A Two-Coordinate Nickel Imido Complex That Effects C-H Amination
Carl A. Laskowski; Alexander J. M. Miller; Gregory L. Hillhouse; Thomas R. Cundari; Journal of the American Chemical Society 133 (2011) 771–773; doi:10.1021/ja1101213

data_4105552
_publ_section_title
;
 A Two-Coordinate Nickel Imido Complex That Effects C-H Amination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              771
_journal_page_last               773
_journal_paper_doi               10.1021/ja1101213
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C87 H80 N2 Ni'
_chemical_formula_weight         1212.24
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_secondary   difmap
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_cell_angle_gamma                89.2870(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9750(6)
_cell_length_b                   16.0260(9)
_cell_length_c                   19.3760(11)
_cell_measurement_reflns_used    32689
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.8222
_cell_measurement_theta_min      0.9352
_cell_volume                     3333.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32689
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.9352
_exptl_absorpt_correction_T_min  0.8222
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Norton et. al.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         11703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                10192
_reflns_number_total             11703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1101213_si_002_3.cif
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