Aerial Oxidation of a V(IV)-Iminopyridine Hydroquinonate Complex: A Trap for the V(IV)-Semiquinonate Radical Intermediate.
Stylianou, Marios; Drouza, Chryssoula; Giapintzakis, John; Athanasopoulos, Georgios I.; Keramidas, Anastasios D.; Inorganic chemistry 54 (2015) 7218–7229; doi:10.1021/acs.inorgchem.5b00571

data_4343982
_publ_section_title
;
 Aerial Oxidation of a V(IV)-Iminopyridine Hydroquinonate Complex: A Trap
 for the V(IV)-Semiquinonate Radical Intermediate.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7218
_journal_page_last               7229
_journal_paper_doi               10.1021/acs.inorgchem.5b00571
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C32 H30 N6 O6 V2'
_chemical_formula_weight         696.50
_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                97.637(10)
_cell_angle_beta                 101.977(11)
_cell_angle_gamma                102.252(11)
_cell_formula_units_Z            1
_cell_length_a                   6.5655(9)
_cell_length_b                   10.0810(13)
_cell_length_c                   11.7778(14)
_cell_measurement_temperature    100
_cell_volume                     732.32(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.697
_diffrn_measurement_device_type  'KM4 XCALIBUR2'
_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  0.0671
_diffrn_reflns_av_sigmaI/netI    0.0945
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9306
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.75
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.1524
_exptl_crystal_size_mid          0.1044
_exptl_crystal_size_min          0.0642
_refine_diff_density_max         1.202
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1257P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.2325
_reflns_number_gt                2757
_reflns_number_total             4414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00571_si_008.cif
_cod_data_source_block           V4
_cod_depositor_comments
'Adding full bibliography for 4343981--4343988.cif.'
_cod_original_cell_volume        732.32(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4343982