Connecting Organometallic Ni(III) and Ni(IV): Reactions of Carbon-Centered Radicals with High-Valent Organonickel Complexes.
Bour, James R.; Ferguson, Devin M.; McClain, Edward J.; Kampf, Jeff W.; Sanford, Melanie S.; Journal of the American Chemical Society 141 (2019) 8914–8920; doi:10.1021/jacs.9b02411

data_4127555
_publ_section_title
;
 Connecting Organometallic Ni(III) and Ni(IV): Reactions of
 Carbon-Centered Radicals with High-Valent Organonickel Complexes.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8914
_journal_page_last               8920
_journal_paper_doi               10.1021/jacs.9b02411
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C22 H21 B F8 N6 Ni'
_chemical_formula_sum            'C22 H21 B F8 N6 Ni'
_chemical_formula_weight         590.97
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 96.6667(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.18015(5)
_cell_length_b                   18.14258(9)
_cell_length_c                   13.24800(6)
_cell_measurement_reflns_used    27038
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      69.0450
_cell_measurement_theta_min      4.1280
_cell_volume                     2430.28(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36328
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.282
_diffrn_reflns_theta_min         4.150
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80014
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_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00258(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0475P)^2^+1.3617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4444
_reflns_number_total             4509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02411_si_003.cif
_cod_data_source_block           jrb4112
_cod_database_code               4127555
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.759
_shelx_estimated_absorpt_t_max   0.844
_shelx_res_checksum              70170
_shelx_hkl_checksum              99882