#------------------------------------------------------------------------------ #$Date: 2024-01-06 10:06:41 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288811 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/75/7247567.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_7247567 loop_ _publ_author_name 'Cicirello, Andrea' 'Swindle, Andrew' 'Wang, Jian' _publ_section_title ; Visualizing the alignment of lone pair electrons in La3AsS5Br2 and La5As2S9Cl3 to form an acentric or centrosymmetric structure ; _journal_issue 45 _journal_name_full CrystEngComm _journal_page_first 6354 _journal_page_last 6360 _journal_paper_doi 10.1039/D3CE00834G _journal_volume 25 _journal_year 2023 _chemical_formula_sum 'As2 Cl3 La5 S9' _chemical_formula_weight 1239.28 _space_group_crystal_system orthorhombic _space_group_IT_number 57 _space_group_name_Hall '-P 2c 2b' _space_group_name_H-M_alt 'P b c m' _audit_creation_method SHELXL-2019/1 _audit_update_record ; 2023-07-15 deposited with the CCDC. 2023-10-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.0472(3) _cell_length_b 7.1152(3) _cell_length_c 37.1137(13) _cell_measurement_reflns_used 4561 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 51.179 _cell_measurement_theta_min 2.381 _cell_volume 1860.96(13) _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_publication_material 'SHELXL-2019 (Sheldrick, 2019)' _computing_structure_refinement 'SHELXL-2019 (Sheldrick, 2019)' _computing_structure_solution 'SHELXS-2019 (Sheldrick, 2019)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker X8 PROSPECTOR' _diffrn_measurement_method 'profile data from \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_unetI/netI 0.0366 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 4561 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 51.179 _diffrn_reflns_theta_max 51.179 _diffrn_reflns_theta_min 2.381 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 103.931 _exptl_absorpt_correction_T_max 3.09 _exptl_absorpt_correction_T_min 1.03 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 4.423 _exptl_crystal_description Block _exptl_crystal_F_000 2184 _exptl_crystal_size_max 0.030 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.010 _refine_diff_density_max 2.380 _refine_diff_density_min -2.390 _refine_diff_density_rms 0.375 _refine_ls_extinction_coef 0.00015(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2019/1 (Sheldrick 2019)' _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 43 _refine_ls_number_reflns 1019 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0398 _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^)+(0.0736P)^2^+35.3120P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1123 _refine_ls_wR_factor_ref 0.1138 _reflns_Friedel_coverage 0.000 _reflns_number_gt 957 _reflns_number_total 1019 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00834g2.cif _cod_data_source_block x1_CCDC1 _cod_depositor_comments 'Adding full bibliography for 7247566--7247567.cif.' _cod_database_code 7247567 _shelx_shelxl_version_number 2019/1 _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 0.147 _shelx_estimated_absorpt_t_max 0.423 _shelx_res_file ; TITL x1 in Pbcm x1.res created by SHELXL-2019/1 at 10:07:07 on 13-Jul-2023 CELL 1.54178 7.04720 7.11520 37.11370 90.0000 90.0000 90.0000 ZERR 4.00 0.00030 0.00030 0.00130 0.0000 0.0000 0.0000 LATT 1 SYMM -X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM X, 0.5-Y, -Z SFAC S CL AS LA UNIT 36 12 8 20 TEMP 23.000 SIZE 0.01 0.02 0.03 L.S. 14 BOND acta twin FMAP 2 PLAN -5 WGHT 0.073600 35.311996 EXTI 0.000151 BASF 1.20056 FVAR 0.03600 LA1 4 0.792815 0.193294 0.750000 10.50000 0.00303 LA2 4 1.205199 0.274591 0.839268 11.00000 0.00445 LA3 4 0.714531 0.041649 0.957526 11.00000 0.00363 AS1 3 0.691887 0.308047 0.867814 11.00000 0.00635 S1 1 0.917327 0.105893 0.887866 11.00000 0.00590 S2 1 1.452454 0.247852 0.907162 11.00000 0.00520 S3 1 0.580084 0.124661 0.677079 11.00000 0.00603 S4 1 0.613667 -0.168432 0.750000 10.50000 0.01142 S5 1 1.112033 -0.090262 0.964710 11.00000 0.00867 CL1 2 0.553804 -0.250000 1.000000 10.50000 0.00674 CL2 2 1.057859 -0.020705 0.703327 11.00000 0.00784 HKLF 4 REM x1 in Pbcm REM wR2 = 0.1138, GooF = S = 1.046, Restrained GooF = 1.046 for all data REM R1 = 0.0398 for 957 Fo > 4sig(Fo) and 0.0414 for all 1019 data REM 43 parameters refined using 0 restraints END WGHT 0.0734 35.4605 REM Highest difference peak 2.380, deepest hole -2.390, 1-sigma level 0.375 Q1 1 0.7934 0.2813 0.7500 10.50000 0.05 2.38 Q2 1 0.7906 -0.1546 0.6674 11.00000 0.05 2.38 Q3 1 0.7138 0.1287 0.9582 11.00000 0.05 2.37 Q4 1 0.8013 0.1082 0.7500 10.50000 0.05 2.32 Q5 1 0.8014 -0.2963 0.6513 11.00000 0.05 2.31 ; _shelx_res_checksum 75372 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, 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_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 La1 La 0.79282(15) 0.19329(15) 0.750000 0.0030(4) Uiso 1 2 d S . P . . La2 La 1.20520(11) 0.27459(11) 0.83927(2) 0.0044(4) Uiso 1 1 d . . . . . La3 La 0.71453(11) 0.04165(10) 0.95753(2) 0.0036(4) Uiso 1 1 d . . . . . As1 As 0.6919(2) 0.3080(2) 0.86781(4) 0.0064(5) Uiso 1 1 d . . . . . S1 S 0.9173(5) 0.1059(4) 0.88787(8) 0.0059(8) Uiso 1 1 d . . . . . S2 S 1.4525(5) 0.2479(4) 0.90716(8) 0.0052(8) Uiso 1 1 d . . . . . S3 S 0.5801(4) 0.1247(5) 0.67708(8) 0.0060(8) Uiso 1 1 d . . . . . S4 S 0.6137(7) -0.1684(7) 0.750000 0.0114(12) Uiso 1 2 d S . P . . S5 S 1.1120(5) -0.0903(5) 0.96471(8) 0.0087(8) Uiso 1 1 d . . . . . Cl1 Cl 0.5538(7) -0.250000 1.000000 0.0067(11) Uiso 1 2 d S . P . . Cl2 Cl 1.0579(5) -0.0207(4) 0.70333(8) 0.0078(8) Uiso 1 1 d . . . . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -1.4094 9.0376 '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 S4 La1 Cl2 142.89(6) . 3_756 ? S4 La1 Cl2 142.89(6) . 8_765 ? Cl2 La1 Cl2 74.18(12) 3_756 8_765 ? S4 La1 Cl2 79.43(10) . 6_557 ? Cl2 La1 Cl2 77.34(6) 3_756 6_557 ? Cl2 La1 Cl2 119.01(6) 8_765 6_557 ? S4 La1 Cl2 79.43(10) . . ? Cl2 La1 Cl2 119.01(6) 3_756 . ? Cl2 La1 Cl2 77.34(6) 8_765 . ? Cl2 La1 Cl2 71.42(12) 6_557 . ? S4 La1 S4 82.83(8) . 3_656 ? Cl2 La1 S4 96.68(10) 3_756 3_656 ? Cl2 La1 S4 96.68(10) 8_765 3_656 ? Cl2 La1 S4 139.63(8) 6_557 3_656 ? Cl2 La1 S4 139.63(8) . 3_656 ? S4 La1 S3 69.47(8) . . ? Cl2 La1 S3 143.80(9) 3_756 . ? Cl2 La1 S3 76.39(9) 8_765 . ? Cl2 La1 S3 136.52(9) 6_557 . ? Cl2 La1 S3 73.56(8) . . ? S4 La1 S3 66.29(7) 3_656 . ? S4 La1 S3 69.47(8) . 6_557 ? Cl2 La1 S3 76.39(9) 3_756 6_557 ? Cl2 La1 S3 143.80(9) 8_765 6_557 ? Cl2 La1 S3 73.56(8) 6_557 6_557 ? Cl2 La1 S3 136.52(9) . 6_557 ? S4 La1 S3 66.30(7) 3_656 6_557 ? S3 La1 S3 119.55(12) . 6_557 ? Cl2 La2 Cl2 80.21(6) 6_557 3_756 ? Cl2 La2 S3 86.82(10) 6_557 6_657 ? Cl2 La2 S3 131.62(9) 3_756 6_657 ? Cl2 La2 S1 77.77(9) 6_557 . ? Cl2 La2 S1 95.71(10) 3_756 . ? S3 La2 S1 126.75(9) 6_657 . ? Cl2 La2 S3 134.00(9) 6_557 3_756 ? Cl2 La2 S3 77.83(9) 3_756 3_756 ? S3 La2 S3 78.64(5) 6_657 3_756 ? S1 La2 S3 144.06(8) . 3_756 ? Cl2 La2 S2 128.43(9) 6_557 . ? Cl2 La2 S2 149.29(8) 3_756 . ? S3 La2 S2 68.50(9) 6_657 . ? S1 La2 S2 82.19(8) . . ? S3 La2 S2 86.02(9) 3_756 . ? Cl2 La2 S1 142.23(10) 6_557 8_765 ? Cl2 La2 S1 75.60(8) 3_756 8_765 ? S3 La2 S1 130.85(9) 6_657 8_765 ? S1 La2 S1 76.28(7) . 8_765 ? S3 La2 S1 67.84(9) 3_756 8_765 ? S2 La2 S1 74.15(8) . 8_765 ? Cl2 La2 As1 63.14(7) 6_557 8_755 ? Cl2 La2 As1 141.03(7) 3_756 8_755 ? S3 La2 As1 62.33(7) 6_657 8_755 ? S1 La2 As1 65.24(7) . 8_755 ? S3 La2 As1 137.52(7) 3_756 8_755 ? S2 La2 As1 65.30(6) . 8_755 ? S1 La2 As1 126.47(6) 8_765 8_755 ? Cl1 La3 Cl1 79.05(3) . 5_657 ? Cl1 La3 S5 140.89(7) . 8_765 ? Cl1 La3 S5 76.19(9) 5_657 8_765 ? Cl1 La3 S5 95.48(11) . . ? Cl1 La3 S5 137.33(9) 5_657 . ? S5 La3 S5 83.08(6) 8_765 . ? Cl1 La3 S1 141.45(7) . . ? Cl1 La3 S1 135.25(7) 5_657 . ? S5 La3 S1 74.94(9) 8_765 . ? S5 La3 S1 71.01(9) . . ? Cl1 La3 S2 117.13(11) . 1_455 ? Cl1 La3 S2 71.66(7) 5_657 1_455 ? S5 La3 S2 82.85(9) 8_765 1_455 ? S5 La3 S2 142.15(9) . 1_455 ? S1 La3 S2 71.44(9) . 1_455 ? Cl1 La3 S2 71.62(7) . 8_755 ? Cl1 La3 S2 115.92(10) 5_657 8_755 ? S5 La3 S2 147.10(9) 8_765 8_755 ? S5 La3 S2 101.72(9) . 8_755 ? S1 La3 S2 76.03(9) . 8_755 ? S2 La3 S2 73.49(6) 1_455 8_755 ? Cl1 La3 S5 74.15(8) . 5_757 ? Cl1 La3 S5 72.33(9) 5_657 5_757 ? S5 La3 S5 69.74(11) 8_765 5_757 ? S5 La3 S5 65.57(11) . 5_757 ? S1 La3 S5 126.12(10) . 5_757 ? S2 La3 S5 138.84(9) 1_455 5_757 ? S2 La3 S5 142.00(9) 8_755 5_757 ? S3 As1 S1 96.89(12) 6_557 . ? S3 As1 S2 96.09(12) 6_557 1_455 ? S1 As1 S2 100.94(12) . 1_455 ? S3 As1 La2 112.98(10) 6_557 8_765 ? S1 As1 La2 123.11(10) . 8_765 ? S2 As1 La2 121.23(9) 1_455 8_765 ? As1 S1 La2 91.31(11) . . ? As1 S1 La3 92.63(11) . . ? La2 S1 La3 156.09(12) . . ? As1 S1 La2 95.54(11) . 8_755 ? La2 S1 La2 98.32(9) . 8_755 ? La3 S1 La2 104.74(10) . 8_755 ? As1 S2 La3 92.02(11) 1_655 1_655 ? As1 S2 La3 123.56(13) 1_655 8_765 ? La3 S2 La3 101.00(9) 1_655 8_765 ? As1 S2 La2 83.24(10) 1_655 . ? La3 S2 La2 152.68(11) 1_655 . ? La3 S2 La2 104.02(10) 8_765 . ? As1 S3 La2 87.20(10) 6_557 6_457 ? As1 S3 La2 98.96(11) 6_557 3_746 ? La2 S3 La2 136.46(12) 6_457 3_746 ? As1 S3 La1 112.36(12) 6_557 . ? La2 S3 La1 123.85(11) 6_457 . ? La2 S3 La1 93.63(9) 3_746 . ? La1 S4 La1 135.08(18) . 3_646 ? La3 S5 La3 132.45(12) 8_755 . ? La3 S5 La3 91.14(10) 8_755 5_757 ? La3 S5 La3 114.43(11) . 5_757 ? La3 Cl1 La3 133.02(18) . 4_547 ? La3 Cl1 La3 109.55(4) . 8_655 ? La3 Cl1 La3 100.95(4) 4_547 8_655 ? La3 Cl1 La3 100.95(4) . 5_657 ? La3 Cl1 La3 109.55(4) 4_547 5_657 ? La3 Cl1 La3 97.70(14) 8_655 5_657 ? La2 Cl2 La2 108.05(10) 6_557 3_746 ? La2 Cl2 La1 136.83(13) 6_557 3_746 ? La2 Cl2 La1 102.22(10) 3_746 3_746 ? La2 Cl2 La1 100.15(9) 6_557 . ? La2 Cl2 La1 100.21(11) 3_746 . ? La1 Cl2 La1 104.01(9) 3_746 . ? 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 La1 S4 2.867(5) . ? La1 Cl2 2.872(3) 3_756 ? La1 Cl2 2.872(3) 8_765 ? La1 Cl2 2.968(3) 6_557 ? La1 Cl2 2.968(3) . ? La1 S4 3.029(5) 3_656 ? La1 S3 3.132(3) . ? La1 S3 3.132(3) 6_557 ? La2 Cl2 2.827(3) 6_557 ? La2 Cl2 2.839(3) 3_756 ? La2 S3 2.913(3) 6_657 ? La2 S1 2.968(3) . ? La2 S3 2.977(3) 3_756 ? La2 S2 3.069(3) . ? La2 S1 3.091(3) 8_765 ? La2 As1 3.5592(16) 8_755 ? La3 Cl1 2.841(2) . ? La3 Cl1 2.874(3) 5_657 ? La3 S5 2.902(4) 8_765 ? La3 S5 2.966(4) . ? La3 S1 2.989(3) . ? La3 S2 3.010(3) 1_455 ? La3 S2 3.041(3) 8_755 ? La3 S5 3.153(3) 5_757 ? As1 S3 2.258(3) 6_557 ? As1 S1 2.269(3) . ? As1 S2 2.272(4) 1_455 ?