Diastereoselectivity Switch in Cooperatively Catalyzed Three-Component Reactions of an Aryldiazoacetate, an Alcohol, and a β,γ-Unsaturated α-Keto Ester
Jingjing Ji; Xia Zhang; Yingguang Zhu; Yu Qian; Jing Zhou; Liping Yang; Wenhao Hu; Journal of Organic Chemistry 76 (2011) 5821–5824; doi:10.1021/jo102423c

data_4026449
_publ_section_title
;
 Diastereoselectivity Switch in Cooperatively Catalyzed Three-Component
 Reactions of an Aryldiazoacetate, an Alcohol, and a \b,\g-Unsaturated
 \a-Keto Ester
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5821
_journal_page_last               5824
_journal_paper_doi               10.1021/jo102423c
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C28 H27 Cl O7'
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.5550(10)
_cell_angle_beta                 100.8540(10)
_cell_angle_gamma                98.8340(10)
_cell_formula_units_Z            2
_cell_length_a                   7.0490(3)
_cell_length_b                   10.2248(4)
_cell_length_c                   17.5540(7)
_cell_measurement_temperature    173(2)
_cell_volume                     1214.41(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_T_max  0.9448
_exptl_absorpt_correction_T_min  0.9134
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4253
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_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0339
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_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^)+(0.0385P)^2^+0.4762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           z
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