Preparation of Preyssler-type Phosphotungstate with One Central Potassium Cation and Potassium Cation Migration into the Preyssler Molecule to form Di-Potassium-Encapsulated Derivative.
Hayashi, Akio; Wihadi, Muh Nur Khoiru; Ota, Hiromi; López, Xavier; Ichihashi, Katsuya; Nishihara, Sadafumi; Inoue, Katsuya; Tsunoji, Nao; Sano, Tsuneji; Sadakane, Masahiro; ACS omega 3 (2018) 2363–2373; doi:10.1021/acsomega.8b00163

data_4516013
_publ_section_title
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 Preparation of Preyssler-type Phosphotungstate with One Central Potassium
 Cation and Potassium Cation Migration into the Preyssler Molecule to form
 Di-Potassium-Encapsulated Derivative.
;
_journal_issue                   2
_journal_name_full               'ACS omega'
_journal_page_first              2363
_journal_page_last               2373
_journal_paper_doi               10.1021/acsomega.8b00163
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'O110 P5 W30, 40.66(H2O), K12.87'
_chemical_formula_sum            'H81.32 K12.87 O150.66 P5 W30'
_chemical_formula_weight         8666
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.6621(15)
_cell_length_b                   21.5252(10)
_cell_length_c                   19.0566(9)
_cell_measurement_reflns_used    9101
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.15
_cell_volume                     13397.9(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.0(3)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0196
_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
_diffrn_reflns_number            150063
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.220
_exptl_absorpt_correction_T_max  0.2282
_exptl_absorpt_correction_T_min  0.1791
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             14955
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.884
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         15370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+147.3121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0522
_reflns_number_gt                12790
_reflns_number_total             15370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ao8b00163_si_002.cif
_cod_data_source_block           KPOM
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_diffrn_ambient_temperature' value '173(0.3)' was changed
to '173.0(3)' -- precision was estimated.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_database_code               4516013
_shelx_f_squared_multiplier      1.000