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_4304194
_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            'Fe H140 Mo36 N22 O172 Sb12'
_chemical_formula_weight         8171.96
_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                69.633(3)
_cell_angle_beta                 82.564(3)
_cell_angle_gamma                69.733(2)
_cell_formula_units_Z            1
_cell_length_a                   13.834(3)
_cell_length_b                   17.908(3)
_cell_length_c                   19.789(4)
_cell_measurement_temperature    273(2)
_cell_volume                     4311.3(15)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22711
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    4.570
_exptl_absorpt_correction_T_max  0.401
_exptl_absorpt_correction_T_min  0.250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Bruker,1996)
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3819
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.036
_refine_diff_density_min         -3.862
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         15761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0877P)^2^+37.4817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1660
_reflns_number_gt                12550
_reflns_number_total             15761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7016648-file003.cif
_cod_data_source_block           0043
_cod_original_cell_volume        4311.4(15)
_cod_database_code               4304194