Selective sp3 C-H Activation of Ketones at the β Position by Ir(I). Origin of Regioselectivity and Water Effect
Moran Feller; Amir Karton; Gregory Leitus; Jan M. L. Martin; David Milstein; Journal of the American Chemical Society 128 (2006) 12400–12401; doi:10.1021/ja0641352

data_4110915
_publ_section_title
;
 Selective sp3 C-H Activation of Ketones at the \b Position by Ir(I).
 Origin of Regioselectivity and Water Effect
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12400
_journal_page_last               12401
_journal_paper_doi               10.1021/ja0641352
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C26 H49 B F4 Ir N O3.5 P2'
_chemical_formula_weight         772.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                85.42(3)
_cell_angle_beta                 83.28(3)
_cell_angle_gamma                78.76(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2720(19)
_cell_length_b                   11.005(2)
_cell_length_c                   17.211(3)
_cell_measurement_reflns_used    7399
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1707.7(6)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        HKL
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7648
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    4.052
_exptl_absorpt_correction_T_max  0.4979
_exptl_absorpt_correction_T_min  0.2365
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       prism
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.958
_refine_diff_density_min         -2.637
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         7648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0885P)^2^+10.8412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                7041
_reflns_number_total             7648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0641352si20060612_120847.cif
_cod_data_source_block           m572a
_cod_original_formula_sum        'C26 H49 B F4 Ir N O3.50 P2'
_cod_database_code               4110915