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_4307721
_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            'C8 H28 Na4 O32 V4'
_chemical_formula_weight         932.02
_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                88.76(3)
_cell_angle_beta                 78.53(3)
_cell_angle_gamma                62.85(3)
_cell_formula_units_Z            2
_cell_length_a                   10.627(2)
_cell_length_b                   11.392(2)
_cell_length_c                   14.167(3)
_cell_measurement_temperature    120(2)
_cell_volume                     1490.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0142
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9382
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    1.397
_exptl_absorpt_correction_T_max  0.8178
_exptl_absorpt_correction_T_min  0.6406
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0019(3)
_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   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         5084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+0.6724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                4732
_reflns_number_total             5084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062223hsi20061122_084359.cif
_cod_data_source_block           dlvina
_cod_original_cell_volume        1490.9(5)
_cod_database_code               4307721