Flexible, Bowl-Shaped N-Heterocyclic Carbene Ligands: Substrate Specificity in Iridium-Catalyzed Ketone Hydrosilylation
Chianese, Anthony R.; Mo, Allen; Datta, Dibyadeep; Organometallics 28 (2009) 465–472; doi:10.1021/om800878m

data_4063528
_publ_contact_author_address
'Department of Chemistry, Colgate University, Hamilton, NY 13346, USA'
_publ_contact_author_email       ' achianese@colgate.edu '
_publ_contact_author_fax         ' (315)-228-7935 '
_publ_contact_author_name        ' Anthony R. Chianese'
_publ_contact_author_phone       ' (315)-228-7718 '
_publ_section_title
;
 Flexible, Bowl-Shaped N-Heterocyclic Carbene Ligands: Substrate
 Specificity in Iridium-Catalyzed Ketone Hydrosilylation
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              465
_journal_page_last               472
_journal_paper_doi               10.1021/om800878m
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C31 H34 Cl Ir N2'
_chemical_formula_sum            'C31 H34 Cl Ir N2'
_chemical_formula_weight         662.25
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.661(3)
_cell_angle_beta                 83.367(3)
_cell_angle_gamma                70.772(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9618(18)
_cell_length_b                   11.220(3)
_cell_length_c                   16.253(4)
_cell_measurement_reflns_used    7894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.25
_cell_volume                     1352.8(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9466
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         1.93
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.055
_exptl_absorpt_correction_T_max  0.3623
_exptl_absorpt_correction_T_min  0.2624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SAINTABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_recrystallization_method dichloromethane/pentane
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.728
_refine_diff_density_min         -2.663
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.0051(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.7303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                5803
_reflns_number_total             6156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800878m_si_003.cif
_cod_data_source_block           arc01a
_cod_original_cell_volume        1352.9(6)
_cod_database_code               4063528