[Tris(o-iminosemiquinone)cobalt(III)]—a radical complex with an St = 3/2 ground state
Verani, Cláudio Nazari; Gallert, Stefan; Bill, Eckhard; Weyhermüller, Thomas; Wieghardt, Karl; Chaudhuri, Phalguni; Chemical Communications  (1999) 1747–; doi:10.1039/a903778k

data_7115245
_publ_section_title
;
 [Tris(o-iminosemiquinone)cobalt(III)]---a radical complex with an St =
 3/2 ground state
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1747
_journal_paper_doi               10.1039/a903778k
_journal_year                    1999
_chemical_formula_sum            'C60 H75 Co N3 O3'
_chemical_formula_weight         945.16
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 103.62(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0426(12)
_cell_length_b                   13.9533(9)
_cell_length_c                   27.594(2)
_cell_measurement_reflns_used    7842
_cell_measurement_temperature    100(2)
_cell_volume                     5628.9(9)
_computing_cell_refinement       'Siemens SAINT 5.0'
_computing_data_collection       'Siemens SAINT 5.0'
_computing_data_reduction        'Siemens SAINT 5.0'
_computing_molecular_graphics    'Siemens ShelXTL 5'
_computing_publication_material  'Siemens ShelXTL 5'
_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, 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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            53106
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.9423
_exptl_absorpt_correction_T_min  0.7483
_exptl_absorpt_correction_type   'SADABS, G.M. Sheldrick, 1994'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.59
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         16074
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.086
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_refine_ls_R_factor_obs          0.0415
_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^)+(0.0538P)^2^+1.2480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1063
_refine_ls_wR_factor_obs         0.0971
_reflns_number_observed          12104
_reflns_number_total             16129
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903778k.txt
_cod_data_source_block           1,CoL3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+1.2480P] 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^)+(0.0538P)^2^+1.2480P] 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        5629.0(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7115245