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_4063527
_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         'C163 H202 Cl Ir N2, 2(C4 H10 O)'
_chemical_formula_sum            'C171 H222 Cl Ir N2 O2'
_chemical_formula_weight         2565.32
_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                105.1818(12)
_cell_angle_beta                 91.6623(12)
_cell_angle_gamma                112.4566(12)
_cell_formula_units_Z            2
_cell_length_a                   20.6701(20)
_cell_length_b                   21.1109(21)
_cell_length_c                   21.9235(21)
_cell_measurement_reflns_used    9576
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1598
_cell_measurement_theta_min      2.2324
_cell_volume                     8442.9(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.909
_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  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            121184
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.55
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.7585
_exptl_absorpt_correction_T_min  0.5654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SAINTABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_recrystallization_method ethanol/ether
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.33
_platon_squeeze_details
;
;
_refine_diff_density_max         5.348
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1645
_refine_ls_number_reflns         38383
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0800P)^2^+0.6702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1358
_reflns_number_gt                31582
_reflns_number_total             38383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800878m_si_002.cif
_cod_data_source_block           arc02
_cod_original_cell_volume        8442.8(14)
_cod_database_code               4063527