Pd(II)-Catalyzed Enantioselective C-H Olefination of Diphenylacetic Acids
Bing-Feng Shi; Yang-Hui Zhang; Jonathan K. Lam; Dong-Hui Wang; Jin-Quan Yu; Journal of the American Chemical Society 132 (2010) 460–461; doi:10.1021/ja909571z

data_4101799
_publ_section_title
;
 Pd(II)-Catalyzed Enantioselective C-H Olefination of Diphenylacetic Acids
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              460
_journal_page_last               461
_journal_paper_doi               10.1021/ja909571z
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C23 H19 Cl O2'
_chemical_formula_weight         362.83
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 105.836(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9623(6)
_cell_length_b                   17.6350(13)
_cell_length_c                   12.5098(8)
_cell_measurement_reflns_used    6260
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.12
_cell_measurement_theta_min      4.45
_cell_volume                     1902.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9471
_diffrn_reflns_theta_full        55.00
_diffrn_reflns_theta_max         65.12
_diffrn_reflns_theta_min         3.67
_exptl_absorpt_coefficient_mu    1.877
_exptl_absorpt_correction_T_max  0.8345
_exptl_absorpt_correction_T_min  0.5762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                4762
_reflns_number_total             5127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909571z_si_001.cif
_cod_data_source_block           yu14
_cod_database_code               4101799