Pd/Josiphos-Catalyzed Enantioselective α-Arylation of Silyl Ketene Acetals and Mechanistic Studies on Transmetalation and Enantioselection
Kobayashi, Kenya; Yamamoto, Yasunori; Miyaura, Norio; Organometallics 30 (2011) 6323–; doi:10.1021/om200945q

data_4065543
_publ_section_title
;
 Pd/Josiphos-Catalyzed Enantioselective \a-Arylation of Silyl Ketene
 Acetals and Mechanistic Studies on Transmetalation and Enantioselection
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6323
_journal_paper_doi               10.1021/om200945q
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C49 H64 Cl4 Fe O2 P2 Pd'
_chemical_formula_sum            'C49 H64 Cl4 Fe O2 P2 Pd'
_chemical_formula_weight         1051.05
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 108.6200(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   11.0323(5)
_cell_length_b                   18.9610(7)
_cell_length_c                   12.4461(5)
_cell_measurement_reflns_used    17222
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.04
_cell_volume                     2467.24(18)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla, et al., 2003)'
_diffrn_ambient_temperature      213
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23919
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088.00
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.159
_refine_diff_density_max         1.680
_refine_diff_density_min         -1.560
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  5377 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     533
_refine_ls_number_reflns         11163
_refine_ls_number_restraints     6
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0066P)^2^+6.9478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                6990
_reflns_number_total             11163
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om200945q_si_001.cif
_cod_data_source_block           kobayashi20110221
_cod_original_cell_volume        2467.24(16)
_cod_database_code               4065543