Ni(I)-Ni(III) Cycle in Buchwald-Hartwig Amination of Aryl Bromide Mediated by NHC-ligated Ni(I) Complexes
Inatomi, Takahiro; Fukahori, Yukino; Yamada, Yuji; Ishikawa, Ryuta; Kanegawa, Shinji; Koga, Yuji; Matsubara, Kouki; Catalysis Science & Technology  (2019) –; doi:10.1039/C8CY02427H

data_1550593
_publ_section_title
;
 Ni(I)-Ni(III) Cycle in Buchwald-Hartwig Amination of Aryl Bromide
 Mediated by NHC-ligated Ni(I) Complexes
;
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_paper_doi               10.1039/C8CY02427H
_journal_year                    2019
_chemical_formula_moiety         'C49 H54 N5 Ni'
_chemical_formula_sum            'C49 H54 N5 Ni'
_chemical_formula_weight         771.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-11-09 deposited with the CCDC.    2019-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.636(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.812(3)
_cell_length_b                   21.544(4)
_cell_length_c                   16.480(4)
_cell_measurement_reflns_used    10843
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.06
_cell_volume                     4192.1(17)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            63987
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1644.00
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.710
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     504
_refine_ls_number_reflns         9570
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0628P)^2^+2.6855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                8886
_reflns_number_total             9591
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c8cy02427h2.cif
_cod_data_source_block           3a
_cod_database_code               1550593