Metal-substituted tungstosulfates with Keggin structure: synthesis and characterization.
Azuma, Shinya; Kadoguchi, Taiga; Eguchi, Yohei; Hirabaru, Hikaru; Ota, Hiromi; Sadakane, Masahiro; Yanagisawa, Kazumichi; Hasegawa, Takuya; Ueda, Tadaharu; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2766–2770; doi:10.1039/c9dt04737a

data_7703428
_publ_section_title
;
 Metal-substituted tungstosulfates with Keggin structure: synthesis and
 characterization.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2766
_journal_page_last               2770
_journal_paper_doi               10.1039/c9dt04737a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'O39 S W11'
_chemical_formula_sum            'O39 S W11'
_chemical_formula_weight         2678.39
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-11-27 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   17.565(10)
_cell_length_b                   17.565(10)
_cell_length_c                   17.565(10)
_cell_measurement_reflns_used    6466
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.20
_cell_measurement_theta_min      2.30
_cell_volume                     5419(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_molecular_graphics    'CrystalStructure 4.2.4'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 28.626
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0931
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42711
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         3.281
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.690
_exptl_absorpt_correction_T_max  0.311
_exptl_absorpt_correction_T_min  0.203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2284.00
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.64
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_number_parameters     19
_refine_ls_number_reflns         649
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0931
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0631P)^2^+120.4308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2188
_refine_ls_wR_factor_ref         0.2189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                645
_reflns_number_total             649
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9dt04737a2.cif
_cod_data_source_block           257_0119p
_cod_depositor_comments
'Adding full bibliography for 7703428--7703432.cif.'
_cod_database_code               7703428
_shelx_res_checksum              18786
_shelx_fab_checksum              11656