Molecular and Electronic Structures of Tetrahedral Complexes of Nickel and Cobalt ContainingN,N‘-Disubstituted, Bulkyo-Diiminobenzosemiquinonate(1−) π-Radical Ligands
Chłopek, Krzysztof; Bothe, Eberhard; Neese, Frank; Weyhermüller, Thomas; Wieghardt, Karl; Inorganic Chemistry 45 (2006) 6298–6307; doi:10.1021/ic060242l

data_4332322
_publ_section_title
;
 Molecular and Electronic Structures of Tetrahedral Complexes of Nickel
 and Cobalt ContainingN,N&#x2018;-Disubstituted,
 Bulkyo-Diiminobenzosemiquinonate(1&#x2212;) \p-Radical Ligands
;
_journal_issue                   16
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6298
_journal_page_last               6307
_journal_paper_doi               10.1021/ic060242l
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         '[C68 H92 N4 Ni], MeCN'
_chemical_formula_sum            'C70 H95 N5 Ni'
_chemical_formula_weight         1065.22
_chemical_name_systematic
; 
 ? 
;
_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                 109.59(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.3092(8)
_cell_length_b                   15.1637(5)
_cell_length_c                   18.5850(6)
_cell_measurement_temperature    100(2)
_cell_volume                     6454.2(5)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method
'1026 images at 1.0 deg. in \w, 50 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1131
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            113899
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         11290
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+9.8895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                9222
_reflns_number_total             11290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060242lsup1.cif
_cod_data_source_block           1*MeCN
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+9.8895P] 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^)+(0.0266P)^2^+9.8895P] 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        6454.2(4)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4332322