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_4349221
_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         'K11 O128 P5 W30'
_chemical_formula_sum            'K11 O128 P5 W30'
_chemical_formula_weight         8148.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
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_cell_length_b                   21.455(4)
_cell_length_c                   19.126(4)
_cell_measurement_reflns_used    20876
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
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_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
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_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1291
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
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_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         3.041
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.023
_exptl_absorpt_correction_T_max  0.353
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             14112.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         4.75
_refine_diff_density_min         -4.15
_refine_ls_extinction_method     none
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_refine_ls_number_parameters     461
_refine_ls_number_reflns         15430
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0522P)^2^+2525.7449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                14102
_reflns_number_total             15430
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
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