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_4113980
_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 Pd'
_chemical_formula_weight         470.84
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_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                73.74(1)
_cell_angle_beta                 75.84(1)
_cell_angle_gamma                63.36(1)
_cell_formula_units_Z            2
_cell_length_a                   9.5312(6)
_cell_length_b                   10.2585(6)
_cell_length_c                   11.7914(6)
_cell_measurement_reflns_used    14050
_cell_measurement_temperature    100(2)
_cell_volume                     979.73(14)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        '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'
_diffrn_measurement_method       '129 images at 1.0 deg. in \w and 40 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_theta_max         33.15
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   'gaussian, face-indexed'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       'opaque needle'
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.707
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7344
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_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0536
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_refine_ls_shift/esd_max         0.000
_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^+0.7518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0807
_refine_ls_wR_factor_obs         0.0714
_reflns_number_observed          5509
_reflns_number_total             7391
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja030123u_3.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.7518P] 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^+0.7518P] 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        979.73(10)
_cod_database_code               4113980