Experimental and theoretical study of crystal structure and bandgap of CdBi2S4
Matyszczak, Grzegorz; Sutuła, Szymon; Krawczyk, Krzysztof; Woźniak, Krzysztof; Journal of Solid State Chemistry 305 (2022) 122695–; doi:10.1016/j.jssc.2021.122695

data_1566060
_publ_section_title
;
 Experimental and theoretical study of crystal structure and bandgap of
 CdBi2S4
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              122695
_journal_paper_doi               10.1016/j.jssc.2021.122695
_journal_volume                  305
_journal_year                    2022
_chemical_formula_moiety         '0.25(Bi8.09 Cd3.91 S16)'
_chemical_formula_sum            'Bi2.02 Cd0.98 S4'
_chemical_formula_weight         660.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 116.2782(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.12051(19)
_cell_length_b                   3.98623(4)
_cell_length_c                   14.6231(2)
_cell_measurement_reflns_used    8622
_cell_measurement_temperature    296.2(5)
_cell_measurement_theta_max      35.6200
_cell_measurement_theta_min      3.0950
_cell_volume                     685.769(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43d (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.2(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0026
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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    -32.00   0.00   1.00   10.00    --  -30.00 -77.00 -30.00   32
  2  \w     10.00  58.00   1.00   10.00    --   34.79 -37.00-180.00   48
  3  \w     22.00 111.00   1.00   10.00    --   34.79-160.00 -90.00   89
  4  \w      5.00 104.00   1.00   10.00    --   34.79  77.00  90.00   99
  5  \w     22.00  78.00   1.00   20.00    --   34.79-160.00-150.00   56
  6  \w    -17.00  68.00   1.00   20.00    --   34.79 -99.00 -30.00   85
  7  \w     15.00 101.00   1.00   20.00    --   34.79  57.00 -30.00   86
  8  \w      5.00  46.00   1.00   20.00    --   34.79  77.00 -90.00   41
  9  \w     80.00 105.00   1.00   20.00    --   34.79  77.00 -90.00   25
 10  \w      9.00 104.00   1.00   20.00    --   34.79  37.00  60.00   95
 11  \w    -30.00  64.00   1.00   20.00    --   34.79 -77.00  30.00   94
 12  \w     44.00 104.00   1.00   20.00    --   34.79   0.00 -60.00   60
 13  \w      5.00  89.00   1.00   20.00    --   34.79  77.00-180.00   84
 14  \w    -36.00 -10.00   1.00   20.00    --   34.79   0.00 -60.00   26
 15  \w    -32.00   0.00   1.00   20.00    --  -30.00 -77.00 -30.00   32
 16  \w      5.00 104.00   1.00   20.00    --   34.79  77.00  90.00   99
 17  \w     22.00 111.00   1.00   20.00    --   34.79-160.00 -90.00   89
 18  \w     10.00  58.00   1.00   20.00    --   34.79 -37.00-180.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0190656000
_diffrn_orient_matrix_UB_12      -0.0091965000
_diffrn_orient_matrix_UB_13      -0.0535239000
_diffrn_orient_matrix_UB_21      0.0069363000
_diffrn_orient_matrix_UB_22      0.1759766000
_diffrn_orient_matrix_UB_23      -0.0017225000
_diffrn_orient_matrix_UB_31      0.0567721000
_diffrn_orient_matrix_UB_32      -0.0245927000
_diffrn_orient_matrix_UB_33      0.0076571000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12342
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.969
_diffrn_reflns_theta_min         3.105
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    55.865
_exptl_absorpt_correction_T_max  0.110
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43d (Rigaku Oxford Diffraction, 2018)
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            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    6.400
_exptl_crystal_description       block
_exptl_crystal_F_000             1115
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.077
_refine_diff_density_max         4.030
_refine_diff_density_min         -3.852
_refine_diff_density_rms         0.597
_refine_ls_extinction_coef       0.0166(4)
_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   1.165
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         1678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0435P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1626
_reflns_number_total             1678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2022-305-122695.cif
_cod_data_source_block           57p600_red1_abs1
_cod_original_cell_volume        685.770(19)
_cod_database_code               1566060
_chemical_oxdiff_formula         Bi2CdS4
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     34.26
_olex2_refinement_description
;
1. Shared sites
{CdM2, BiM2}
{BiM1, CdM1}
2. Uiso/Uaniso restraints and constraints
Uanis(CdM2) = Uanis(BiM2)
Uanis(BiM1) = Uanis(CdM1)
3. Others
 Sof(CdM2)=0.25*(1-FVAR(2))
 Sof(BiM2)=0.25*FVAR(2)
 Sof(CdM1)=0.5*(1-FVAR(3))
 Sof(BiM1)=0.5*FVAR(3)
;
_shelx_res_checksum              54920
_shelx_hkl_checksum              33134
_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 1.610
_oxdiff_exptl_absorpt_empirical_full_min 0.672