Catalytic C-H Amination Mediated by Dipyrrin Cobalt Imidos.
Baek, Yunjung; Betley, Theodore A.; Journal of the American Chemical Society 141 (2019) 7797–7806; doi:10.1021/jacs.9b01262

data_4127253
_publ_section_title
;
 Catalytic C-H Amination Mediated by Dipyrrin Cobalt Imidos.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7797
_journal_page_last               7806
_journal_paper_doi               10.1021/jacs.9b01262
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C42 H33.5 Br0.5 Co0.5 N'
_chemical_formula_weight         621.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.561(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9671(16)
_cell_length_b                   22.041(2)
_cell_length_c                   18.9148(18)
_cell_measurement_reflns_used    9676
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.084
_cell_measurement_theta_min      2.2465
_cell_volume                     6380.6(11)
_computing_cell_refinement       'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33973
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.228
_diffrn_reflns_theta_max         25.228
_diffrn_reflns_theta_min         2.247
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         5707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1577
_refine_ls_R_factor_gt           0.0887
_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^)+(0.0714P)^2^+44.1335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1894
_refine_ls_wR_factor_ref         0.2186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3425
_reflns_number_total             5707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01262_si_002.cif
_cod_data_source_block           LCoBr
_cod_depositor_comments
'Adding full bibliography for 4127253--4127260.cif.'
_cod_original_formula_sum        'C42 H33.50 Br0.50 Co0.50 N'
_cod_database_code               4127253
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.834
_shelx_estimated_absorpt_t_max   0.920
_shelx_res_checksum              9188
_shelx_hkl_checksum              89396