Oxidovanadium Catechol Complexes: Radical versus Non-Radical States and Redox Series
Suman Kundu; Suvendu Maity; Thomas Weyhermüller; Prasanta Ghosh; Inorganic Chemistry 52 (2013) 7417–7430; doi:10.1021/ic400166z

data_4335329
_publ_section_title
;
 Oxidovanadium Catechol Complexes: Radical versus Non-Radical States and
 Redox Series
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7417
_journal_page_last               7430
_journal_paper_doi               10.1021/ic400166z
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'dichloromethane, pentane'
_chemical_formula_moiety         'C26 H30 N3 O4 V'
_chemical_formula_sum            'C26 H30 N3 O4 V'
_chemical_formula_weight         499.47
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                WGT-PG-500-10
_audit_creation_date             2011-02-18
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.545(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9332(8)
_cell_length_b                   9.8988(5)
_cell_length_c                   18.1730(6)
_cell_measurement_reflns_used    76065
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0996
_cell_measurement_theta_min      2.6966
_cell_volume                     2490.1(2)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69606
_diffrn_reflns_theta_full        33.16
_diffrn_reflns_theta_max         33.16
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.94061
_exptl_absorpt_correction_T_min  0.91270
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         9492
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+1.6444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                7940
_reflns_number_total             9492
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400166z_si_003_2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4335329