Wide band gap thiophosphates ASrPS4 (A=Li, Na, K, Rb, Cs): cation size effect induced successive structure transformation
Huang, Yi; Huang, Junben; Zhang, Yong; Dalton Transactions  (2022) –; doi:10.1039/D2DT02321K

data_7711161
_publ_section_title
;
 Wide band gap thiophosphates ASrPS4 (A=Li, Na, K, Rb, Cs): cation size
 effect induced successive structure transformation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02321K
_journal_year                    2022
_chemical_formula_moiety         'C64 H54 N4 P2 Ru2 S4'
_chemical_formula_sum            'C64 H54 N4 P2 Ru2 S4'
_chemical_formula_weight         1271.43
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-08 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   34.2817(3)
_cell_length_b                   34.2817(3)
_cell_length_c                   13.16739(12)
_cell_measurement_reflns_used    27427
_cell_measurement_temperature    94(2)
_cell_measurement_theta_max      70.2350
_cell_measurement_theta_min      2.6490
_cell_volume                     13401.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      94(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            42303
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.731
_diffrn_reflns_theta_min         3.672
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.254
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015).
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model. Empirical absorption correction using
spherical harmonics, frame scaling and detector area scaling,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       plate
_exptl_crystal_F_000             5832
_exptl_crystal_recrystallization_method
'diffusing hexane vapor into a toluene solution'
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         5382
_refine_ls_number_restraints     673
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+19.8873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1336
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4783
_reflns_number_total             5382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02321k2.cif
_cod_data_source_block           jk418_sq
_cod_original_cell_volume        13401.6(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7711161
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.406
_shelx_estimated_absorpt_t_max   0.907
_shelx_res_checksum              23881
_shelx_hkl_checksum              18874
_shelx_fab_checksum              93538