Valence Delocalization in a Mixed-Oxidation Divanadium (IV, V) Complex Electrogenerated from Its Structurally Characterized Divanadium (V) Analogue with a Tridentate (ONO) Ligand
Rupam Dinda; Parbati Sengupta; Saktiprosad Ghosh; Thomas C. W. Mak; Inorganic Chemistry 41 (2002) 1684–1688; doi:10.1021/ic010865t

data_4317699
_publ_section_title
;
 Valence Delocalization in a Mixed-Oxidation Divanadium (IV, V) Complex
 Electrogenerated from Its Structurally Characterized Divanadium (V)
 Analogue with a Tridentate (ONO) Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1684
_journal_page_last               1688
_journal_paper_doi               10.1021/ic010865t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C30 H26 N6 O7 V2'
_chemical_formula_weight         684.45
_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                 96.145(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9240(18)
_cell_length_b                   16.211(4)
_cell_length_c                   23.381(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2986.2(12)
_computing_cell_refinement       'Bruker SMART CCD Diffractometer'
_computing_data_collection       'Bruker SMART CCD Diffractometer'
_computing_data_reduction        'Bruker SMART CCD Diffractometer'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD Diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20687
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7621
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Dark blue'
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.93
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          3.069
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+1.7533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                4880
_reflns_number_total             7242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010865t.cif
_cod_data_source_block           r06
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2986.1(12)
_cod_database_code               4317699