) 0.0226(18) 0.0274(19) -0.0010(16) -0.0063(16) -0.0045(16) S3 0.0227(19) 0.0278(19) 0.038(2) -0.0069(18) 0.0084(18) -0.0033(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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' 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 S2 Sn1 S1 114.04(15) . . ? S2 Sn1 S3 106.93(16) . . ? S1 Sn1 S3 116.20(16) . . ? S2 Sn1 S3 113.14(16) . 7_554 ? S1 Sn1 S3 102.62(15) . 7_554 ? S3 Sn1 S3 103.52(14) . 7_554 ? S2 Sn1 K1 48.57(11) . . ? S1 Sn1 K1 153.51(13) . . ? S3 Sn1 K1 63.17(14) . . ? S3 Sn1 K1 103.10(12) 7_554 . ? S1 Ag1 S1 177.1(2) 14 . ? S1 Ag1 Ag2 88.57(11) 14 . ? S1 Ag1 Ag2 88.57(11) . . ? S1 Ag1 K1 58.54(11) 14 15_455 ? S1 Ag1 K1 120.19(12) . 15_455 ? Ag2 Ag1 K1 67.61(8) . 15_455 ? S1 Ag1 K1 120.19(12) 14 16_545 ? S1 Ag1 K1 58.54(11) . 16_545 ? Ag2 Ag1 K1 67.61(8) . 16_545 ? K1 Ag1 K1 135.21(16) 15_455 16_545 ? S1 Ag1 K1 133.00(13) 14 7 ? S1 Ag1 K1 49.61(12) . 7 ? Ag2 Ag1 K1 132.89(7) . 7 ? K1 Ag1 K1 111.35(10) 15_455 7 ? K1 Ag1 K1 98.89(6) 16_545 7 ? S1 Ag1 K1 49.61(12) 14 8_545 ? S1 Ag1 K1 133.00(13) . 8_545 ? Ag2 Ag1 K1 132.89(7) . 8_545 ? K1 Ag1 K1 98.89(6) 15_455 8_545 ? K1 Ag1 K1 111.35(10) 16_545 8_545 ? K1 Ag1 K1 94.22(13) 7 8_545 ? S2 Ag2 S2 175.0(2) . 14 ? S2 Ag2 Ag1 87.48(11) . . ? S2 Ag2 Ag1 87.48(11) 14 . ? S2 Ag2 K1 116.75(13) . 16_545 ? S2 Ag2 K1 60.69(12) 14 16_545 ? Ag1 Ag2 K1 63.32(7) . 16_545 ? S2 Ag2 K1 60.68(12) . 15_455 ? S2 Ag2 K1 116.75(13) 14 15_455 ? Ag1 Ag2 K1 63.32(7) . 15_455 ? K1 Ag2 K1 126.64(14) 16_545 15_455 ? S2 Ag2 K1 127.74(13) . 8_544 ? S2 Ag2 K1 56.23(12) 14 8_544 ? Ag1 Ag2 K1 129.61(7) . 8_544 ? K1 Ag2 K1 113.12(10) 16_545 8_544 ? K1 Ag2 K1 100.36(5) 15_455 8_544 ? S2 Ag2 K1 56.23(12) . 7_554 ? S2 Ag2 K1 127.74(14) 14 7_554 ? Ag1 Ag2 K1 129.61(7) . 7_554 ? K1 Ag2 K1 100.36(6) 16_545 7_554 ? K1 Ag2 K1 113.12(10) 15_455 7_554 ? K1 Ag2 K1 100.78(13) 8_544 7_554 ? S2 K1 S1 141.15(19) . 12_554 ? S2 K1 S1 123.78(17) . 15_454 ? S1 K1 S1 90.44(11) 12_554 15_454 ? S2 K1 S3 90.15(16) . 9_454 ? S1 K1 S3 117.64(17) 12_554 9_454 ? S1 K1 S3 76.94(15) 15_454 9_454 ? S2 K1 S2 83.25(14) . 15_455 ? S1 K1 S2 79.87(14) 12_554 15_455 ? S1 K1 S2 139.76(17) 15_454 15_455 ? S3 K1 S2 73.54(14) 9_454 15_455 ? S2 K1 S2 81.94(14) . 7_554 ? S1 K1 S2 98.55(15) 12_554 7_554 ? S1 K1 S2 66.09(13) 15_454 7_554 ? S3 K1 S2 127.96(17) 9_454 7_554 ? S2 K1 S2 153.7(2) 15_455 7_554 ? S2 K1 Ag1 111.97(14) . 7_554 ? S1 K1 Ag1 39.29(9) 12_554 7_554 ? S1 K1 Ag1 95.87(12) 15_454 7_554 ? S3 K1 Ag1 156.52(15) 9_454 7_554 ? S2 K1 Ag1 100.39(14) 15_455 7_554 ? S2 K1 Ag1 65.74(11) 7_554 7_554 ? S2 K1 S3 67.00(13) . . ? S1 K1 S3 74.28(13) 12_554 . ? S1 K1 S3 145.72(16) 15_454 . ? S3 K1 S3 137.34(19) 9_454 . ? S2 K1 S3 68.54(13) 15_455 . ? S2 K1 S3 85.67(13) 7_554 . ? Ag1 K1 S3 53.11(9) 7_554 . ? S2 K1 Ag2 119.63(14) . 7_554 ? S1 K1 Ag2 66.32(11) 12_554 7_554 ? S1 K1 Ag2 50.02(10) 15_454 7_554 ? S3 K1 Ag2 126.85(16) 9_454 7_554 ? S2 K1 Ag2 145.70(15) 15_455 7_554 ? S2 K1 Ag2 38.05(8) 7_554 7_554 ? Ag1 K1 Ag2 49.07(7) 7_554 7_554 ? S3 K1 Ag2 95.76(11) . 7_554 ? S2 K1 Ag2 119.99(14) . 15_455 ? S1 K1 Ag2 48.59(10) 12_554 15_455 ? S1 K1 Ag2 111.10(13) 15_454 15_455 ? S3 K1 Ag2 79.59(11) 9_454 15_455 ? S2 K1 Ag2 37.01(8) 15_455 15_455 ? S2 K1 Ag2 146.93(14) 7_554 15_455 ? Ag1 K1 Ag2 82.37(9) 7_554 15_455 ? S3 K1 Ag2 81.76(11) . 15_455 ? Ag2 K1 Ag2 113.12(10) 7_554 15_455 ? S2 K1 Sn1 33.91(9) . . ? S1 K1 Sn1 108.81(14) 12_554 . ? S1 K1 Sn1 136.92(14) 15_454 . ? S3 K1 Sn1 121.81(14) 9_454 . ? S2 K1 Sn1 82.62(11) 15_455 . ? S2 K1 Sn1 73.00(10) 7_554 . ? Ag1 K1 Sn1 78.69(8) 7_554 . ? S3 K1 Sn1 35.44(8) . . ? Ag2 K1 Sn1 102.32(9) 7_554 . ? Ag2 K1 Sn1 110.41(10) 15_455 . ? S2 K1 Ag1 133.20(15) . 15_454 ? S1 K1 Ag1 85.21(12) 12_554 15_454 ? S1 K1 Ag1 34.39(9) 15_454 15_454 ? S3 K1 Ag1 51.46(10) 9_454 15_454 ? S2 K1 Ag1 105.49(13) 15_455 15_454 ? S2 K1 Ag1 100.49(12) 7_554 15_454 ? Ag1 K1 Ag1 111.35(10) 7_554 15_454 ? S3 K1 Ag1 159.29(13) . 15_454 ? Ag2 K1 Ag1 78.21(8) 7_554 15_454 ? Ag2 K1 Ag1 82.50(8) 15_455 15_454 ? Sn1 K1 Ag1 165.09(12) . 15_454 ? Sn1 S1 Ag1 99.34(16) . . ? Sn1 S1 K1 117.25(18) . 16_545 ? Ag1 S1 K1 82.17(14) . 16_545 ? Sn1 S1 K1 102.92(15) . 7 ? Ag1 S1 K1 96.00(15) . 7 ? K1 S1 K1 139.60(18) 16_545 7 ? Sn1 S2 Ag2 101.69(17) . . ? Sn1 S2 K1 97.52(15) . . ? Ag2 S2 K1 160.8(2) . . ? Sn1 S2 K1 94.97(16) . 7_554 ? Ag2 S2 K1 86.76(14) . 7_554 ? K1 S2 K1 92.66(16) . 7_554 ? Sn1 S2 K1 110.30(17) . 15_455 ? Ag2 S2 K1 81.27(14) . 15_455 ? K1 S2 K1 91.14(15) . 15_455 ? K1 S2 K1 153.7(2) 7_554 15_455 ? Sn1 S3 Sn1 110.54(17) . 15_455 ? Sn1 S3 K1 103.46(17) . 9 ? Sn1 S3 K1 131.0(2) 15_455 9 ? Sn1 S3 K1 81.39(15) . . ? Sn1 S3 K1 82.96(14) 15_455 . ? K1 S3 K1 137.34(19) 9 . ? 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 Sn1 S2 2.343(5) . ? Sn1 S1 2.367(4) . ? Sn1 S3 2.442(4) . ? Sn1 S3 2.453(5) 7_554 ? Sn1 K1 4.164(4) . ? Ag1 S1 2.384(4) 14 ? Ag1 S1 2.384(4) . ? Ag1 Ag2 3.153(3) . ? Ag1 K1 3.729(4) 15_455 ? Ag1 K1 3.729(4) 16_545 ? Ag1 K1 4.196(5) 7 ? Ag1 K1 4.196(5) 8_545 ? Ag2 S2 2.406(4) . ? Ag2 S2 2.406(4) 14 ? Ag2 K1 3.859(4) 16_545 ? Ag2 K1 3.859(4) 15_455 ? Ag2 K1 3.991(4) 8_544 ? Ag2 K1 3.991(4) 7_554 ? K1 S2 3.149(6) . ? K1 S1 3.211(6) 12_554 ? K1 S1 3.214(6) 15_454 ? K1 S3 3.272(6) 9_454 ? K1 S2 3.323(6) 15_455 ? K1 S2 3.404(6) 7_554 ? K1 S3 3.758(7) . ?