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_4135231
_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            'C16 H21 Br F6 N2 Ni'
_chemical_formula_weight         493.97
_chemical_name_common            NT3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     SHELXT
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.6761(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3083(5)
_cell_length_b                   22.6701(11)
_cell_length_c                   7.3209(3)
_cell_measurement_reflns_used    4976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6645
_cell_measurement_theta_min      2.5667
_cell_volume                     1844.30(14)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2014.11.0.1'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Photon 100 CMOS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.797
_diffrn_source                   'fine focus tube'
_exptl_absorpt_coefficient_mu    3.278
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            'translucent pale red'
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.432
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4579
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+2.3752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3620
_reflns_number_total             4579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c05901_si_002.cif
_cod_data_source_block           mo_PDJNT3_0ma
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4135231
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.538
_shelx_estimated_absorpt_t_max   0.886
_shelx_res_checksum              65039
_shelx_hkl_checksum              12685