An unprecedented vanadoniobate cluster with 'trans-vanadium' bicapped Keggin-type {VNb12O40(VO)2}
Guiling Guo; Yanqing Xu; Jie Cao; Changwen Hu; Chem.Commun. 47 (2011) 9411–; doi:10.1039/c1cc12329g

data_7106756
_publ_section_title
;
 An unprecedented vanadoniobate cluster with 'trans-vanadium' bicapped
 Keggin-type {VNb12O40(VO)2}
;
_journal_name_full               Chem.Commun.
_journal_page_first              9411
_journal_paper_doi               10.1039/c1cc12329g
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C22 H124 Cu5.5 N22 Nb12 O60 V3'
_chemical_formula_weight         3274.64
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 103.0880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.6242(17)
_cell_length_b                   14.3236(9)
_cell_length_c                   25.0786(16)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.45
_cell_volume                     8965.5(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44647
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         0.82
_exptl_absorpt_coefficient_mu    3.148
_exptl_absorpt_correction_T_max  0.5577
_exptl_absorpt_correction_T_min  0.3970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SMART'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    2.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             6442
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.824
_refine_diff_density_min         -2.209
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1147
_refine_ls_number_reflns         16490
_refine_ls_number_restraints     2960
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+80.5795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                14990
_reflns_number_total             16490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12329g.txt
_cod_data_source_block           e
_cod_original_sg_symbol_H-M      P2/c
_cod_original_formula_sum        'C22 H124 Cu5.50 N22 Nb12 O60 V3'
_cod_database_code               7106756