Vanadium(V) Tartrato Complexes: Speciation in the H3O+(OH-)/H2VO4-/(2R,3R)-Tartrate System and X-ray Crystal Structures of Na4[V4O8(rac-tart)2].12H2O and (NEt4)4[V4O8((R,R)-tart)2].6H2O (tart = C4H2O64-)
Peter Schwendt; Alan S. Tracey; Jozef Tatiersky; Jana Gáliková; Zdirad Žák; Inorganic Chemistry 46 (2007) 3971–3983; doi:10.1021/ic062223h

data_4307722
_publ_section_title
;
Vanadium(V) Tartrato Complexes: Speciation in the
H3O+(OH-)/H2VO4-/(2R,3R)-Tartrate System and X-ray Crystal Structures of
Na4[V4O8(rac-tart)2].12H2O and (NEt4)4[V4O8((R,R)-tart)2].6H2O (tart =
C4H2O64-)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3971
_journal_page_last               3983
_journal_paper_doi               10.1021/ic062223h
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C40 H96 N4 O26 V4'
_chemical_formula_weight         1252.97
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 108.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.225(2)
_cell_length_b                   14.029(3)
_cell_length_c                   18.298(4)
_cell_measurement_reflns_used    5726
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.5
_cell_measurement_theta_min      2.3
_cell_volume                     2971.6(12)
_computing_cell_refinement       'KUMA Crysalis 168'
_computing_data_collection       'KUMA Crysalis 168'
_computing_data_reduction        'KUMA Crysalis 168'
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '0.06 mm'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'KUMA KM-4 CCD'
_diffrn_measurement_method       'omega scan'
_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  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35252
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'each 100 frames'
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.9036
_exptl_absorpt_correction_T_min  0.7700
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.201
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         9531
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                7008
_reflns_number_total             9531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062223hsi20061122_084420.cif
_cod_data_source_block           lvina
_cod_original_cell_volume        2971.6(10)
_cod_database_code               4307722