Enantioselective Construction of Spiroindolenines by Ir-Catalyzed Allylic Alkylation Reactions
Qing-Feng Wu; Hu He; Wen-Bo Liu; Shu-Li You; Journal of the American Chemical Society 132 (2010) 11418–11419; doi:10.1021/ja105111n

data_4102937
_publ_section_title
;
 Enantioselective Construction of Spiroindolenines by Ir-Catalyzed Allylic
 Alkylation Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11418
_journal_page_last               11419
_journal_paper_doi               10.1021/ja105111n
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C44 H60.5 Br2 Cl4 N4 O2.5'
_chemical_formula_weight         987.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.0114(19)
_cell_length_b                   26.305(3)
_cell_length_c                   24.520(3)
_cell_measurement_temperature    293(2)
_cell_volume                     9682(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1616
_diffrn_reflns_av_sigmaI/netI    0.2787
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25644
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    1.935
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4084
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.069(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.659
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9015
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.666
_refine_ls_R_factor_all          0.2630
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          7.656
_refine_ls_shift/su_mean         0.166
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1084P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.2279
_reflns_number_gt                1968
_reflns_number_total             9015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105111n_si_002.cif
_cod_data_source_block           cd201234
_cod_original_formula_sum        'C44 H60.50 Br2 Cl4 N4 O2.50'
_cod_database_code               4102937