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_7711160
_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         'C32 H28 Cl N2 P Ru S2, 1.5(C6 H6)'
_chemical_formula_sum            'C41 H37 Cl N2 P Ru S2'
_chemical_formula_weight         789.33
_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_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                 95.1615(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.28954(11)
_cell_length_b                   8.79277(9)
_cell_length_c                   30.6796(3)
_cell_measurement_reflns_used    18740
_cell_measurement_temperature    94(2)
_cell_measurement_theta_max      74.4160
_cell_measurement_theta_min      3.5400
_cell_volume                     3570.43(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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      94(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            31467
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.123
_diffrn_reflns_theta_min         3.518
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.007
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (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    1.468
_exptl_crystal_description       prism
_exptl_crystal_F_000             1620
_exptl_crystal_recrystallization_method
'vapor diffusion of pentane into a benzene solution'
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6974
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0370P)^2^+4.4546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6254
_reflns_number_total             6974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02321k2.cif
_cod_data_source_block           jk934
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7711160
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.523
_shelx_estimated_absorpt_t_max   0.836
_shelx_res_checksum              44121
_shelx_hkl_checksum              74525