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_7711158
_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         'C16 H19 Cl N2 O Ru S3'
_chemical_formula_sum            'C16 H19 Cl N2 O Ru S3'
_chemical_formula_weight         488.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 91.3511(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5064(3)
_cell_length_b                   14.3080(3)
_cell_length_c                   9.18732(16)
_cell_measurement_reflns_used    6792
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      69.8780
_cell_measurement_theta_min      5.7150
_cell_volume                     1774.95(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      95(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_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  0.0612
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14005
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         4.503
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    11.888
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.229
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020).
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            orange
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_recrystallization_method
'vapor diffusion of pentane into a benzene solution'
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.022
_refine_diff_density_max         2.569
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3205
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0761
_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^)+(0.1319P)^2^+6.9512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2110
_refine_ls_wR_factor_ref         0.2177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2771
_reflns_number_total             3205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02321k2.cif
_cod_data_source_block           jk948
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7711158
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.190
_shelx_estimated_absorpt_t_max   0.780
_shelx_res_checksum              31444
_shelx_hkl_checksum              46923