A highly reduced vanadium(III/IV) polyoxovanadate comprising an octavanadyl square-prism surrounding a dimetallic vanadium(III) fragment.
Laye, Rebecca H; Wei, Qiang; Mason, Pamela V; Shanmugam, Maheswaran; Teat, Simon J; Brechin, Euan K; Collison, David; McInnes, Eric J L; Journal of the American Chemical Society 128 (2006) 9020–9021; doi:10.1021/ja062723+

data_4101335
_publ_section_title
;
 A highly reduced vanadium(III/IV) polyoxovanadate comprising an
 octavanadyl square-prism surrounding a dimetallic vanadium(III)
 fragment.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9020
_journal_page_last               9021
_journal_paper_doi               10.1021/ja062723+
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C74 H98 N24 O22 V10'
_chemical_formula_weight         2185.16
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.4950(18)
_cell_length_b                   17.4950(18)
_cell_length_c                   18.5306(19)
_cell_measurement_reflns_used    5444
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      3.06
_cell_volume                     5671.8(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6778
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_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            31855
_diffrn_reflns_theta_full        28.95
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2359
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0783
_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^)+(0.1695P)^2^+5.9130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2658
_refine_ls_wR_factor_ref         0.2826
_reflns_number_gt                1936
_reflns_number_total             2359
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja062723+si20060419_071032.cif
_cod_data_source_block           rl355a
_cod_original_sg_symbol_H-M      I4/mmm
_cod_database_code               4101335