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_4130795
_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         'C26 H32 N4 Ni, C4 H8 O'
_chemical_formula_sum            'C30 H40 N4 Ni O'
_chemical_formula_weight         531.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.026(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5021(9)
_cell_length_b                   17.8327(13)
_cell_length_c                   12.9451(11)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.63
_cell_volume                     2655.2(4)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.969
_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_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29108
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.624
_diffrn_reflns_theta_min         1.142
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.746070
_exptl_absorpt_correction_T_min  0.621766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'twinabs v2012/1'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.589
_exptl_crystal_size_mid          0.566
_exptl_crystal_size_min          0.232
_refine_diff_density_max         1.273
_refine_diff_density_min         -1.586
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
; 
 Flack x determined using 3484 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.010(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         29108
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0458P)^2^+5.0651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1316
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.836
_reflns_number_gt                26486
_reflns_number_total             29108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06862_si_002.cif
_cod_data_source_block           l19415t5_(MeN4)Ni(cycloneophyl)
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4130795
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.663
_shelx_estimated_absorpt_t_max   0.843
_shelx_res_checksum              37537
_shelx_hkl_checksum              83211