An Unusual Asymmetric Polyoxomolybdate Containing Mixed-Valence Antimony and Its Derivatives: [Sb4VSb2IIIMo18O73(H2O)2]12- and {M(H2O)2[Sb4VSb2IIIMo18O73(H2O)2]2}22- (M = MnII, FeII, CuII or CoII)
Ganglin Xue; Xuemei Liu; Haisheng Xu; Huaiming Hu; Feng Fu; Jiwu Wang; Inorganic Chemistry 47 (2008) 2011–2016; doi:10.1021/ic7016648

data_4304193
_publ_section_title
;
An Unusual Asymmetric Polyoxomolybdate Containing Mixed-Valence Antimony
and Its Derivatives: [Sb4VSb2IIIMo18O73(H2O)2]12- and
{M(H2O)2[Sb4VSb2IIIMo18O73(H2O)2]2}22- (M = MnII, FeII, CuII or CoII)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2011
_journal_page_last               2016
_journal_paper_doi               10.1021/ic7016648
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'H140 Mn Mo36 N22 O172 Sb12'
_chemical_formula_weight         8171.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.8010(10)
_cell_angle_beta                 82.7290(10)
_cell_angle_gamma                69.3450(10)
_cell_formula_units_Z            1
_cell_length_a                   13.8612(9)
_cell_length_b                   17.9531(12)
_cell_length_c                   19.8574(14)
_cell_measurement_temperature    293(2)
_cell_volume                     4339.5(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22183
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    4.672
_exptl_absorpt_correction_T_max  0.496
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadbas
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    3.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3909
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.954
_refine_diff_density_min         -3.638
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         15213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+54.0595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                12693
_reflns_number_total             15213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7016648-file002.cif
_cod_data_source_block           liu1
_cod_database_code               4304193