Carbon-Fluorine Bond Activation Coupled with Carbon-Carbon Bond Formation at Iridium. Confirmation of Complete Kinetic Diastereoselectivity at the New Carbon Stereocenter by Intramolecular Trapping Using Vinyl as the Migrating Group
Russell P. Hughes; Roman B. Laritchev; Lev N. Zakharov; Arnold L. Rheingold; Journal of the American Chemical Society 127 (2005) 6325–6334; doi:10.1021/ja042345d

data_4111641
_publ_section_title
;
 Carbon-Fluorine Bond Activation Coupled with Carbon-Carbon Bond Formation
 at Iridium. Confirmation of Complete Kinetic Diastereoselectivity at the
 New Carbon Stereocenter by Intramolecular Trapping Using Vinyl as the
 Migrating Group
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6325
_journal_page_last               6334
_journal_paper_doi               10.1021/ja042345d
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C50 H38 B F30 Ir P'
_chemical_formula_weight         1442.78
_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                84.3880(10)
_cell_angle_beta                 73.3670(10)
_cell_angle_gamma                84.6180(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1256(9)
_cell_length_b                   12.5665(9)
_cell_length_c                   18.2649(13)
_cell_measurement_reflns_used    8384
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.31
_cell_volume                     2647.6(3)
_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, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22728
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    2.694
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             1410
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.795
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         11762
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+9.1893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                10863
_reflns_number_total             11762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja042345dsi20050107_115716_3.cif
_cod_data_source_block           rph270_compound8
_cod_database_code               4111641