Synthesis and Characterization of V(IV)O Complexes of Picolinate and Pyrazine Derivatives. Behavior in the Solid State and Aqueous Solution and Biotransformation in the Presence of Blood Plasma Proteins.
Koleša-Dobravc, Tanja; Lodyga-Chruscinska, Elzbieta; Symonowicz, Marzena; Sanna, Daniele; Meden, Anton; Perdih, Franc; Garribba, Eugenio; Inorganic chemistry 53 (2014) 7960–; doi:10.1021/ic500766t

data_4340458
_publ_section_title
;
 Synthesis and Characterization of V(IV)O Complexes of Picolinate and
 Pyrazine Derivatives. Behavior in the Solid State and Aqueous Solution
 and Biotransformation in the Presence of Blood Plasma Proteins.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7960
_journal_paper_doi               10.1021/ic500766t
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C10 H8 N4 O6 V'
_chemical_formula_sum            'C10 H8 N4 O6 V'
_chemical_formula_weight         331.14
_chemical_name_systematic
;
\D-aqua-bis(pyrazine-2-carboxylato-N,O)-oxidovanadium(IV)
;
_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                 105.377(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.96600(10)
_cell_length_b                   13.0237(2)
_cell_length_c                   8.51240(10)
_cell_measurement_reflns_used    5253
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.6030
_cell_measurement_theta_min      5.3630
_cell_volume                     637.731(17)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics
'ORTEP-3 for Windows version 2.02 (Farrugia, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4933
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5923
_diffrn_reflns_theta_full        74.80
_diffrn_reflns_theta_max         74.80
_diffrn_reflns_theta_min         5.39
_exptl_absorpt_coefficient_mu    6.874
_exptl_absorpt_correction_T_max  0.8203
_exptl_absorpt_correction_T_min  0.2783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2011)'
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             334
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_coef       0.0230(13)
_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   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2608
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0569P)^2^+0.0232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                2591
_reflns_number_total             2608
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic500766t_si_002.cif
_cod_data_source_block           5-delta
_cod_depositor_comments
'Adding full bibliography for 4340454--4340458.cif.'
_cod_original_cell_volume        637.731(16)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4340458