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_4331196
_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            'C30 H33 N5 O2'
_chemical_formula_weight         495.61
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ds44
_audit_creation_method           SHELXL-97
_audit_update_record             'Tue Sep 18 12:03:39 CEST 2012'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.210(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.362(6)
_cell_length_b                   12.353(6)
_cell_length_c                   15.330(8)
_cell_measurement_reflns_used    8121
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.48
_cell_measurement_theta_min      2.25
_cell_volume                     2526(2)
_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 1.000
_diffrn_measured_fraction_theta_max 0.954
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31824
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         32.18
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'fine-focus sealed tube (Mo)'
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.8037
_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            red
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.065
_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   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4422
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0771P)^2^+0.7897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                3953
_reflns_number_total             4422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3020749_si_002_04.cif
_cod_data_source_block           RR-9
_cod_original_sg_symbol_H-M      'I 2'
_cod_database_code               4331196
_audit_block_refno               1301
_audit_block_usercomment         des482