[Ba4X][In19S32] (X = Cl, Br): two quaternary metal chalcohalides exhibiting remarkable photocurrent responses
Tang, Chunlan; Xing, Wen-Hao; Liang, Fei; Tang, Jian; Wu, Jieyun; Yin, Wenlong; Bin, Kang; Dalton Transactions  (2023) –; doi:10.1039/D3DT02766J

data_7714015
_publ_section_title
;
 [Ba4X][In19S32] (X = Cl, Br): two quaternary metal chalcohalides
 exhibiting remarkable photocurrent responses
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02766J
_journal_year                    2023
_chemical_formula_moiety         '0.25(Ba16 Cl4 In76 S128)'
_chemical_formula_sum            'Ba4 Cl In19 S32'
_chemical_formula_weight         3792.31
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d :2'
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-08-15 deposited with the CCDC.	2023-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6105(6)
_cell_length_b                   22.6105(6)
_cell_length_c                   10.4904(4)
_cell_measurement_reflns_used    8172
_cell_measurement_temperature    295.4(3)
_cell_measurement_theta_max      26.3780
_cell_measurement_theta_min      3.2990
_cell_volume                     5363.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.4(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -33.00  11.00   0.50   30.00    --   -8.37 -73.00 -67.00   88
  2  \w    -23.00   4.00   0.50   30.00    --   -8.37 -99.00 -90.00   54
  3  \w    -80.00 -41.00   0.50   30.00    --   -8.37 -73.00 -67.00   78
  4  \w    -16.00  20.00   0.50   30.00    --   -8.37 -99.00 150.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0155042000
_diffrn_orient_matrix_UB_12      -0.0098677000
_diffrn_orient_matrix_UB_13      0.0548325000
_diffrn_orient_matrix_UB_21      -0.0185705000
_diffrn_orient_matrix_UB_22      0.0252439000
_diffrn_orient_matrix_UB_23      -0.0033589000
_diffrn_orient_matrix_UB_31      -0.0199512000
_diffrn_orient_matrix_UB_32      -0.0158290000
_diffrn_orient_matrix_UB_33      -0.0393998000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10826
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         2.798
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    4.697
_exptl_crystal_description       block
_exptl_crystal_F_000             6736
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.039
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.000016(3)
_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   1.238
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+7.2481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1407
_reflns_number_total             1444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02766j2.cif
_cod_data_source_block           '[Ba4Cl][In19S32]'
_cod_original_cell_volume        5363.1(4)
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               7714015
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         BaInPSCl
_chemical_oxdiff_usercomment     '4/m  0.75 0.5 43S RT'
_shelx_estimated_absorpt_t_max   0.581
_shelx_estimated_absorpt_t_min   0.442
_reflns_odcompleteness_completeness 82.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
;
_shelx_res_checksum              27993
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.086
_oxdiff_exptl_absorpt_empirical_full_min 0.611