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_4310251
_publ_contact_author_address
;
Department of Chemistry
Kwansei Gakuin University
2-1 Gakuen, Sanda 669-1337
Japan
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_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_sum            'C50 H114 I Mo6 N3 O24'
_chemical_formula_weight         1843.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.324(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4009(1)
_cell_length_b                   14.6658(3)
_cell_length_c                   23.5395(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.24
_cell_volume                     3532.52(10)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\w scans with 0.3 \% steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57128
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.541
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'xprep (Bruker, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.208
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         10755
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s2^(Fo2^)+(0.0000P)2^+12.4727P] where P=(Fo2^+2Fc2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                9714
_reflns_number_total             10755
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic051351nsi20050808_023541_2.cif
_cod_data_source_block           IMo6O22(OMe)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3532.5(1)
_cod_database_code               4310251