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_4335330
_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        'dichlormethane, methanole'
_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           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                WGT-PG-500-09
_audit_creation_date             2011-02-18
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   38.113(4)
_cell_length_b                   38.113(4)
_cell_length_c                   10.0207(11)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0984
_cell_measurement_theta_min      2.6071
_cell_volume                     12606(2)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0150
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            152632
_diffrn_reflns_theta_full        33.26
_diffrn_reflns_theta_max         33.26
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  0.94734
_exptl_absorpt_correction_T_min  0.89848
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       prism
_exptl_crystal_F_000             4716
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         10780
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0499P)^2^+10.3455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                9287
_reflns_number_total             10780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400166z_si_003_3.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4335330