Carbon-Hydrogen Bond Activation, C-N Bond Coupling, and Cycloaddition Reactivity of a Three-Coordinate Nickel Complex Featuring a Terminal Imido Ligand.
Mindiola, Daniel J.; Waterman, Rory; Iluc, Vlad M.; Cundari, Thomas R.; Hillhouse, Gregory L.; Inorganic chemistry  (2014) 141201110357006–; doi:10.1021/ic5026153

data_4341877
_publ_section_title
;
 Carbon-Hydrogen Bond Activation, C-N Bond Coupling, and Cycloaddition
 Reactivity of a Three-Coordinate Nickel Complex Featuring a Terminal
 Imido Ligand.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141201110357006
_journal_paper_doi               10.1021/ic5026153
_journal_year                    2014
_chemical_formula_sum            'C38 H63 N Ni O1.5 P2'
_chemical_formula_weight         678.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.4030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9378(6)
_cell_length_b                   18.7987(12)
_cell_length_c                   20.7194(13)
_cell_measurement_temperature    373(2)
_cell_volume                     3818.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15316
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.9756
_exptl_absorpt_correction_T_min  0.8354
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00000(13)
_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   1.317
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         4992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.317
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          4.951
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+13.5934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                4802
_reflns_number_total             4992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5026153_si_005.cif
_cod_data_source_block           danm13t
_cod_original_formula_sum        'C38 H63 N Ni O1.50 P2'
_cod_database_code               4341877