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_4127396
_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         'C36 H44 Co N5 O2 P, 2(B F4)'
_chemical_formula_sum            'C36 H44 B2 Co F8 N5 O2 P'
_chemical_formula_weight         842.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 99.1850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3076(4)
_cell_length_b                   11.2515(4)
_cell_length_c                   14.7336(5)
_cell_measurement_reflns_used    9056
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      3.04
_cell_volume                     2014.13(12)
_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 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18338
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        62.372
_diffrn_reflns_theta_max         62.372
_diffrn_reflns_theta_min         3.038
_exptl_absorpt_coefficient_mu    4.378
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.201
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.062(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5302
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0896P)^2^+3.4442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.956
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                5130
_reflns_number_total             5302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06035_si_002.cif
_cod_data_source_block           L8Co(ACN)2(BF4)2
_cod_database_code               4127396
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.420
_shelx_estimated_absorpt_t_max   0.473
_shelx_res_checksum              94441
_shelx_hkl_checksum              75985