Molecular and Electronic Structures of Bis-(o-diiminobenzosemiquinonato)metal(II) Complexes (Ni, Pd, Pt), Their Monocations and -Anions, and of Dimeric Dications Containing Weak Metal-Metal Bonds
Diran Herebian; Eberhard Bothe; Frank Neese; Thomas Weyhermüller; Karl Wieghardt; Journal of the American Chemical Society 125 (2003) 9116–9128; doi:10.1021/ja030123u

data_4113979
_publ_section_title
;
 Molecular and Electronic Structures of
 Bis-(o-diiminobenzosemiquinonato)metal(II) Complexes (Ni, Pd, Pt), Their
 Monocations and -Anions, and of Dimeric Dications Containing Weak
 Metal-Metal Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9116
_journal_page_last               9128
_journal_paper_doi               10.1021/ja030123u
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C24 H20 N4 Ni'
_chemical_formula_weight         423.15
_chemical_name_systematic
; 
 ? 
;
_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                74.30(1)
_cell_angle_beta                 75.88(1)
_cell_angle_gamma                62.74(1)
_cell_formula_units_Z            2
_cell_length_a                   9.6222(6)
_cell_length_b                   10.2880(6)
_cell_length_c                   11.5222(8)
_cell_measurement_reflns_used    11780
_cell_measurement_temperature    100(2)
_cell_volume                     966.46(14)
_computing_cell_refinement       'DENZO, Nonius Collect Software'
_computing_data_collection       'DENZO, Nonius Collect Software'
_computing_data_reduction        'DENZO, Nonius Collect Software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa-CCD, rotating anode'
_diffrn_measurement_method       '397 images at 1 deg. in \w and 30 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating Mo-anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11780
_diffrn_reflns_theta_max         33.31
_diffrn_reflns_theta_min         4.72
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  0.9301
_exptl_absorpt_correction_T_min  0.7949
_exptl_absorpt_correction_type   'gaussian, face-indexed'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.079
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         7316
_refine_ls_number_restraints     1
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_refine_ls_restrained_S_obs      1.079
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_obs          0.0401
_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^)+(0.0000P)^2^+0.3198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0987
_refine_ls_wR_factor_obs         0.0858
_reflns_number_observed          5626
_reflns_number_total             7342
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja030123u_2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.3198P] 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^)+(0.0000P)^2^+0.3198P] 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        966.47(11)
_cod_database_code               4113979