Quaternary alkaline-earth metal thiophosphate SrAgPS4: syntheses, structure, and optical properties
Xing, Wenhao; Tang, Jian; Liang, Fei; Tang, Chunlan; Wu, Jieyun; Yin, Wenlong; Bin, Kang; Deng, Jianguo; Dalton Transactions  (2023) –; doi:10.1039/D3DT00793F

data_7712866
_publ_section_title
;
 Quaternary alkaline-earth metal thiophosphate SrAgPS4: syntheses,
 structure, and optical properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00793F
_journal_year                    2023
_chemical_formula_moiety         '0.25(Ag4 P4 S16 Sr4)'
_chemical_formula_sum            'Ag P S4 Sr'
_chemical_formula_weight         354.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           40
_space_group_name_Hall           'A 2 -2a'
_space_group_name_H-M_alt        'A m a 2'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-02-07 deposited with the CCDC.	2023-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0941(3)
_cell_length_b                   10.0305(2)
_cell_length_c                   6.4002(2)
_cell_measurement_reflns_used    1788
_cell_measurement_temperature    295.66(10)
_cell_measurement_theta_max      73.2550
_cell_measurement_theta_min      8.2080
_cell_volume                     648.01(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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      295.66(10)
_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 0.979
_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     44.00  70.00   0.50    0.07    --   47.84-125.00-180.00   52
  2  \w     79.00 112.00   0.50    0.29    --  109.10-125.00 150.00   66
  3  \w     97.00 122.00   0.50    0.29    --  109.10 125.00 -60.00   50
  4  \w    153.00 178.00   0.50    0.29    --  109.10 125.00 -60.00   50
  5  \w     97.00 161.00   0.50    0.29    --  109.10 125.00-180.00  128
  6  \w     77.00 110.00   0.50    0.29    --  109.10-125.00 -60.00   66
  7  \w     45.00 104.00   0.50    0.29    --  109.10 -99.00 -60.00  118
  8  \w     42.00 100.00   0.50    0.29    --  109.10-125.00  30.00  116
  9  \w     63.00 107.00   0.50    0.29    --  109.10-125.00 120.00   88
 10  \w     37.00  74.00   0.50    0.29    --  109.10-125.00 150.00   74
 11  \w     72.00 105.00   0.50    0.29    --  109.10 -77.00 150.00   66
 12  \w     38.00  64.00   0.50    0.29    --  109.10 -57.00   0.00   52
 13  \w    -10.00  17.00   0.50    0.07    --   47.84 -19.00 -60.00   54
 14  \w    -20.00  11.00   0.50    0.07    --  -47.84  19.00-150.00   62
 15  \w     -5.00  21.00   0.50    0.07    --  -47.84   0.00-180.00   52
 16  \w    -26.00  26.00   0.50    0.07    --  -47.84  19.00 150.00  104
 17  \w   -117.00 -39.00   0.50    0.07    --  -47.84   0.00-180.00  156
 18  \w    -57.00 -25.00   0.50    0.29    --  -91.75  57.00-150.00   64
 19  \w    -53.00 -28.00   0.50    0.29    --  -91.75  57.00-120.00   50
 20  \w    -73.00 -21.00   0.50    0.29    --  -91.75 125.00 -90.00  104
 21  \w    -84.00 -48.00   0.50    0.29    --  -91.75 125.00 120.00   72
 22  \w   -157.00 -79.00   0.50    0.29    --  -91.75 -19.00-120.00  156
 23  \w   -163.00-110.00   0.50    0.29    --  -91.75 -77.00-120.00  106
 24  \w   -100.00 -69.00   0.50    0.29    --  -91.75 -77.00-120.00   62
 25  \w   -116.00 -90.00   0.50    0.29    --  -91.75 -77.00   0.00   52
 26  \w   -161.00-119.00   0.50    0.29    --  -91.75 -77.00   0.00   84
 27  \w   -109.00 -73.00   0.50    0.29    --  -91.75-125.00 150.00   72
 28  \w   -157.00-131.00   0.50    0.29    --  -91.75-125.00 150.00   52
;
_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      -0.0157286000
_diffrn_orient_matrix_UB_12      0.0387774000
_diffrn_orient_matrix_UB_13      -0.1473285000
_diffrn_orient_matrix_UB_21      -0.2253041000
_diffrn_orient_matrix_UB_22      0.0491451000
_diffrn_orient_matrix_UB_23      0.0224306000
_diffrn_orient_matrix_UB_31      0.0832571000
_diffrn_orient_matrix_UB_32      0.1402687000
_diffrn_orient_matrix_UB_33      0.0328347000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2530
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.965
_diffrn_reflns_theta_min         8.215
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    48.431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light white'
_exptl_crystal_density_diffrn    3.636
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.332
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 272 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(18)
_refine_ls_extinction_coef       0.00123(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         660
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.4240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    0.932
_reflns_Friedel_fraction_max     0.879
_reflns_number_gt                651
_reflns_number_total             660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00793f2.cif
_cod_data_source_block           SrAgPS4
_cod_database_code               7712866
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         AgSrPS
_chemical_oxdiff_usercomment     RT
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Ag1A) \\sim Ueq, Uanis(Ag1B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
2. Others
 Sof(Ag1B)=0.5*(1-FVAR(2))
 Sof(Ag1A)=0.5*FVAR(2)
;
_shelx_res_checksum              66970
_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 1.424
_oxdiff_exptl_absorpt_empirical_full_min 0.793