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_4304192
_publ_section_title
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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            'H74 Mo18 N12 O86 Sb6'
_chemical_formula_weight         4076.1
_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                69.542(2)
_cell_angle_beta                 82.375(2)
_cell_angle_gamma                69.846(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8137(6)
_cell_length_b                   17.8810(7)
_cell_length_c                   19.7340(8)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     4286.9(3)
_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 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46766
_diffrn_reflns_theta_full        28.72
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    4.516
_exptl_absorpt_correction_T_max  0.582
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Bruker,1996)
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3816
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.634
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         21475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1825
_reflns_number_gt                13612
_reflns_number_total             21475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7016648-file001.cif
_cod_data_source_block           xb0379m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4304192