o-Iminobenzosemiquinonate and o-Imino-p-methylbenzosemiquinonate Anion Radicals Coupled VO2+ Stabilization
Amit Saha Roy; Pinaki Saha; Nirmal Das Adhikary; Prasanta Ghosh; Inorganic Chemistry 50 (2011) 2488–2500; doi:10.1021/ic102296p

data_4324659
_publ_section_title
;
 o-Iminobenzosemiquinonate and o-Imino-p-methylbenzosemiquinonate Anion
 Radicals Coupled VO2+ Stabilization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2488
_journal_page_last               2500
_journal_paper_doi               10.1021/ic102296p
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C25.5 H24 N3 O4.5 V'
_chemical_formula_weight         495.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.9010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.05980(10)
_cell_length_b                   15.1237(3)
_cell_length_c                   19.2297(3)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.82
_cell_measurement_theta_min      2.53
_cell_volume                     2343.70(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMAINT'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16907
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 - Bruker AXS'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       'opaque rectangle'
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+2.5900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                3751
_reflns_number_total             4076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102296p_si_001_1.cif
_cod_data_source_block           RKM-VO(1.3/2MeOH)
_cod_original_formula_sum        'C25.50 H24 N3 O4.50 V'
_cod_database_code               4324659