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_7711163
_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         'C18 H18 N4 Ru S2, C7 H8'
_chemical_formula_sum            'C25 H26 N4 Ru S2'
_chemical_formula_weight         547.69
_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   mixed
_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                 104.0386(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.10525(5)
_cell_length_b                   15.03284(6)
_cell_length_c                   23.47074(8)
_cell_measurement_reflns_used    88748
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      79.5880
_cell_measurement_theta_min      3.2220
_cell_volume                     4828.14(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      98(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            108602
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.100
_diffrn_reflns_theta_min         3.230
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.025
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.500
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018).
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    1.507
_exptl_crystal_description       plate
_exptl_crystal_F_000             2240
_exptl_crystal_recrystallization_method
'by cooling a saturated toluene solution at -20 \%C'
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     766
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+3.8819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9076
_reflns_number_total             9360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02321k2.cif
_cod_data_source_block           jk675
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7711163
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.446
_shelx_estimated_absorpt_t_max   0.844
_shelx_res_checksum              52712
_shelx_hkl_checksum              30299