Tetrahedral Connection of ε-Keggin-type Polyoxometalates To Form an All-Inorganic Octahedral Molecular Sieve with an Intrinsic 3D Pore System.
Zhang, Zhenxin; Sadakane, Masahiro; Murayama, Toru; Izumi, Shoko; Yasuda, Nobuhiro; Sakaguchi, Norihito; Ueda, Wataru; Inorganic chemistry 53 (2014) 903–911; doi:10.1021/ic4022849

data_4337117
_publ_section_title
;
 Tetrahedral Connection of \e-Keggin-type Polyoxometalates To Form an
 All-Inorganic Octahedral Molecular Sieve with an Intrinsic 3D Pore
 System.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              903
_journal_page_last               911
_journal_paper_doi               10.1021/ic4022849
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'Bi2 Mo9.40 O40 V3.60, K1.70, 5.03(H2 O)'
_chemical_formula_sum            'Bi2 H10.07 K1.7 Mo9.4 O45.03 V3.6'
_chemical_formula_weight         2300.21
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           227
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_atom_sites_solution_hydrogens   geom
_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            8
_cell_length_a                   19.6850(6)
_cell_length_b                   19.6850(6)
_cell_length_c                   19.6850(6)
_cell_measurement_reflns_used    10887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.71
_cell_measurement_theta_min      2.1
_cell_volume                     7627.9(4)
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 29
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_radiation_source         'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.83112
_diffrn_reflns_av_R_equivalents  0.1418
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10887
_diffrn_reflns_theta_full        31.71
_diffrn_reflns_theta_max         31.71
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    14.838
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.006
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8369
_exptl_crystal_size_max          0.004
_exptl_crystal_size_mid          0.003
_exptl_crystal_size_min          0.003
_refine_diff_density_max         1.272
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         430
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0646
_reflns_number_gt                291
_reflns_number_total             430
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic4022849_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Cubic' changed to 'cubic' according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_original_formula_sum        'Bi2 H10.07 K1.70 Mo9.40 O45.03 V3.60'
_cod_database_code               4337117