Isolated Organometallic Nickel(III) and Nickel(IV) Complexes Relevant to Carbon-Carbon Bond Formation Reactions.
Schultz, Jason W.; Fuchigami, Kei; Zheng, Bo; Rath, Nigam P.; Mirica, Liviu M.; Journal of the American Chemical Society 138 (2016) 12928–12934; doi:10.1021/jacs.6b06862

data_4130794
_publ_section_title
;
 Isolated Organometallic Nickel(III) and Nickel(IV) Complexes Relevant to
 Carbon-Carbon Bond Formation Reactions.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12928
_journal_page_last               12934
_journal_paper_doi               10.1021/jacs.6b06862
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C24 H20 B, C18 H26 N4 Ni, C4 H8 O'
_chemical_formula_sum            'C46 H54 B N4 Ni O'
_chemical_formula_weight         748.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                88.779(4)
_cell_angle_beta                 75.985(4)
_cell_angle_gamma                73.867(4)
_cell_formula_units_Z            2
_cell_length_a                   8.9600(7)
_cell_length_b                   14.2611(10)
_cell_length_c                   16.7826(12)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.44
_cell_volume                     1996.3(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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40240
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_min         1.252
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2012/1'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             798
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.149
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9164
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.2182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7557
_reflns_number_total             9164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06862_si_002.cif
_cod_data_source_block           l8714_sq_[(MeN4)NiMe2]BPh4
_cod_database_code               4130794
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2013-4
_shelx_res_checksum              11552
_shelx_hkl_checksum              38883
_shelx_fab_checksum              51927