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_4117688
_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_formula_moiety         'C27.03 H38.10 Co N3, 2(C27 H38 Co N3)'
_chemical_formula_sum            'C81.03 H114.1 Co3 N9'
_chemical_formula_weight         1390.60
_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                 92.985(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0290(9)
_cell_length_b                   19.6508(18)
_cell_length_c                   19.1243(17)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.90
_cell_volume                     3763.9(6)
_computing_cell_refinement       'SHELXL-97 (Sheldrick, 2008)'
_computing_data_collection       'BRUKER APEX II software suite (Bruker AXS)'
_computing_data_reduction        'BRUKER APEX II software suite (Bruker AXS)'
_computing_molecular_graphics    'ORTEP 3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Farrugia, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35242
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.9331
_exptl_absorpt_correction_T_min  0.7912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs 2008/2'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 7983 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.003(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         16832
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                14317
_reflns_number_total             16832
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja300503k_si_001_7.cif
_cod_data_source_block           sm16
_cod_original_formula_sum        'C81.03 H114.10 Co3 N9'
_cod_database_code               4117688