A Structurally Rigid Bis(amido) Ligand Framework in Low-Coordinate Ni(I), Ni(II), and Ni(III) Analogues Provides Access to a Ni(III) Methyl Complex via Oxidative Addition
Michael I. Lipschutz; Xinzheng Yang; Ruchira Chatterjee; T. Don Tilley; Journal of the American Chemical Society 135 (2013) 15298–15301; doi:10.1021/ja408151h

data_4120947
_publ_section_title
;
 A Structurally Rigid Bis(amido) Ligand Framework in Low-Coordinate Ni(I),
 Ni(II), and Ni(III) Analogues Provides Access to a Ni(III) Methyl Complex
 via Oxidative Addition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15298
_journal_page_last               15301
_journal_paper_doi               10.1021/ja408151h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C30 H52 Co N2 Si2'
_chemical_formula_weight         555.85
_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-97
_cell_angle_alpha                102.530(4)
_cell_angle_beta                 92.358(4)
_cell_angle_gamma                113.879(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8146(8)
_cell_length_b                   9.1675(8)
_cell_length_c                   11.1307(10)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.55
_cell_volume                     794.44(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0131
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21145
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.9750
_exptl_absorpt_correction_T_min  0.9277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             301
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.3594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                2773
_reflns_number_total             2919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408151h_si_006.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        794.44(12)
_cod_database_code               4120947