Reaction of a Redox-Active Ligand Complex of Nickel with Dioxygen Probes Ligand-Radical Character
Tony D. Manuel; Jan-Uwe Rohde; Journal of the American Chemical Society 131 (2009) 15582–15583; doi:10.1021/ja9065943

data_4105259
_publ_section_title
;
 Reaction of a Redox-Active Ligand Complex of Nickel with Dioxygen Probes
 Ligand-Radical Character
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15582
_journal_page_last               15583
_journal_paper_doi               10.1021/ja9065943
_journal_volume                  131
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C32 H40 N3 O) Cl].2C H3 N O2'
_chemical_formula_moiety         'C32 H40 Cl N3 Ni O, 2(C H3 N O2)'
_chemical_formula_structural     '(Ni (C32 H40 N3 O) Cl) (C H3 N O2)2'
_chemical_formula_sum            'C34 H46 Cl N5 Ni O5'
_chemical_formula_weight         698.92
_chemical_name_systematic
; 
Chlorido{6-[1-(2,6-diisopropylphenylimino-\k<i>N</i>)ethyl]pyridyl-
\k<i>N</i>-2-<i>N</i>-(2,6-diisopropylphenyl)carboxamidato-
\k<i>N</i>}nickel(II)--nitromethane (1/2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 107.454(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1976(15)
_cell_length_b                   15.7496(17)
_cell_length_c                   16.8785(18)
_cell_measurement_reflns_used    15615
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.84
_cell_volume                     3600.4(7)
_computing_cell_refinement       'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond 3.2 (Crystal Impact, 1997-2009)'
_computing_publication_material  'SHELXTL v6.1 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXTL v6.1 (Bruker AXS, 2001)'
_computing_structure_solution    'SHELXTL v6.1 (Bruker AXS, 2001)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'area detector, \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29201
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.8686
_exptl_absorpt_correction_T_min  0.7974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL-2000 (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_recrystallization_method
;
nitromethane, -25 deg C
;
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         8549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+1.4026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                6454
_reflns_number_total             8549
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja9065943_si_002.cif
_cod_data_source_block           roh84
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4105259