Synthesis of polyoxothiometalates through site-selective post-editing sulfurization of polyoxometalates.
Yonesato, Kentaro; Yamaguchi, Kazuya; Suzuki, Kosuke; Chemical science 15 (2024) 11267–11271; doi:10.1039/d4sc02912g

data_1571894
_publ_section_title
;
 Synthesis of polyoxothiometalates through site-selective post-editing
 sulfurization of polyoxometalates.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              11267
_journal_page_last               11271
_journal_paper_doi               10.1039/d4sc02912g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C98 H83 N O28 P4 S12 Si W12'
_chemical_formula_weight         4465.54
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-12-28 deposited with the CCDC.	2024-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                67.9371(13)
_cell_angle_beta                 68.7098(13)
_cell_angle_gamma                89.8358(11)
_cell_formula_units_Z            1
_cell_length_a                   13.6691(2)
_cell_length_b                   14.5906(2)
_cell_length_c                   17.0239(2)
_cell_measurement_reflns_used    58251
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.7680
_cell_measurement_theta_min      0.8100
_cell_volume                     2896.62(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023) (IMPORT)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'PILATUS3 X CdTe 1M'
_diffrn_measurement_device_type  'Four-circle diffractmeter'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  Si(311)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41420
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0232
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55158
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        14.390
_diffrn_reflns_theta_max         15.003
_diffrn_reflns_theta_min         0.817
_diffrn_source                   'SPring-8, BL02B1'
_exptl_absorpt_coefficient_mu    2.977
_exptl_crystal_colour            'Light yellow'
_exptl_crystal_density_diffrn    2.560
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.796
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.234(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1903
_refine_ls_number_reflns         23134
_refine_ls_number_restraints     303
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+1.8248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    0.958
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                22987
_reflns_number_total             23134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02912g2.cif
_cod_data_source_block           II_Si
_cod_depositor_comments          'Adding full bibliography for 1571894.cif.'
_cod_database_code               1571894
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.819
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              87094
_shelx_hkl_checksum              41169