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_4130797
_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         'C20 H26 N6 Ni, 2(F6 P)'
_chemical_formula_sum            'C20 H26 F12 N6 Ni P2'
_chemical_formula_weight         699.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 92.739(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2668(5)
_cell_length_b                   16.5937(10)
_cell_length_c                   18.2485(11)
_cell_measurement_reflns_used    8890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.23
_cell_volume                     2802.9(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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.980
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23715
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.534
_diffrn_reflns_theta_min         1.660
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2014/3'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.303
_exptl_crystal_size_min          0.257
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0663
_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^)+(0.1015P)^2^+9.4713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.2007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4605
_reflns_number_total             6328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06862_si_002.cif
_cod_data_source_block           l10215_[(MeN4)Ni(MeCN)2](PF6)2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4130797
_shelx_estimated_absorpt_t_min   0.727
_shelx_estimated_absorpt_t_max   0.800
_shelxl_version_number           2014/6
_shelx_res_checksum              6827
_shelx_hkl_checksum              72638