Crystal Structures and Solution Properties of Discrete Complexes Composed of Saddle-Distorted Molybdenum(V)-Dodecaphenylporphyrins and Keggin-Type Heteropolyoxometalates Linked by Direct Coordination
Atsutoshi Yokoyama; Takahiko Kojima; Kei Ohkubo; Shunichi Fukuzumi; Inorganic Chemistry 49 (2010) 11190–11198; doi:10.1021/ic1019586

data_4317248
_publ_section_title
;
 Crystal Structures and Solution Properties of Discrete Complexes Composed
 of Saddle-Distorted Molybdenum(V)-Dodecaphenylporphyrins and Keggin-Type
 Heteropolyoxometalates Linked by Direct Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11190
_journal_page_last               11198
_journal_paper_doi               10.1021/ic1019586
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C184 H122 Mo2 N8 O42 Si W12 '
_chemical_formula_sum            'C184 H122 Mo2 N8 O42 Si W12'
_chemical_formula_weight         5543.18
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 118.897(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   18.4212(11)
_cell_length_b                   37.5328(17)
_cell_length_c                   17.8126(11)
_cell_measurement_reflns_used    8621
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      5.2
_cell_volume                     10782.2(11)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2002
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33298
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_exptl_absorpt_coefficient_mu    6.559
_exptl_absorpt_correction_T_max  0.374
_exptl_absorpt_correction_T_min  0.181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5208.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.34
_refine_diff_density_min         -3.75
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     560
_refine_ls_number_reflns         9879
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0416P)^2^+392.6626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1817
_reflns_number_gt                8264
_reflns_number_total             9879
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic1019586_si_002.cif
_cod_data_source_block           '__sc0080'
_cod_original_cell_volume        10782.2(10)
_cod_original_formula_sum        'C184 H122 Mo2 N8 O42 Si W12 '
_cod_database_code               4317248