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_7719293
_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 K2 Nb S4'
_chemical_formula_sum            'Ba Cl K2 Nb S4'
_chemical_formula_weight         472.14
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-02
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_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            4
_cell_length_a                   8.3800(2)
_cell_length_b                   8.3800(2)
_cell_length_c                   14.1605(4)
_cell_measurement_reflns_used    4336
_cell_measurement_temperature    278.5(7)
_cell_measurement_theta_max      33.8180
_cell_measurement_theta_min      2.8720
_cell_volume                     994.41(4)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      278.5(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.936
_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     -2.00  85.00   0.50    0.50    --   12.93  57.00-180.00  174
  2  \w    -86.00   9.00   0.50    0.50    --  -13.71 -77.00-120.00  190
  3  \w     27.00  75.00   0.50    0.50    --   12.93-151.00-164.00   96
  4  \w    -62.00   5.00   0.50    0.50    --   12.93 -19.00-120.00  134
  5  \w      8.00  54.00   0.50    0.50    --   12.93-118.00  40.00   92
  6  \w    -61.00   3.00   0.50    0.50    --   12.93 -10.00 173.00  128
  7  \w    -62.00 -37.00   0.50    0.50    --   12.93 -19.00 120.00   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      -0.0094950000
_diffrn_orient_matrix_UB_12      0.0840737000
_diffrn_orient_matrix_UB_13      0.0012531000
_diffrn_orient_matrix_UB_21      -0.0833294000
_diffrn_orient_matrix_UB_22      -0.0097090000
_diffrn_orient_matrix_UB_23      0.0066792000
_diffrn_orient_matrix_UB_31      0.0114447000
_diffrn_orient_matrix_UB_32      -0.0008175000
_diffrn_orient_matrix_UB_33      0.0496277000
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7562
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.723
_diffrn_reflns_theta_min         2.877
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.953
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.318
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.154
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_exptl_crystal_size_rad          0.111
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00456(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     20
_refine_ls_number_reflns         525
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0155
_refine_ls_R_factor_gt           0.0139
_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^)+(0.0117P)^2^+0.5429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0306
_refine_ls_wR_factor_ref         0.0311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                485
_reflns_number_total             525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01676b2.cif
_cod_data_source_block           full_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7719288--7719294.cif.'
_cod_original_cell_volume        994.41(6)
_cod_database_code               7719293
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ba K2 Nb S4 Cl'
_cell_oxdiff_angle_alpha         89.9991(19)
_cell_oxdiff_angle_beta          89.9933(18)
_cell_oxdiff_angle_gamma         90.0113(18)
_cell_oxdiff_length_a            8.37961(17)
_cell_oxdiff_length_b            8.3806(2)
_cell_oxdiff_length_c            14.1603(3)
_cell_oxdiff_measurement_reflns_used 4336
_cell_oxdiff_volume              994.42(4)
_shelx_estimated_absorpt_t_max   0.443
_shelx_estimated_absorpt_t_min   0.246
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Shared sites
{Ba1, K1}
{Ba2, K2}
2. Uiso/Uaniso restraints and constraints
Uanis(Ba1) = Uanis(K1)
Uanis(Ba2) = Uanis(K2)
3. Others
 1*[Sof(Ba1)+Sof(K1)]+2*[Sof(Ba2)+Sof(K2)]=1 with esd of 0
 Sof(K1)=0.125*(1-FVAR(2))
 Sof(Ba1)=0.125*FVAR(2)
 Sof(K2)=0.25*(1-FVAR(3))
 Sof(Ba2)=0.25*FVAR(3)
;
_shelx_res_checksum              7402
_shelx_hkl_checksum              90318
_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 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.804