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_4307364
_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 +)3, (I Mo6 O24 H2 3-), 2(C3 H7 N O)'
_chemical_formula_sum            'C54 H124 I Mo6 N5 O26'
_chemical_formula_weight         1962.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_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                 91.475(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6105(4)
_cell_length_b                   15.5432(5)
_cell_length_c                   29.3316(9)
_cell_measurement_reflns_used    24808
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      0.69
_cell_volume                     8026.1(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku Mercury-7 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  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67267
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         0.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.8778
_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    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.507
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         20886
_refine_ls_number_restraints     665
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0588
_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/[\s^2^(Fo^2^)+(0.0938P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1842
_reflns_number_gt                12616
_reflns_number_total             20886
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic061881zsi20060929_095237_1.cif
_cod_data_source_block           imo6o22_oh_2
_cod_database_code               4307364