Cobalt Alkyl Complexes of a New Family of Chiral 1,3-Bis(2-pyridylimino)isoindolates and Their Application in Asymmetric Hydrosilylation
Désirée C. Sauer; Hubert Wadepohl; Lutz H. Gade; Inorganic Chemistry 51 (2012) 12948–12958; doi:10.1021/ic3020749

data_4331202
_publ_section_title
;
 Cobalt Alkyl Complexes of a New Family of Chiral
 1,3-Bis(2-pyridylimino)isoindolates and Their Application in Asymmetric
 Hydrosilylation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12948
_journal_page_last               12958
_journal_paper_doi               10.1021/ic3020749
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C30 H35 Co N5 Si'
_chemical_formula_weight         552.65
_chemical_properties_physical    air-sensitive
_space_group_IT_number           2
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ds55
_audit_creation_date
;
'Mon Apr 16 16:54:21 2012'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_audit_update_record             'Mon Apr 16 17:12:45 CEST 2012'
_cell_angle_alpha                87.707(12)
_cell_angle_beta                 68.561(10)
_cell_angle_gamma                76.285(9)
_cell_formula_units_Z            2
_cell_length_a                   10.5259(8)
_cell_length_b                   11.7868(17)
_cell_length_c                   12.0577(18)
_cell_measurement_reflns_used    3951
_cell_measurement_temperature    109.96(14)
_cell_measurement_theta_max      72.5930
_cell_measurement_theta_min      3.8623
_cell_volume                     1350.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      109.96(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega  -17.00   19.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   90.0000 36

  2 omega   35.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  120.0000 34

  3 omega  -16.00   27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  120.0000 43

  4 omega  -68.00  -27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   90.0000 41

  5 omega -104.00  -64.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   60.0000 40

  6 omega  -46.00  -12.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -180.0000 34

  7 omega  -57.00  -12.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000    0.0000 45

  8 omega  -47.00  -12.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   60.0000 35

  9 omega -113.00  -76.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -60.0000 37

 10 omega  -79.00  -34.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000 -180.0000 45

 11 omega  -45.00  -12.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -60.0000 33

 12 omega  -46.00  -13.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -120.0000 33

 13 omega -100.00  -73.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -120.0000 27

 14 omega -119.00  -80.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000 -180.0000 39

 15 omega -111.00  -83.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -180.0000 28

 16 omega  -40.00  -12.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  120.0000 28

 17 omega   35.00  125.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   77.0000   60.0000 90

 18 omega   44.00   72.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   77.0000  -30.0000 28

 19 omega   25.00   52.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   77.0000   30.0000 27

 20 omega   77.00  119.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   77.0000  -30.0000 42

 21 omega   35.00  114.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   66.0000 -174.0000 79

 22 omega   28.00  122.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   77.0000  120.0000 94

 23 omega   88.00  124.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296 -143.0000 -120.0000 36

 24 omega  -16.00   78.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296  -38.0000 -180.0000 94

 25 omega  -13.00   74.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296  -57.0000  -60.0000 87

 26 omega  -13.00   77.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296  -57.0000   30.0000 90

 27 omega   26.00  110.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   77.0000 -120.0000 84

 28 omega   26.00  116.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   77.0000  -60.0000 90

 29 omega    2.00   78.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296  -99.0000 -180.0000 76

 30 omega   95.00  123.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  -30.0000 28

 31 omega   87.00  114.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000  120.0000 27

 32 omega   40.00  109.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592 -111.0000  120.0000 69

 33 omega   85.00  113.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000   90.0000 28

 34 omega  123.00  175.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   30.0000 52

 35 omega   91.00  125.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000   60.0000 34

 36 omega   85.00  112.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000 -150.0000 27

 37 omega   81.00  109.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   30.0000 28

 38 omega   81.00  108.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   60.0000 27

 39 omega  148.00  176.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -120.0000 28

 40 omega   82.00  108.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -120.0000 26

 41 omega  119.00  171.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000    0.0000 52

 42 omega   91.00  123.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000   90.0000 32

 43 omega   89.00  118.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000   30.0000 29

 44 omega   81.00  109.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000    0.0000 28

 45 omega   89.00  173.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000  -60.0000 84

 46 omega   81.00  108.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -90.0000 27

 47 omega   86.00  112.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000   60.0000 26

 48 omega   85.00  123.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000  -60.0000 38

 49 omega   96.00  176.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  120.0000 80

 50 omega   88.00  115.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000 -120.0000 27

 51 omega   88.00  167.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000  -30.0000 79

 52 omega  122.00  173.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   60.0000 51

 53 omega   77.00  105.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   25.0000   30.0000 28

 54 omega   81.00  108.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -60.0000 27

 55 omega   83.00  108.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   90.0000 25

 56 omega  125.00  162.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   90.0000 37

 57 omega   68.00   96.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -91.0000  -60.0000 28

 58 omega  119.00  149.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -91.0000  -60.0000 30

 59 omega   90.00  119.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000 -180.0000 29

 60 omega   90.00  178.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  -90.0000 88

 61 omega  141.00  168.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000 -120.0000 27

 62 omega   81.00  108.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -150.0000 27

 63 omega   47.00  138.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -77.0000 -150.0000 91

 64 omega   85.00  112.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000 -180.0000 27

 65 omega   91.00  116.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000 -120.0000 25

 66 omega   85.00  112.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000 -120.0000 27

 67 omega  121.00  176.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -180.0000 55

 68 omega   86.00  114.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000   30.0000 28

 69 omega   88.00  116.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000   30.0000 28

 70 omega   81.00  109.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -180.0000 28

 71 omega  116.00  174.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  150.0000 58

 72 omega   78.00  107.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   25.0000 -120.0000 29

 73 omega   83.00  115.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592 -111.0000 -180.0000 32

 74 omega  117.00  177.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -150.0000 60

 75 omega   86.00  111.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000  150.0000 25

 76 omega   81.00  113.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  150.0000 32

 77 omega   82.00  108.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -30.0000 26

 78 omega   44.00  111.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592 -111.0000   30.0000 67

 79 omega   89.00  118.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  150.0000 29

 80 omega   44.00  130.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -63.0000   90.0000 86

 81 omega  -69.00   21.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -150.0000 90

 82 omega  -72.00   26.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000 -120.0000 98

 83 omega  -21.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 90

 84 omega -110.00  -20.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -63.0000   90.0000 90

 85 omega   25.00  126.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   77.0000  -90.0000 101

 86 omega   23.00  113.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296 -125.0000   30.0000 90

 87 omega  -18.00  128.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296    0.0000 -150.0000 146

 88 omega   31.00  124.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   69.0000 -146.0000 93

 89 omega   33.00   87.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296   64.0000   31.0000 54

 90 omega  -17.00   81.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296  -38.0000  120.0000 98

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.1524506000
_diffrn_orient_matrix_UB_12      -0.0095194000
_diffrn_orient_matrix_UB_13      0.0305285000
_diffrn_orient_matrix_UB_21      0.0481436000
_diffrn_orient_matrix_UB_22      -0.1341294000
_diffrn_orient_matrix_UB_23      -0.0010745000
_diffrn_orient_matrix_UB_31      -0.0258038000
_diffrn_orient_matrix_UB_32      0.0082206000
_diffrn_orient_matrix_UB_33      0.1340095000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_av_sigmaI/netI    0.1908
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20629
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         72.5930
_diffrn_reflns_theta_min         3.8623
_diffrn_source                   'Agilent SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    5.619
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       plate
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.2423
_exptl_crystal_size_mid          0.0710
_exptl_crystal_size_min          0.0140
_refine_diff_density_max         2.190
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0895
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+3.7402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2138
_refine_ls_wR_factor_ref         0.2301
_reflns_number_gt                3972
_reflns_number_total             5195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3020749_si_002_10.cif
_cod_data_source_block           23
_cod_database_code               4331202
_audit_block_refno               1477
_audit_block_usercomment         'des580, plate, red'
_cell_oxdiff_length_a            10.5259(8)
_cell_oxdiff_length_b            11.7868(17)
_cell_oxdiff_length_c            12.0577(18)
_cell_oxdiff_angle_alpha         87.707(12)
_cell_oxdiff_angle_beta          68.560(10)
_cell_oxdiff_angle_gamma         76.285(9)
_cell_oxdiff_volume              1350.9(3)
_cell_oxdiff_measurement_reflns_used 3951
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1