Structurally characterised vanadium(v)-substituted Keggin-type heteropolysulfates [SVM11O40](3-) (M = Mo, W): voltammetric and spectroscopic studies related to the V(v)/V(iv) redox couple.
Ueda, Tadaharu; Nambu, Jun-Ichi; Lu, Jinzhen; Guo, Si-Xuan; Li, Qi; Boas, John F.; Martin, Lisandra L.; Bond, Alan M.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5462–5473; doi:10.1039/c3dt53161a

data_7029532
_publ_section_title
;
 Structurally characterised vanadium(v)-substituted Keggin-type
 heteropolysulfates [SVM11O40](3-) (M = Mo, W): voltammetric and
 spectroscopic studies related to the V(v)/V(iv) redox couple.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5462
_journal_page_last               5473
_journal_paper_doi               10.1039/c3dt53161a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C96 H216 Mo22 N6 O81.50 S2 V2'
_chemical_formula_sum            'C96 H216 Mo22 N6 O81.5 S2 V2'
_chemical_formula_weight         5035.43
_chemical_name_common            'SVMo final'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.793(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   49.3884(12)
_cell_length_b                   14.0771(4)
_cell_length_c                   26.1812(7)
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      1.92
_cell_volume                     16524.6(9)
_computing_cell_refinement       'Bruker Apex2 v2.0'
_computing_data_collection       'Bruker Apex2 v2.0'
_computing_data_reduction        'Bruker Apex2 v2.0'
_computing_molecular_graphics    x-seed
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX CCD'
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38646
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.827
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'red orange'
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9952
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.34
_refine_diff_density_max         2.057
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         14525
_refine_ls_number_restraints     1903
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+655.6444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.1861
_reflns_number_gt                12449
_reflns_number_total             14525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53161a3.cif
_cod_data_source_block           pom3
_cod_original_cell_volume        16524.6(8)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C96 H216 Mo22 N6 O81.50 S2 V2'
_cod_database_code               7029532