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_4127395
_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         'C26 H25 Co I N2 O2 P, C4 H8 O [+ solvent]'
_chemical_formula_sum            'C30 H33 Co I N2 O3 P'
_chemical_formula_weight         686.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4527(3)
_cell_length_b                   25.1917(8)
_cell_length_c                   27.5943(9)
_cell_measurement_reflns_used    9668
_cell_measurement_temperature    172(2)
_cell_measurement_theta_max      68.26
_cell_measurement_theta_min      3.20
_cell_volume                     6571.0(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      172(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0776
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            65551
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.422
_diffrn_reflns_theta_min         2.375
_exptl_absorpt_coefficient_mu    12.169
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_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   0.4441
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.087(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         11942
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0846P)^2^+11.9415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                10312
_reflns_number_total             11942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06035_si_004.cif
_cod_data_source_block           L4CoI(THF)
_cod_database_code               4127395
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.158
_shelx_estimated_absorpt_t_max   0.195
_shelx_res_checksum              78926
_shelx_hkl_checksum              90179
_shelx_fab_checksum              3262