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_4325676
_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         'C72 H120 Mo12 N18 O40 Si'
_chemical_formula_sum            'C72 H120 Mo12 N18 O40 Si'
_chemical_formula_weight         3057.20
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      161
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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            6
_cell_length_a                   28.649(3)
_cell_length_b                   28.649(3)
_cell_length_c                   20.480(3)
_cell_measurement_reflns_used    93108
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.08
_cell_measurement_theta_min      3.13
_cell_volume                     14557(3)
_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)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.001
_diffrn_measured_fraction_theta_max 1.001
_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  0.0379
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            75943
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.599
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_description       platelet
_exptl_crystal_F_000             9096.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.620
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3582 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.33(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7294
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0383P)^2^+73.3877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                6716
_reflns_number_total             7294
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic200683e_si_002_1.cif
_cod_data_source_block           TA
_cod_original_sg_symbol_H-M      'R 3 c:H'
_cod_database_code               4325676