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_4331195
_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_absolute_configuration syn
_chemical_formula_sum            'C40 H37 N5 O2'
_chemical_formula_weight         619.75
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ds42
_audit_creation_method           SHELXL-97
_audit_update_record             'Tue Sep 18 11:59:15 CEST 2012'
_cell_angle_alpha                90.00
_cell_angle_beta                 113.144(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.171(7)
_cell_length_b                   7.052(3)
_cell_length_c                   16.168(7)
_cell_measurement_reflns_used    8084
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.89
_cell_measurement_theta_min      2.36
_cell_volume                     1590.5(12)
_computing_cell_refinement
;
SAINT 8.x (Bruker AXS, 1997-2011). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT 8.x (Bruker AXS, 1997-2011)'
_computing_publication_material  'encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40254
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         32.29
_diffrn_reflns_theta_min         2.36
_diffrn_source                   'fine-focus sealed tube (Mo)'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.8106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.064
_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   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         5802
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0843P)^2^+0.1304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                5463
_reflns_number_total             5802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3020749_si_002_03.cif
_cod_data_source_block           SS-8
_cod_original_cell_volume        1590.6(12)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4331195
_audit_block_refno               1281
_audit_block_usercomment         des490