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_4113978
_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            'C28 H44 N4 Ni'
_chemical_formula_weight         495.38
_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                 103.16(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7105(12)
_cell_length_b                   9.5010(10)
_cell_length_c                   13.889(2)
_cell_measurement_temperature    100(2)
_cell_volume                     1376.2(3)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '402 images at 1.0 deg. in \w and 180 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  0.1947
_diffrn_reflns_av_sigmaI/netI    0.1308
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13274
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         4.99
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.9715
_exptl_absorpt_correction_T_min  0.8804
_exptl_absorpt_correction_type   'gaussian, face-indexed'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.071
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.005(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3984
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.1058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+9.0422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2363
_refine_ls_wR_factor_ref         0.2435
_reflns_number_gt                3206
_reflns_number_total             3984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja030123u_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+9.0422P] 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^+9.0422P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4113978