Heterolytic Dissociation of Water Demonstrated by Crystal-to-Crystal Core Interconversion from (μ-Oxo)divanadium to Bis(μ-hydroxo)divanadium Substituted Polyoxometalates
Kazuhiro Uehara; Noritaka Mizuno; Journal of the American Chemical Society 133 (2011) 1622–1625; doi:10.1021/ja108245g

data_4105616
_publ_contact_author_address
;
Department of Applied Chemistry, School of Engineering,
The University of Tokyo
7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656, Japan
;
_publ_contact_author_email       tmizuno@mail.ecc.u-tokyo.ac.jp
_publ_contact_author_fax         +81-3-5841-7220
_publ_contact_author_name        'Noritaka Mizuno'
_publ_contact_author_phone       +81-3-5841-7272
_publ_section_title
;
 Heterolytic Dissociation of Water Demonstrated by Crystal-to-Crystal Core
 Interconversion from (\m-Oxo)divanadium to Bis(\m-hydroxo)divanadium
 Substituted Polyoxometalates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1622
_journal_page_last               1625
_journal_paper_doi               10.1021/ja108245g
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C68 Cl4 N4 O39 Si V2 W10'
_chemical_formula_sum            'C68 Cl4 N4 O39 Si V2 W10'
_chemical_formula_weight         3606.99
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_audit_creation_date             2010-03-24T21:05:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.65670(10)
_cell_length_b                   35.65670(10)
_cell_length_c                   16.98670(10)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     21596.89(15)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      153
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30832
_diffrn_reflns_theta_full        29.58
_diffrn_reflns_theta_max         29.58
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    10.948
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.219
_exptl_crystal_description       prism
_exptl_crystal_F_000             12928
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.669
_refine_diff_density_min         -2.46
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.508(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         29921
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_gt           0.052
_refine_ls_shift/su_max          0.923
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+346.4947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                26946
_reflns_number_total             29921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108245g_si_002_2.cif
_cod_data_source_block           compound_1
_cod_database_code               4105616