Synthesis, molecular structure and properties of oxo-vanadium(iv) complexes containing the oxydiacetate ligand
del Río, Diego; Galindo, Agustín; Vicente, Ramón; Mealli, Carlo; Ienco, Andrea; Masi, Dante; Dalton Transactions  (2003) 1813–; doi:10.1039/b300914a

data_7012758
_publ_section_title
;
 Synthesis, molecular structure and properties of oxo-vanadium(iv)
 complexes containing the oxydiacetate ligand
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1813
_journal_paper_doi               10.1039/b300914a
_journal_year                    2003
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C10 H14 O14 V2, 2(H2O), 2Na'
_chemical_formula_sum            'C10 H18 Na2 O16 V2'
_chemical_formula_weight         546.14
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      36
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2002-10-22T15:26:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.884(5)
_cell_length_b                   6.860(5)
_cell_length_c                   18.394(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      9
_cell_measurement_wavelength     0.71073
_cell_volume                     2004.3(17)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.02409
_diffrn_orient_matrix_UB_12      0.050505
_diffrn_orient_matrix_UB_13      -0.031326
_diffrn_orient_matrix_UB_21      -0.084167
_diffrn_orient_matrix_UB_22      -0.024797
_diffrn_orient_matrix_UB_23      -0.038874
_diffrn_orient_matrix_UB_31      -0.116625
_diffrn_orient_matrix_UB_32      0.028291
_diffrn_orient_matrix_UB_33      0.021528
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1053
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  0.8987
_exptl_absorpt_correction_T_min  0.7861
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   1
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1053
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.067
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1707
_reflns_number_gt                898
_reflns_number_total             1053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300914a.txt
_cod_data_source_block           die88
_cod_database_code               7012758
_exptl_absorpt_factor_mur        0.105
_exptl_absorpt_correction_t_ave  0.8661
_diffrn_standards_decay_corr_max 1.017
_diffrn_standards_decay_corr_min 0.994