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_7012757
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H24 N4 O12 V2, 2(H2 O)'
_chemical_formula_sum            'C14 H14 N2 O7 V'
_chemical_formula_weight         373.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2002-10-22T16:47:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.00
_cell_angle_beta                 114.010(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.995(5)
_cell_length_b                   10.784(5)
_cell_length_c                   19.143(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     3016.3(19)
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4321
_diffrn_reflns_theta_full        22.98
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.9523
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Linear fit to sin(theta)/lambda - 12 parameters
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         4180
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.097
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+12.5431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                2749
_reflns_number_total             4180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300914a.txt
_cod_data_source_block           die44
_cod_database_code               7012757
_exptl_absorpt_factor_mur        4.895
_exptl_absorpt_correction_t_ave  0.5275