Enantiopure C1-Symmetric Bis(imino)pyridine Cobalt Complexes for Asymmetric Alkene Hydrogenation
Sebastien Monfette; Zoë R. Turner; Scott P. Semproni; Paul J. Chirik; Journal of the American Chemical Society 134 (2012) 4561–4564; doi:10.1021/ja300503k

data_4117687
_publ_section_title
;
 Enantiopure C1-Symmetric Bis(imino)pyridine Cobalt Complexes for
 Asymmetric Alkene Hydrogenation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4561
_journal_page_last               4564
_journal_paper_doi               10.1021/ja300503k
_journal_volume                  134
_journal_year                    2012
_chemical_absolute_configuration syn
_chemical_formula_sum            'C27 H39 Cl Co N3'
_chemical_formula_weight         499.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.094(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.611(2)
_cell_length_b                   12.746(3)
_cell_length_c                   24.056(6)
_cell_measurement_reflns_used    66
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.4092
_cell_measurement_theta_min      3.2823
_cell_volume                     2935.3(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_radiation_monochromator  'Triumph curved-crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33480
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'clear dark purple-blue'
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.036
_platon_squeeze_details
;The unit cell contains 3 diethyl ether molecules which have been treated
as a diffuse contribution to the overall scattering without specific
atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         13017
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                10055
_reflns_number_total             13017
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja300503k_si_001_6.cif
_cod_data_source_block           sm2
_cod_original_cell_volume        2935.2(12)
_cod_database_code               4117687