The synthesis and structure-property relation analysis of metal chalcohalide crystals Cs2InPS4X2 (X = Cl, Br) with mixed anions
Tang, Chunlan; Xing, Wen-Hao; Wang, Naizheng; Tang, Jian; Lin, Zheshuai; Wu, Jieyun; Yin, Wenlong; Bin, Kang; Dalton Transactions  (2022) –; doi:10.1039/D2DT00078D

data_7709599
_publ_section_title
;
 The synthesis and structure-property relation analysis of metal
 chalcohalide crystals Cs2InPS4X2 (X = Cl, Br) with mixed anions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00078D
_journal_year                    2022
_chemical_formula_moiety         'Br2 Cs2 In P S4'
_chemical_formula_sum            'Br2 Cs2 In P S4'
_chemical_formula_weight         699.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.011(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8353(4)
_cell_length_b                   7.9969(3)
_cell_length_c                   16.4742(6)
_cell_measurement_reflns_used    8614
_cell_measurement_temperature    296.67(10)
_cell_measurement_theta_max      32.0980
_cell_measurement_theta_min      3.2580
_cell_volume                     1286.04(9)
_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      296.67(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.875
_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     -5.00  79.00   0.50    5.50    --    9.62  77.00   0.00  168
  2  \w      1.00  80.00   0.50    5.50    --    9.62  57.00 -90.00  158
  3  \w    -20.00  25.00   0.50    5.50    --   -8.52 -99.00 -60.00   90
  4  \w    -26.00  -1.00   0.50    5.50    --   -8.52 -99.00 120.00   50
  5  \w    -25.00  20.00   0.50    5.50    --    9.62 -99.00 150.00   90
  6  \w    -58.00  21.00   0.50    5.50    --    9.62 -37.00  60.00  158
  7  \w     12.00  43.00   0.50    5.50    --    9.62 -99.00-150.00   62
  8  \w    -25.00  39.00   0.50    5.50    --    9.62 -99.00-180.00  128
;
_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      0.0553166000
_diffrn_orient_matrix_UB_12      0.0571789000
_diffrn_orient_matrix_UB_13      0.0010180000
_diffrn_orient_matrix_UB_21      -0.0065203000
_diffrn_orient_matrix_UB_22      -0.0002600000
_diffrn_orient_matrix_UB_23      -0.0433555000
_diffrn_orient_matrix_UB_31      -0.0466675000
_diffrn_orient_matrix_UB_32      0.0677990000
_diffrn_orient_matrix_UB_33      -0.0009675000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19817
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.433
_diffrn_reflns_theta_min         3.293
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75655
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.614
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.477
_refine_diff_density_min         -1.493
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.00059(6)
_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   1.070
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         4051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0165P)^2^+1.0071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2928
_reflns_number_total             4051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00078d1.cif
_cod_data_source_block           Cs2Br2InPS4
_cod_database_code               7709599
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         InPSCsBr
_chemical_oxdiff_usercomment     'hemisphere  0.75  0.5  5.5s  RT'
_shelx_estimated_absorpt_t_max   0.433
_shelx_estimated_absorpt_t_min   0.278
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
;
_shelx_res_checksum              45434
_shelx_hkl_checksum              12143
_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 1.200
_oxdiff_exptl_absorpt_empirical_full_min 0.805