Synthesis and Structure of an Air-Stable, Free-Radical Cobalt(III) Semiquinone Complex
Steven Arzberger; Jake Soper; Oren P. Anderson; Agnete la Cour; Mark Wicholas; Inorganic Chemistry 38 (1999) 757–761; doi:10.1021/ic981052g

data_4321792
_publ_section_title
;
 Synthesis and Structure of an Air-Stable, Free-Radical Cobalt(III)
 Semiquinone Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              757
_journal_page_last               761
_journal_paper_doi               10.1021/ic981052g
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C50.25 H93.5 Cl0.5 Co N6 O2.5'
_chemical_formula_weight         898.47
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.4330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.5207(3)
_cell_length_b                   18.4345(3)
_cell_length_c                   22.1614(3)
_cell_measurement_reflns_used    15764
_cell_measurement_temperature    162(2)
_cell_measurement_theta_max      23.36
_cell_measurement_theta_min      0.76
_cell_volume                     10979.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      162(2)
_diffrn_measurement_device       'Bruker SMART-CCD Area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1221
_diffrn_reflns_av_sigmaI/netI    0.1563
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49604
_diffrn_reflns_theta_max         23.36
_diffrn_reflns_theta_min         0.76
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_description       plate
_exptl_crystal_F_000             3940
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.00008(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_all   1.003
_refine_ls_goodness_of_fit_obs   1.174
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1115
_refine_ls_number_reflns         15764
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.003
_refine_ls_restrained_S_obs      1.174
_refine_ls_R_factor_all          0.1663
_refine_ls_R_factor_obs          0.0980
_refine_ls_shift/esd_max         2.032
_refine_ls_shift/esd_mean        0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1653P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2902
_refine_ls_wR_factor_obs         0.2491
_reflns_number_observed          8668
_reflns_number_total             15764
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981052g.cif
_cod_data_source_block           mwsad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1653P)^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^)+(0.1653P)^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_formula_sum        'C50.25 H93.50 Cl0.50 Co N6 O2.50'
_cod_database_code               4321792