Protonation and Methylation of an Anderson-Type Polyoxoanion [IMo6O24]5-
Daisuke Honda; Shusaku Ikegami; Tomoaki Inoue; Tomoji Ozeki; Atsushi Yagasaki; Inorganic Chemistry 46 (2007) 1464–1470; doi:10.1021/ic061881z

data_4307368
_publ_contact_author_address
;Department of Chemistry
Kwansei Gakuin University
Sanda 669-1337
Japan
;
_publ_contact_author_email       yagasaki@kwansei.ac.jp
_publ_contact_author_fax         +81-79-565-9077
_publ_contact_author_name        'Atsushi Yagasaki'
_publ_contact_author_phone       +81-79-565-8396
_publ_section_title
;
Protonation and Methylation of an Anderson-Type Polyoxoanion [IMo6O24]5-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1464
_journal_page_last               1470
_journal_paper_doi               10.1021/ic061881z
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
'(C16 H36 N +)4, (I Mo6 O24 C H3 4-), 3(H2 O)'
_chemical_formula_sum            'C65 H153 I Mo6 N4 O27'
_chemical_formula_weight         2125.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   17.0679(4)
_cell_length_b                   25.6998(6)
_cell_length_c                   20.7428(4)
_cell_measurement_reflns_used    37479
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      1.86
_cell_volume                     9098.7(3)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       CrystalClear
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury CCD diffractometer'
_diffrn_measurement_method       'oscillation method, \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku UltraX18 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            88967
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  0.9183
_exptl_absorpt_correction_T_min  0.8282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.805
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         13831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+4.0953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                9369
_reflns_number_total             13831
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic061881zsi20060929_095237_5.cif
_cod_data_source_block           imo6o23_ome
_cod_database_code               4307368