Mechanistic Analysis of Metallaphotoredox C-N Coupling: Photocatalysis Initiates and Perpetuates Ni(I)/Ni(III) Coupling Activity.
Till, Nicholas A.; Tian, Lei; Dong, Zhe; Scholes, Gregory D.; MacMillan, David W. C.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c05901

data_4135229
_publ_section_title
;
 Mechanistic Analysis of Metallaphotoredox C-N Coupling: Photocatalysis
 Initiates and Perpetuates Ni(I)/Ni(III) Coupling Activity.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c05901
_journal_year                    2020
_chemical_formula_sum            'C17 H30 Br F6 N3 Ni'
_chemical_formula_weight         529.06
_chemical_name_common            NT2
_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   mixed
_cell_angle_alpha                90
_cell_angle_beta                 95.4095(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1264(3)
_cell_length_b                   9.0714(2)
_cell_length_c                   20.8156(6)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      70.1501
_cell_measurement_theta_min      4.0604
_cell_volume                     2279.59(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2016)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Photon 100 CMOS'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33696
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         4.06
_diffrn_source                   'I\mS microfocus source'
_exptl_absorpt_coefficient_mu    3.793
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'translucent intense yellow'
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.345
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4160
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0318P)^2^+3.8456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                3849
_reflns_number_total             4160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c05901_si_003.cif
_cod_data_source_block           PDJNT2
_cod_database_code               4135229
_shelx_res_checksum              26100
_shelx_hkl_checksum              66500