Hydrogen-Bonded Assemblies of Two-Electron Reduced Mixed-Valence [XMo12O40] (X = P and Si) withp-Phenylenediamines
Tomoyuki Akutagawa; Fumito Kudo; Ryo Tsunashima; Shin-ichiro Noro; Leroy Cronin; Takayoshi Nakamura; Inorganic Chemistry 50 (2011) 6711–6718; doi:10.1021/ic200683e

data_4325677
_publ_section_title
;
 Hydrogen-Bonded Assemblies of Two-Electron Reduced Mixed-Valence
 [XMo12O40] (X = P and Si) withp-Phenylenediamines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6711
_journal_page_last               6718
_journal_paper_doi               10.1021/ic200683e
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C30 H47 Mo12 N12 O40 P'
_chemical_formula_sum            'C30 H47 Mo12 N12 O40 P'
_chemical_formula_weight         2398.01
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_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            3
_cell_length_a                   23.214(4)
_cell_length_b                   23.214(4)
_cell_length_c                   10.184(3)
_cell_measurement_reflns_used    18008
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.04
_cell_volume                     4752.8(18)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
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_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
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_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
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_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.415
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_description       block
_exptl_crystal_F_000             3450.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.270
_refine_diff_density_min         -1.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1750
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    7170.7500    10014.9000    3085.0300
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                1243
_reflns_number_total             2410
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic200683e_si_002_2.cif
_cod_data_source_block           TAkuta
_cod_original_cell_volume        4752.7(18)
_cod_original_sg_symbol_H-M      'R -3:H'
_cod_database_code               4325677