Mixed-anion chalcogenide-halide semiconductors A<sub>2</sub>BaTaS<sub>4</sub>Cl (A = K, Rb, Cs) and K<sub>2</sub>BaNbS<sub>4</sub>Cl.
Ie, Thomas S.; Nathan, Siddhartha S.; Rondinelli, James M.; Kanatzidis, Mercouri G.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13588–13597; doi:10.1039/d5dt01676b

data_7719294
_publ_section_title
;
 Mixed-anion chalcogenide-halide semiconductors
 A<sub>2</sub>BaTaS<sub>4</sub>Cl (A = K, Rb, Cs) and
 K<sub>2</sub>BaNbS<sub>4</sub>Cl.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13588
_journal_page_last               13597
_journal_paper_doi               10.1039/d5dt01676b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'Ba1 Cl Cs2 S4 Ta'
_chemical_formula_sum            'Ba Cl Cs2 S4 Ta'
_chemical_formula_weight         747.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-13 deposited with the CCDC.	2025-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   12.7216(2)
_cell_length_b                   25.4311(4)
_cell_length_c                   14.1934(3)
_cell_measurement_reflns_used    16793
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      33.5710
_cell_measurement_theta_min      2.8550
_cell_volume                     4591.91(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.136a 64-bit (release 23-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.908
_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    -10.00  98.00   0.50  100.00    --   17.62  23.00-107.00  216
  2  \w    -10.00  98.00   0.50  100.00    --   17.62  23.00-107.00  216
  3  \w     42.00  96.00   0.50  100.00    --   17.62 178.00 -30.00  108
  4  \w     10.00  67.00   0.50  100.00    --   17.62-120.00  18.00  114
  5  \w     42.00  96.00   0.50  100.00    --   17.62 178.00  60.00  108
  6  \w     42.00  96.00   0.50  100.00    --   17.62 178.00   0.00  108
  7  \w    -96.00 -41.00   0.50  100.00    --  -18.41-178.00  90.00  110
  8  \w    -63.00 -38.00   0.50  100.00    --   17.62 -23.00  88.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0277194000
_diffrn_orient_matrix_UB_12      0.0226549000
_diffrn_orient_matrix_UB_13      0.0152741000
_diffrn_orient_matrix_UB_21      -0.0479068000
_diffrn_orient_matrix_UB_22      -0.0142407000
_diffrn_orient_matrix_UB_23      -0.0020238000
_diffrn_orient_matrix_UB_31      0.0068608000
_diffrn_orient_matrix_UB_32      -0.0078895000
_diffrn_orient_matrix_UB_33      0.0475113000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            38084
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.614
_diffrn_reflns_theta_min         2.681
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.076
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.70a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.327
_exptl_crystal_description       block
_exptl_crystal_F_000             5120
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.024
_refine_diff_density_max         5.165
_refine_diff_density_min         -1.871
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         4277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0306P)^2^+25.1787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3606
_reflns_number_total             4277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01676b2.cif
_cod_data_source_block           full5_block_100k
_cod_depositor_comments
'Adding full bibliography for 7719288--7719294.cif.'
_cod_database_code               7719294
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cs2 Ba Ta S4 Cl'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8662(19)
 0.1338(19)
2. Shared sites
{Ba1, Cs1}
{Ba2, Cs2}
3. Uiso/Uaniso restraints and constraints
Uanis(Ba1) = Uanis(Cs1)
Uanis(Ba2) = Uanis(Cs2)
4. Others
 Fixed Sof: Ba1(0.166667) Ba2(0.333333) Cs1(0.083333) Cs2(0.166667)
;
_shelx_res_checksum              99516
_shelx_hkl_checksum              59867
_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 2.573
_oxdiff_exptl_absorpt_empirical_full_min 0.712