Cobalt-Catalyzed Regio- and Enantioselective Allylic Amination.
Ghorai, Samir; Chirke, Sahadev Shrihari; Xu, Wen-Bin; Chen, Jia-Feng; Li, Changkun; Journal of the American Chemical Society 141 (2019) 11430–11434; doi:10.1021/jacs.9b06035

data_4127397
_publ_section_title
;
 Cobalt-Catalyzed Regio- and Enantioselective Allylic Amination.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11430
_journal_page_last               11434
_journal_paper_doi               10.1021/jacs.9b06035
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C35 H41 Co N4 O3 P, 2(B F4)'
_chemical_formula_sum            'C35 H41 B2 Co F8 N4 O3 P'
_chemical_formula_weight         829.24
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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-2016/6
_cell_angle_alpha                112.897(14)
_cell_angle_beta                 98.386(15)
_cell_angle_gamma                93.96(2)
_cell_formula_units_Z            1
_cell_length_a                   9.7764(18)
_cell_length_b                   10.020(2)
_cell_length_c                   10.928(2)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      4.47
_cell_volume                     966.3(3)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15109
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        63.775
_diffrn_reflns_theta_max         63.775
_diffrn_reflns_theta_min         4.472
_exptl_absorpt_coefficient_mu    4.567
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             427
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.6060
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.031(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         5017
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.5830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                4841
_reflns_number_total             5017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06035_si_003.cif
_cod_data_source_block           L9Co(ACN)2(BF4)2
_cod_original_cell_volume        966.2(4)
_cod_database_code               4127397
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.407
_shelx_estimated_absorpt_t_max   0.462
_shelx_res_checksum              54326
_shelx_hkl_checksum              75375