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_4343981
_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 H50.16 Cl2 N6 O14.58 V2'
_chemical_formula_weight         925.07
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   24.9994(5)
_cell_length_b                   24.9994(5)
_cell_length_c                   17.3225(4)
_cell_measurement_reflns_used    12836
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.8065
_cell_measurement_theta_min      3.0058
_cell_volume                     9375.6(3)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'KM4 XCALIBUR2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0977
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61155
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.866
_diffrn_reflns_theta_min         3.012
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             4326
_exptl_crystal_size_max          0.4278
_exptl_crystal_size_mid          0.2083
_exptl_crystal_size_min          0.0992
_refine_diff_density_max         1.693
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         8389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1131P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4294
_reflns_number_total             8389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00571_si_005.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4343981--4343988.cif.'
_cod_original_cell_volume        9375.6(4)
_cod_database_code               4343981
_shelxl_version_number           2014-3
_shelx_res_checksum              12602
_shelx_hkl_checksum              58983