Cu(I) Tol-BINAP-Catalyzed Enantioselective Michael Reactions of Grignard Reagents and Unsaturated Esters
Shun-Yi Wang; Shun-Jun Ji; Teck-Peng Loh; Journal of the American Chemical Society 129 (2007) 276–277; doi:10.1021/ja0666046

data_4108972
_publ_section_title
;
 Cu(I) Tol-BINAP-Catalyzed Enantioselective Michael Reactions of Grignard
 Reagents and Unsaturated Esters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              276
_journal_page_last               277
_journal_paper_doi               10.1021/ja0666046
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C96 H80 Cu2 I2 P4'
_chemical_formula_weight         1738.36
_chemical_name_systematic
;

 ?

;
_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                 90.9600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6499(3)
_cell_length_b                   14.5155(3)
_cell_length_c                   19.1630(4)
_cell_measurement_reflns_used    9526
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     4074.45(15)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            111660
_diffrn_reflns_theta_full        30.74
_diffrn_reflns_theta_max         30.74
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  0.9725
_exptl_absorpt_correction_T_min  0.7665
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         24074
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                15554
_reflns_number_total             24074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0666046si20060913_062242.cif
_cod_data_source_block           ltp10a
_cod_database_code               4108972