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_7029533
_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         'C48 H108 N3 O41 S V W11'
_chemical_formula_sum            'C48 H108 N3 O41 S V W11'
_chemical_formula_weight         3488.72
_chemical_name_common            SVW11final
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.283(3)
_cell_angle_beta                 92.990(2)
_cell_angle_gamma                90.924(3)
_cell_formula_units_Z            2
_cell_length_a                   13.6813(6)
_cell_length_b                   15.4018(7)
_cell_length_c                   19.2335(9)
_cell_measurement_reflns_used    62323
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      1.06
_cell_volume                     4029.2(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0549
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62323
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    15.851
_exptl_absorpt_correction_T_max  0.2324
_exptl_absorpt_correction_T_min  0.0651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3196
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         6.621
_refine_diff_density_min         -1.944
_refine_diff_density_rms         0.419
_refine_ls_extinction_coef       0.00130(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         14173
_refine_ls_number_restraints     2017
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+99.3615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.2058
_reflns_number_gt                9561
_reflns_number_total             14173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53161a3.cif
_cod_data_source_block           c:\users\lu\desktop\startp~1\lupom4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7029533