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_4320058
_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 H75 Cr N3 O3'
_chemical_formula_weight         938.23
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9544(8)
_cell_length_b                   17.7004(12)
_cell_length_c                   23.295(2)
_cell_measurement_reflns_used    11350
_cell_measurement_temperature    100(2)
_cell_volume                     5341.5(7)
_computing_cell_refinement       'Nonius Collect'
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'Nonius Collect'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '285 frames a 1 deg. in \w and 90 sec.'
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28246
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   'MulScanAbs, Platon99 program suite'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         15071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_obs          0.0472
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+1.3122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1136
_refine_ls_wR_factor_obs         0.1035
_reflns_number_observed          12787
_reflns_number_total             15102
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010106a_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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^)+(0.0423P)^2^+1.3122P] 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^)+(0.0423P)^2^+1.3122P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320058