Direct Catalytic Asymmetric Michael Reaction of Hydroxyketones: Asymmetric Zn Catalysis with a Et2Zn/Linked-BINOL Complex
Shinji Harada; Naoya Kumagai; Tomofumi Kinoshita; Shigeki Matsunaga; Masakatsu Shibasaki; Journal of the American Chemical Society 125 (2003) 2582–2590; doi:10.1021/ja028928+

data_4113519
_publ_section_title
;
 Direct Catalytic Asymmetric Michael Reaction of Hydroxyketones:
 Asymmetric Zn Catalysis with a Et2Zn/Linked-BINOL Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2582
_journal_page_last               2590
_journal_paper_doi               10.1021/ja028928+
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C15 H18 O4 '
_chemical_formula_sum            'C15 H18 O4'
_chemical_formula_weight         262.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 98.839(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1071(8)
_cell_length_b                   12.029(1)
_cell_length_c                   12.839(1)
_cell_measurement_reflns_used    4750
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.6
_cell_volume                     1389.8(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR97
_diffrn_measured_fraction_theta_full 0.9356
_diffrn_measured_fraction_theta_max 0.9356
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5166
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     240
_refine_ls_number_reflns         2980
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.8883
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1525
_reflns_number_gt                1115
_reflns_number_total             2982
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja0289282B-6_s2_1.cif
_cod_data_source_block           020928SH
_cod_original_formula_sum        'C15 H18 O4 '
_cod_database_code               4113519