Encapsulation of Two Potassium Cations in Preyssler-Type Phosphotungstates: Preparation, Structural Characterization, Thermal Stability, Activity as an Acid Catalyst, and HAADF-STEM Images.
Hayashi, Akio; Ota, Hiromi; López, Xavier; Hiyoshi, Norihito; Tsunoji, Nao; Sano, Tsuneji; Sadakane, Masahiro; Inorganic chemistry 55 (2016) 11583–11592; doi:10.1021/acs.inorgchem.6b02116

data_4349222
_publ_section_title
;
 Encapsulation of Two Potassium Cations in Preyssler-Type
 Phosphotungstates: Preparation, Structural Characterization, Thermal
 Stability, Activity as an Acid Catalyst, and HAADF-STEM Images.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11583
_journal_page_last               11592
_journal_paper_doi               10.1021/acs.inorgchem.6b02116
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C40 H120 K2 O130 P5 S20 W30'
_chemical_formula_sum            'C40 H120 K2 O130 P5 S20 W30'
_chemical_formula_weight         9071.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.470(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   22.601(9)
_cell_length_b                   30.731(13)
_cell_length_c                   28.208(12)
_cell_measurement_reflns_used    22046
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     19532(14)
_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'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2013/4 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            105306
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.021
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.992
_exptl_absorpt_correction_T_max  0.237
_exptl_absorpt_correction_T_min  0.147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.084
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             16212.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         3.72
_refine_diff_density_min         -6.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         22342
_refine_ls_number_restraints     1411
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0399P)^2^+359.8053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19956
_reflns_number_total             22342
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
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_cod_data_source_block           249_1220a
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_shelx_res_checksum              21088
_shelx_hkl_checksum              68305
_shelx_fab_checksum              72761