#------------------------------------------------------------------------------ #$Date: 2023-10-24 01:40:04 +0300 (Tue, 24 Oct 2023) $ #$Revision: 287080 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/75/7247566.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_7247566 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_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE00834G _journal_year 2023 _chemical_formula_sum 'As Br2 La3 S5' _chemical_formula_weight 811.77 _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 1' _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 98.471(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 22.3092(14) _cell_length_b 7.1387(5) _cell_length_c 7.1638(5) _cell_measurement_reflns_used 165 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.997 _cell_measurement_theta_min 2.007 _cell_volume 1128.45(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, 1997)' _computing_structure_refinement 'SHELXL-2019 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-2019 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _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 0.0471 _diffrn_reflns_av_unetI/netI 0.0525 _diffrn_reflns_Laue_measured_fraction_full 0.972 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_number 508 _diffrn_reflns_point_group_measured_fraction_full 0.771 _diffrn_reflns_point_group_measured_fraction_max 0.771 _diffrn_reflns_theta_full 25.997 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_min 2.007 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 105.859 _exptl_absorpt_correction_T_max 3.20 _exptl_absorpt_correction_T_min 1.10 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 4.778 _exptl_crystal_description block _exptl_crystal_F_000 1416 _exptl_crystal_size_max 0.030 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.010 _refine_diff_density_max 0.894 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.218 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.22(7) _refine_ls_extinction_coef 0.0019(3) _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 0.832 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 47 _refine_ls_number_reflns 165 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 0.825 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0444 _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^)+(0.1354P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1058 _refine_ls_wR_factor_ref 0.1058 _reflns_Friedel_coverage 0.571 _reflns_Friedel_fraction_full 0.566 _reflns_Friedel_fraction_max 0.566 _reflns_number_gt 163 _reflns_number_total 165 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00834g2.cif _cod_data_source_block x1 _cod_original_sg_symbol_H-M 'C c' _cod_database_code 7247566 _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 0.143 _shelx_estimated_absorpt_t_max 0.417 _shelx_res_file ; TITL wjc038_0m in Cc x1.res created by SHELXL-2019/1 at 10:30:14 on 13-Jul-2023 CELL 1.54178 22.30920 7.13870 7.16380 90.0000 98.4714 90.0000 ZERR 4.00 0.00140 0.00050 0.00050 0.0000 0.0024 0.0000 LATT -7 SYMM X, -Y, 0.5+Z SFAC S AS BR LA UNIT 20 4 8 12 TEMP 23.000 SIZE 0.01 0.02 0.03 L.S. 14 BOND acta TWIN omit -2 52 FMAP 2 PLAN -5 WGHT 0.135400 EXTI 0.001933 BASF 0.21888 FVAR 0.06514 LA1 4 0.122688 0.197749 0.369482 11.00000 0.01924 LA2 4 -0.027795 0.197391 -0.125924 11.00000 0.01829 LA3 4 0.274413 0.208086 0.012911 11.00000 0.01885 AS1 2 0.318919 0.308970 -0.425383 11.00000 0.02334 BR1 3 0.116113 0.378873 -0.019903 11.00000 0.01930 BR2 3 -0.016537 0.387206 0.257009 11.00000 0.03433 S1 1 -0.147678 0.408247 -0.114601 11.00000 0.01985 S2 1 0.200964 0.054892 0.693114 11.00000 0.00206 S3 1 -0.116362 -0.045915 0.049428 11.00000 0.01056 S4 1 0.243135 0.422208 0.354457 11.00000 0.00245 S5 1 0.046615 0.052471 0.614662 11.00000 0.02414 HKLF 4 REM wjc038_0m in Cc REM wR2 = 0.1058, GooF = S = 0.832, Restrained GooF = 0.825 for all data REM R1 = 0.0444 for 163 Fo > 4sig(Fo) and 0.0444 for all 165 data REM 47 parameters refined using 2 restraints END WGHT 0.0918 0.0000 REM Highest difference peak 0.894, deepest hole -0.667, 1-sigma level 0.218 Q1 1 0.1254 0.1861 0.8162 11.00000 0.05 0.89 Q2 1 -0.0277 0.1850 -0.5924 11.00000 0.05 0.88 Q3 1 0.2731 0.1890 0.5053 11.00000 0.05 0.65 Q4 1 0.1198 0.2999 0.5201 11.00000 0.05 0.60 Q5 1 -0.0207 0.2995 -0.3018 11.00000 0.05 0.55 ; _shelx_res_checksum 39070 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, 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_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 0.1227(5) 0.1977(12) 0.3695(16) 0.019(8) Uiso 1 1 d . . . . . La2 La -0.0278(5) 0.1974(13) -0.1259(18) 0.018(8) Uiso 1 1 d . . . . . La3 La 0.2744(6) 0.2081(15) 0.013(2) 0.019(8) Uiso 1 1 d . . . . . As1 As 0.3189(10) 0.309(2) -0.425(4) 0.023(10) Uiso 1 1 d . . . . . Br1 Br 0.1161(9) 0.379(3) -0.020(3) 0.019(10) Uiso 1 1 d . . . . . Br2 Br -0.0165(7) 0.387(3) 0.257(3) 0.034(10) Uiso 1 1 d . . . . . S1 S -0.148(2) 0.408(7) -0.115(8) 0.020(18) Uiso 1 1 d . . . . . S2 S 0.201(2) 0.055(6) 0.693(9) 0.002(16) Uiso 1 1 d . . . . . S3 S -0.116(2) -0.046(6) 0.049(8) 0.01(2) Uiso 1 1 d . . . . . S4 S 0.2431(18) 0.422(5) 0.354(7) 0.00(2) Uiso 1 1 d . . . . . S5 S 0.047(3) 0.052(5) 0.615(8) 0.024(18) 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' As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 '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 S2 La1 S5 73.5(14) . . ? S2 La1 S5 121.1(11) . 2_554 ? S5 La1 S5 79.4(12) . 2_554 ? S2 La1 S2 78.4(11) . 2_554 ? S5 La1 S2 119.7(14) . 2_554 ? S5 La1 S2 71.4(17) 2_554 2_554 ? S2 La1 Br1 145.8(12) . . ? S5 La1 Br1 140.6(14) . . ? S5 La1 Br1 75.1(12) 2_554 . ? S2 La1 Br1 79.5(12) 2_554 . ? S2 La1 Br1 100.6(9) . 2_565 ? S5 La1 Br1 98.2(10) . 2_565 ? S5 La1 Br1 134.8(10) 2_554 2_565 ? S2 La1 Br1 139.2(11) 2_554 2_565 ? Br1 La1 Br1 79.9(4) . 2_565 ? S2 La1 S4 77.7(12) . . ? S5 La1 S4 143.7(16) . . ? S5 La1 S4 135.5(18) 2_554 . ? S2 La1 S4 74.4(12) 2_554 . ? Br1 La1 S4 71.3(11) . . ? Br1 La1 S4 65.7(7) 2_565 . ? S2 La1 Br2 139.7(12) . . ? S5 La1 Br2 71.2(12) . . ? S5 La1 Br2 70.5(10) 2_554 . ? S2 La1 Br2 137.0(16) 2_554 . ? Br1 La1 Br2 72.2(6) . . ? Br1 La1 Br2 66.3(5) 2_565 . ? S4 La1 Br2 123.3(9) . . ? S5 La2 S5 79.9(13) 1_554 2_554 ? S5 La2 S3 122.5(13) 1_554 . ? S5 La2 S3 75.4(17) 2_554 . ? S5 La2 Br2 140.3(13) 1_554 . ? S5 La2 Br2 76.6(14) 2_554 . ? S3 La2 Br2 81.6(11) . . ? S5 La2 S1 141.5(15) 1_554 . ? S5 La2 S1 136.3(15) 2_554 . ? S3 La2 S1 69.4(13) . . ? Br2 La2 S1 73.4(12) . . ? S5 La2 S3 75.3(14) 1_554 2_554 ? S5 La2 S3 120.0(13) 2_554 2_554 ? S3 La2 S3 73.9(9) . 2_554 ? Br2 La2 S3 144.4(11) . 2_554 ? S1 La2 S3 73.9(10) . 2_554 ? S5 La2 Br2 95.3(12) 1_554 2_564 ? S5 La2 Br2 134.5(13) 2_554 2_564 ? S3 La2 Br2 137.9(11) . 2_564 ? Br2 La2 Br2 79.5(4) . 2_564 ? S1 La2 Br2 69.2(10) . 2_564 ? S3 La2 Br2 101.8(11) 2_554 2_564 ? S5 La2 Br1 70.6(10) 1_554 . ? S5 La2 Br1 70.1(11) 2_554 . ? S3 La2 Br1 140.0(13) . . ? Br2 La2 Br1 71.5(5) . . ? S1 La2 Br1 126.6(11) . . ? S3 La2 Br1 142.0(11) 2_554 . ? Br2 La2 Br1 65.8(5) 2_564 . ? S2 La3 S2 79.3(9) 2_554 1_554 ? S2 La3 S4 129.6(12) 2_554 2_564 ? S2 La3 S4 87.6(15) 1_554 2_564 ? S2 La3 S4 76.0(15) 2_554 . ? S2 La3 S4 131.9(13) 1_554 . ? S4 La3 S4 77.8(7) 2_564 . ? S2 La3 S1 93.7(14) 2_554 3_545 ? S2 La3 S1 76.7(12) 1_554 3_545 ? S4 La3 S1 130.3(17) 2_564 3_545 ? S4 La3 S1 144.8(15) . 3_545 ? S2 La3 S3 148(2) 2_554 3 ? S2 La3 S3 132(2) 1_554 3 ? S4 La3 S3 69.3(14) 2_564 3 ? S4 La3 S3 85.1(13) . 3 ? S1 La3 S3 86.8(16) 3_545 3 ? S2 La3 S1 74.0(16) 2_554 4 ? S2 La3 S1 141.5(13) 1_554 4 ? S4 La3 S1 130.8(13) 2_564 4 ? S4 La3 S1 66.8(11) . 4 ? S1 La3 S1 78.0(11) 3_545 4 ? S3 La3 S1 74.5(15) 3 4 ? S4 As1 S1 96(2) 1_554 4_554 ? S4 As1 S3 95.6(18) 1_554 4_554 ? S1 As1 S3 101(2) 4_554 4_554 ? La1 Br1 La1 129.8(7) . 2_564 ? La1 Br1 La2 87.7(6) . . ? La1 Br1 La2 112.6(6) 2_564 . ? La2 Br2 La2 132.2(9) . 2_565 ? La2 Br2 La1 89.3(7) . . ? La2 Br2 La1 115.3(7) 2_565 . ? As1 S1 La3 93(2) 4_455 3_455 ? As1 S1 La2 92.6(17) 4_455 . ? La3 S1 La2 155(2) 3_455 . ? As1 S1 La3 98(2) 4_455 4_454 ? La3 S1 La3 100.3(14) 3_455 4_454 ? La2 S1 La3 103.1(18) . 4_454 ? La3 S2 La1 101(2) 2 . ? La3 S2 La3 108.1(17) 2 1_556 ? La1 S2 La3 136.5(15) . 1_556 ? La3 S2 La1 101.8(12) 2 2 ? La1 S2 La1 103.7(15) . 2 ? La3 S2 La1 102(2) 1_556 2 ? As1 S3 La2 93.9(16) 4_455 . ? As1 S3 La3 85.6(14) 4_455 3_445 ? La2 S3 La3 151(2) . 3_445 ? As1 S3 La2 124(2) 4_455 2 ? La2 S3 La2 97.6(14) . 2 ? La3 S3 La2 106.9(15) 3_445 2 ? As1 S4 La3 86.6(15) 1_556 2_565 ? As1 S4 La3 98.2(15) 1_556 . ? La3 S4 La3 134.1(17) 2_565 . ? As1 S4 La1 110.2(17) 1_556 . ? La3 S4 La1 127.2(17) 2_565 . ? La3 S4 La1 94.0(11) . . ? La2 S5 La2 106(2) 1_556 2 ? La2 S5 La1 137.1(13) 1_556 . ? La2 S5 La1 102(2) 2 . ? La2 S5 La1 99(2) 1_556 2 ? La2 S5 La1 103.3(12) 2 2 ? La1 S5 La1 106(2) . 2 ? 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 S2 2.88(7) . ? La1 S5 2.81(7) . ? La1 S5 2.91(6) 2_554 ? La1 S2 2.92(5) 2_554 ? La1 Br1 3.06(2) . ? La1 Br1 3.13(2) 2_565 ? La1 S4 3.14(4) . ? La1 Br2 3.37(2) . ? La2 S5 2.86(7) 1_554 ? La2 S5 2.84(5) 2_554 ? La2 S3 3.04(4) . ? La2 Br2 3.04(3) . ? La2 S1 3.08(5) . ? La2 S3 3.02(6) 2_554 ? La2 Br2 3.10(2) 2_564 ? La2 Br1 3.44(3) . ? La3 S2 2.92(5) 2_554 ? La3 S2 2.83(6) 1_554 ? La3 S4 2.92(4) 2_564 ? La3 S4 3.05(5) . ? La3 S1 2.98(6) 3_545 ? La3 S3 2.98(5) 3 ? La3 S1 3.08(5) 4 ? As1 S4 2.28(5) 1_554 ? As1 S1 2.26(5) 4_554 ? As1 S3 2.25(5) 4_554 ?