Methoxide of an Anderson-Type Polyoxometalate and Its Conversion to a New Type of Species, [IMo9O32(OH)(OH2)3]4-
Daisuke Honda; Tomoji Ozeki; Atsushi Yagasaki; Inorganic Chemistry 44 (2005) 9616–9618; doi:10.1021/ic051351n

data_4310250
_publ_contact_author_address
;
Department of Chemistry
Kwansei Gakuin University
2-1 Gakuen, Sanda 669-1337
Japan
;
_publ_contact_author_email       yagasaki@kwansei.ac.jp
_publ_contact_author_fax         81(79)5659077
_publ_contact_author_name        'Dr. Atsushi Yagasaki'
_publ_contact_author_phone       81(79)5658396
_publ_section_title
;
Methoxide of an Anderson-Type Polyoxometalate and Its Conversion to a New
Type of Species, [IMo9O32(OH)(OH2)3]4-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9616
_journal_page_last               9618
_journal_paper_doi               10.1021/ic051351n
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '(C16 H36 N +)4, (H7 I Mo9 O36 4-), H2O'
_chemical_formula_sum            'C64 H153 I Mo9 N4 O37'
_chemical_formula_weight         2560.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   24.549(1)
_cell_length_b                   17.979(1)
_cell_length_c                   22.860(1)
_cell_measurement_reflns_used    51461
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      11.82
_cell_measurement_theta_min      0.87
_cell_volume                     10089.6(8)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'DIP Xpress (MAC Science, 1999)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'MAC Science DIP LABO'
_diffrn_measurement_method       'oscillation method, \w scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_source         'SPring-8 BL04B2 bending magnet beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3282
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            100778
_diffrn_reflns_theta_full        11.82
_diffrn_reflns_theta_max         11.82
_diffrn_reflns_theta_min         0.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.6221
_exptl_absorpt_correction_T_min  0.5723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PLATON MULABS (Spek, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5164
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.235
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.204
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.366(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         18130
_refine_ls_number_restraints     1359
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0641
_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/[\s2^(Fo2^)+(0.1092P)2^+73.7319P] where P=(Fo2^+2Fc2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1763
_reflns_number_gt                17360
_reflns_number_total             18130
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic051351nsi20050808_023541_1.cif
_cod_data_source_block           H7IMo9O36
_cod_database_code               4310250