Molecular and Electronic Structure of Octahedral o-Aminophenolato and o-Iminobenzosemiquinonato Complexes of V(V), Cr(III), Fe(III), and Co(III). Experimental Determination of Oxidation Levels of Ligands and Metal Ions
Hyungphil Chun; Claudio Nazari Verani; Phalguni Chaudhuri; Eberhard Bothe; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 40 (2001) 4157–4166; doi:10.1021/ic010106a

data_4320061
_publ_section_title
;
 Molecular and Electronic Structure of Octahedral o-Aminophenolato and
 o-Iminobenzosemiquinonato Complexes of V(V), Cr(III), Fe(III), and
 Co(III). Experimental Determination of Oxidation Levels of Ligands and
 Metal Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4157
_journal_page_last               4166
_journal_paper_doi               10.1021/ic010106a
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C60 H76 N3 O3 V'
_chemical_formula_weight         938.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                93.41(2)
_cell_angle_beta                 97.10(2)
_cell_angle_gamma                112.67(2)
_cell_formula_units_Z            4
_cell_length_a                   15.165(2)
_cell_length_b                   18.128(2)
_cell_length_c                   21.961(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    100(2)
_cell_volume                     5490.2(15)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens ShelXTL'
_computing_publication_material  'Siemens ShelXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w-scan, 0.3 deg./frame'
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43486
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   'SADABS, G.M. Sheldrick 1994'
_exptl_crystal_colour            'dark purple red'
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.004
_refine_ls_goodness_of_fit_obs   1.138
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1283
_refine_ls_number_reflns         18727
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.018
_refine_ls_restrained_S_obs      1.152
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_obs          0.0517
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1356
_refine_ls_wR_factor_obs         0.1180
_reflns_number_observed          11630
_reflns_number_total             18784
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010106a_4.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5490.2(12)
_cod_database_code               4320061