Carbon-Carbon Bond-Forming Reductive Elimination from Isolated Nickel(III) Complexes.
Bour, James R.; Camasso, Nicole M.; Meucci, Elizabeth A.; Kampf, Jeff W.; Canty, Allan J.; Sanford, Melanie S.; Journal of the American Chemical Society 138 (2016) 16105–16111; doi:10.1021/jacs.6b10350

data_4131162
_publ_section_title
;
 Carbon-Carbon Bond-Forming Reductive Elimination from Isolated
 Nickel(III) Complexes.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16105
_journal_page_last               16111
_journal_paper_doi               10.1021/jacs.6b10350
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C19 H24 B F3 N6 Ni P'
_chemical_formula_sum            'C19 H24 B F3 N6 Ni P'
_chemical_formula_weight         493.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 100.4640(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.50891(8)
_cell_length_b                   17.83577(13)
_cell_length_c                   15.13048(14)
_cell_measurement_reflns_used    11867
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.8230
_cell_measurement_theta_min      4.9520
_cell_volume                     2258.06(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.975
_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  0.0610
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17165
_diffrn_reflns_point_group_measured_fraction_full 0.809
_diffrn_reflns_point_group_measured_fraction_max 0.800
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.266
_diffrn_reflns_theta_min         4.959
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    2.292
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90610
_exptl_absorpt_correction_type   multi-scan
_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            blue
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
; 
 Flack x determined using 1285 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.030(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3360
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.3457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.637
_reflns_Friedel_fraction_full    0.635
_reflns_Friedel_fraction_max     0.624
_reflns_number_gt                3337
_reflns_number_total             3360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10350_si_004.cif
_cod_data_source_block           jrb3064
_cod_original_cell_volume        2258.06(4)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4131162
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.956
_shelxl_version_number           2014/6
_shelx_res_checksum              92112
_shelx_hkl_checksum              73608