Flux Crystal Growth, Crystal Structure, and Magnetic Properties of a Ternary Chromium Disulfide Ba<sub>9</sub>Cr<sub>4</sub>S<sub>19</sub> with Unusual Cr<sub>4</sub>S<sub>15</sub> Tetramer Units.
Yan, Hong; Matsushita, Yoshitaka; Chikamatsu, Akira; Hasegawa, Tetsuya; Yamaura, Kazunari; Tsujimoto, Yoshihiro; ACS omega 6 (2021) 6842–6847; doi:10.1021/acsomega.0c06017

data_4518540
_publ_section_title
;
 Flux Crystal Growth, Crystal Structure, and Magnetic Properties of a
 Ternary Chromium Disulfide Ba<sub>9</sub>Cr<sub>4</sub>S<sub>19</sub>
 with Unusual Cr<sub>4</sub>S<sub>15</sub> Tetramer Units.
;
_journal_issue                   10
_journal_name_full               'ACS omega'
_journal_page_first              6842
_journal_page_last               6847
_journal_paper_doi               10.1021/acsomega.0c06017
_journal_volume                  6
_journal_year                    2021
_chemical_formula_moiety         'Ba9 Cr4 S19'
_chemical_formula_sum            'Ba9 Cr4 S19'
_chemical_formula_weight         2053.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-03
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.041(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7695(3)
_cell_length_b                   11.3269(2)
_cell_length_c                   23.2057(6)
_cell_measurement_reflns_used    5581
_cell_measurement_temperature    297
_cell_measurement_theta_max      30.3610
_cell_measurement_theta_min      2.4070
_cell_volume                     3256.16(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      297
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     85.00 110.00   0.50   60.00    --   20.00  54.00 -60.00   50
  2  \w    -61.00   4.00   0.50   60.00    --   20.00  54.00  30.00  130
  3  \w      7.00  33.00   0.50   60.00    --   20.00  54.00  30.00   52
  4  \w     72.00 105.00   0.50   60.00    --   20.00  54.00  30.00   66
  5  \w    -66.00 103.00   0.50   60.00    --   20.00  54.00 150.00  338
  6  \w    -26.00  88.00   0.50   60.00    --   20.00  54.00  90.00  228
  7  \w     10.00  35.00   0.50   60.00    --   20.00  54.00 -90.00   50
  8  \w     84.00 109.00   0.50   60.00    --   20.00  54.00 -90.00   50
  9  \w     39.00  64.00   0.50   60.00    --   20.00  54.00 -60.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0335696000
_diffrn_orient_matrix_UB_12      0.0466443000
_diffrn_orient_matrix_UB_13      0.0142175000
_diffrn_orient_matrix_UB_21      -0.0053203000
_diffrn_orient_matrix_UB_22      -0.0206257000
_diffrn_orient_matrix_UB_23      0.0279934000
_diffrn_orient_matrix_UB_31      0.0461272000
_diffrn_orient_matrix_UB_32      -0.0363136000
_diffrn_orient_matrix_UB_33      0.0023683000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11692
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.436
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    4.188
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.056
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.284
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0114P)^2^+10.6867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2837
_reflns_number_total             3326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c06017_si_002.cif
_cod_data_source_block           exp_64
_cod_depositor_comments          'Adding full bibliography for 4518540.cif.'
_cod_database_code               4518540
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.526
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Sof: S10(0.5) S11(0.5)
;
_shelx_res_checksum              60070
_shelx_hkl_checksum              98250
_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 1.344
_oxdiff_exptl_absorpt_empirical_full_min 0.825