C-H Functionalization Reactivity of a Nickel-Imide
Stefan Wiese; Jason L. McAfee; Dale R. Pahls; Claire L. McMullin; Thomas R. Cundari; Timothy H. Warren; Journal of the American Chemical Society 134 (2012) 10114–10121; doi:10.1021/ja302149k

data_4118073
_publ_contact_author             'Timothy H. Warren'
_publ_contact_author_email       thw@georgetown.edu
_publ_section_title
;
 C-H Functionalization Reactivity of a Nickel-Imide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10114
_journal_page_last               10121
_journal_paper_doi               10.1021/ja302149k
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C43 H58 N3 Ni O0.50'
_chemical_formula_sum            'C43 H58 N3 Ni O0.5'
_chemical_formula_weight         683.63
_chemical_name_common            '[Me3NN]Ni-N(CHMePh)Ad.1/2ether'
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            4
_cell_length_a                   16.670(3)
_cell_length_b                   24.497(4)
_cell_length_c                   9.2897(14)
_cell_measurement_reflns_used    4856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.175
_cell_measurement_theta_min      2.193
_cell_volume                     3793.6(11)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker APEXII'
_computing_molecular_graphics
'XSEED for Windows with POV-Ray; Barbour L (1999)'
_computing_publication_material  'Bruker SHELXTL'
_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_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  0.0903
_diffrn_reflns_av_sigmaI/netI    0.0785
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30102
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS based on Blessing's method; Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7477
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0997P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1610
_reflns_number_gt                5624
_reflns_number_total             7477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja302149k_si_001.cif
_cod_data_source_block           cmpd_3
_cod_original_cell_volume        3793.5(10)
_cod_original_formula_sum        'C43 H58 N3 Ni O0.50'
_cod_database_code               4118073