Encapsulation of Anion/Cation in the Central Cavity of Tetrameric Polyoxometalate, Composed of Four Trititanium(IV)-Substituted α-Dawson Subunits, Initiated by Protonation/Deprotonation of the Bridging Oxygen Atoms on the Intramolecular Surface
Yoshitaka Sakai; Shuji Ohta; Yukihiro Shintoyo; Shoko Yoshida; Yuhki Taguchi; Yusuke Matsuki; Satoshi Matsunaga; Kenji Nomiya; Inorganic Chemistry 50 (2011) 6575–6583; doi:10.1021/ic200355e

data_4325588
_publ_contact_author_email       nomiya@kanagawa-u.ac.jp
_publ_contact_author_fax         +81-463-58-9684
_publ_contact_author_name        'Kenji Nomiya'
_publ_contact_author_phone       +81-463-58-4111
_publ_section_title
;
 Encapsulation of Anion/Cation in the Central Cavity of Tetrameric
 Polyoxometalate, Composed of Four Trititanium(IV)-Substituted \a-Dawson
 Subunits, Initiated by Protonation/Deprotonation of the Bridging Oxygen
 Atoms on the Intramolecular Surface
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6575
_journal_page_last               6583
_journal_paper_doi               10.1021/ic200355e
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'H292 N28 Na8 O332 P8 Ti12 W60'
_chemical_formula_weight         18036.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.228(5)
_cell_angle_beta                 88.604(5)
_cell_angle_gamma                87.418(5)
_cell_formula_units_Z            4
_cell_length_a                   24.906(7)
_cell_length_b                   38.261(11)
_cell_length_c                   38.991(11)
_cell_measurement_reflns_used    7806
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.56
_cell_measurement_theta_min      2.18
_cell_volume                     36459(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0856
_diffrn_reflns_av_sigmaI/netI    0.1454
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            353990
_diffrn_reflns_theta_full        28.48
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    19.243
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.286
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             32224
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         11.683
_refine_diff_density_min         -5.826
_refine_diff_density_rms         0.622
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     6355
_refine_ls_number_reflns         167191
_refine_ls_number_restraints     22344
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1564
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.478
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+1352.3999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.2240
_reflns_number_gt                93212
_reflns_number_total             167191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200355e_si_002.cif
_cod_data_source_block           so01-2s
_cod_original_cell_volume        36460(18)
_cod_database_code               4325588