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_4105550
_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            'C89 H86 Cl2 N2 Ni O5'
_chemical_formula_weight         1393.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.515(3)
_cell_length_b                   28.008(4)
_cell_length_c                   29.362(4)
_cell_measurement_temperature    100(2)
_cell_volume                     14404(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0799
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            18144
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.9242
_exptl_absorpt_correction_T_min  0.7952
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Norton et. al.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             5888
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6295
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.583
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1129P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1832
_reflns_number_gt                4605
_reflns_number_total             6295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1101213_si_002_1.cif
_cod_data_source_block           (IPr*)(THF)NiCl2
_cod_original_cell_volume        14403(3)
_cod_database_code               4105550