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_4127254
_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            'C84 H67 Co N2'
_chemical_formula_weight         1163.32
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                75.348(11)
_cell_angle_beta                 84.047(10)
_cell_angle_gamma                64.970(12)
_cell_formula_units_Z            2
_cell_length_a                   12.594(9)
_cell_length_b                   14.092(10)
_cell_length_c                   20.413(16)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.964
_cell_measurement_theta_min      2.3245
_cell_volume                     3176(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46604
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.057
_diffrn_reflns_theta_max         25.057
_diffrn_reflns_theta_min         1.031
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       cube
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.959
_refine_diff_density_min         -2.123
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         11197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1489P)^2^+11.4101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2532
_refine_ls_wR_factor_ref         0.2734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8562
_reflns_number_total             11197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01262_si_002.cif
_cod_data_source_block           LCo
_cod_depositor_comments
'Adding full bibliography for 4127253--4127260.cif.'
_cod_database_code               4127254
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              85727
_shelx_hkl_checksum              74676