Cationic Co(I)-Intermediates for Hydrofunctionalization Reactions: Regio- and Enantioselective Cobalt-Catalyzed 1,2-Hydroboration of 1,3-Dienes.
Duvvuri, Krishnaja; Dewese, Kendra R.; Parsutkar, Mahesh M.; Jing, Stanley M.; Mehta, Milauni M.; Gallucci, Judith C.; RajanBabu, T. V.; Journal of the American Chemical Society 141 (2019) 7365–7375; doi:10.1021/jacs.8b13812

data_4128701
_publ_section_title
;
 Cationic Co(I)-Intermediates for Hydrofunctionalization Reactions: Regio-
 and Enantioselective Cobalt-Catalyzed 1,2-Hydroboration of 1,3-Dienes.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7365
_journal_page_last               7375
_journal_paper_doi               10.1021/jacs.8b13812
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C81 H78 Cl2 Co2 P6'
_chemical_formula_sum            'C81 H78 Cl2 Co2 P6'
_chemical_formula_weight         1426.01
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2018-09-07T12:01:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                66.4390(10)
_cell_angle_beta                 66.4010(10)
_cell_angle_gamma                71.7220(10)
_cell_formula_units_Z            4
_cell_length_a                   21.4598(9)
_cell_length_b                   21.5413(9)
_cell_length_c                   23.7245(10)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.76
_cell_measurement_wavelength     0.71073
_cell_volume                     9056.8(7)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'Apex3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT_2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON II CPAD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'TRIUMPH curved--crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            242477
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.057
_diffrn_reflns_theta_max         25.057
_diffrn_reflns_theta_min         2.755
_diffrn_source                   'fine--focus tube'
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS )'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
TITL shelx     P -1         R = 0.07
CELL   21.4598   21.5413   23.7245     66.44     66.40     71.72
SPGR P-1
C101 0.766 0.067 0.013 !       2.12 eA-3
C102 0.756 0.141 0.007 !       2.00 eA-3
C103 0.109 0.126 0.280 !       1.93 eA-3
C104 0.882 0.886 0.218 !       1.85 eA-3
C105 0.932 0.235 0.483 !       1.80 eA-3
C106 0.897 0.899 0.260 !       1.79 eA-3
C107 0.098 0.102 0.251 !       1.74 eA-3
C108 0.079 0.091 0.352 !       1.72 eA-3
C109 0.196 0.843 0.016 !       1.69 eA-3
C110 0.145 0.820 0.482 !       1.65 eA-3
C111 0.913 0.915 0.158 !       1.63 eA-3
C112 0.883 0.244 0.501 !       1.57 eA-3
C113 0.849 0.008 0.424 !       1.57 eA-3
C114 0.082 0.065 0.258 !       1.56 eA-3
C115 0.220 0.862 0.225 !       1.55 eA-3
C116 0.088 0.026 0.321 !       1.54 eA-3
C117 0.999 0.180 0.055 !       1.53 eA-3
C118 0.155 0.781 0.257 !       1.51 eA-3
C119 0.142 0.896 0.018 !       1.48 eA-3
C120 0.171 0.945 0.018 !       1.46 eA-3
C121 0.979 0.903 0.183 !       1.45 eA-3
C122 0.162 0.872 0.241 !       1.42 eA-3
C123 0.107 0.041 0.274 !       1.42 eA-3
C124 0.103 0.766 0.459 !       1.41 eA-3
C125 0.805 0.127 0.368 !       1.41 eA-3
C126 0.081 0.041 0.352 !       1.41 eA-3
C127 0.964 0.158 0.136 !       1.38 eA-3
C128 0.222 0.784 0.244 !       1.36 eA-3
C129 0.835 0.046 0.369 !       1.36 eA-3
C130 0.962 0.159 0.066 !       1.32 eA-3
C131 0.040 0.124 0.056 !       1.32 eA-3
C132 0.117 0.834 0.275 !       1.31 eA-3
C133 0.949 0.938 0.211 !       1.26 eA-3
C134 0.837 0.081 0.407 !       1.24 eA-3
C135 0.093 0.860 0.491 !       1.24 eA-3
C136 0.218 0.816 0.273 !       1.19 eA-3
C137 0.871 0.959 0.451 !       1.16 eA-3
C138 0.212 0.826 0.081 !       1.16 eA-3
C139 0.954 0.167 0.479 !       1.16 eA-3
C140 0.915 0.146 0.112 !       1.15 eA-3
C141 0.158 0.820 0.228 !       1.13 eA-3
C142 0.857 0.042 0.435 !       1.12 eA-3
C143 0.051 0.107 0.092 !       1.08 eA-3
C144 0.885 0.947 0.422 !       1.01 eA-3
C145 0.163 0.800 0.425 !       1.00 eA-3
C146 0.856 0.099 0.336 !       0.98 eA-3
C147 0.921 0.975 0.192 !       0.96 eA-3
C148 0.893 0.869 0.486 !       0.95 eA-3
C149 0.970 0.112 0.130 !       0.91 eA-3
C150 0.088 0.131 0.009 !       0.72 eA-3
Q151 0.442 0.312 0.493 !       0.70 eA-3
C152 0.931 0.937 0.429 !       0.68 eA-3
C153 0.916 0.901 0.470 !       0.64 eA-3
Q154 0.517 0.362 0.377 !       0.63 eA-3
Q155 0.319 0.445 0.009 !       0.62 eA-3
C156 0.263 0.734 0.249 !       0.62 eA-3
C157 0.889 0.136 0.195 !       0.58 eA-3
C158 0.080 0.093 0.496 !       0.57 eA-3
C159 0.913 0.082 0.204 !       0.53 eA-3
Q160 0.721 0.318 0.328 !       0.53 eA-3
C161 0.242 0.846 0.132 !       0.53 eA-3
C162 0.101 0.188 0.272 !       0.51 eA-3
Q163 0.819 0.097 0.279 !       0.50 eA-3
Q164 0.510 0.693 0.439 !       0.50 eA-3
;
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1640
_refine_ls_number_reflns         32006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+2.8051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                24933
_reflns_number_total             32006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13812_si_001.cif
_cod_data_source_block           RajanBabu2160
_cod_database_code               4128701
_platon_squeeze_void_probe_radius 1.20