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_4127257
_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            'C166 H144 Co2 N6'
_chemical_formula_weight         2340.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                74.791(2)
_cell_angle_beta                 73.522(2)
_cell_angle_gamma                85.350(2)
_cell_formula_units_Z            2
_cell_length_a                   16.0680(10)
_cell_length_b                   16.5966(10)
_cell_length_c                   24.9849(15)
_cell_measurement_reflns_used    9764
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.007
_cell_measurement_theta_min      2.3025
_cell_volume                     6165.2(7)
_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)'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1770
_diffrn_reflns_av_unetI/netI     0.2215
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            83893
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.076
_diffrn_reflns_theta_max         25.076
_diffrn_reflns_theta_min         2.412
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       plate
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1501
_refine_ls_number_reflns         21790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.2475
_refine_ls_R_factor_gt           0.1113
_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^)+(0.0403P)^2^+32.2226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.2265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9542
_reflns_number_total             21790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01262_si_002.cif
_cod_data_source_block           LCoNAd
_cod_depositor_comments
'Adding full bibliography for 4127253--4127260.cif.'
_cod_database_code               4127257
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              92123
_shelx_hkl_checksum              5334