Gold(i)-catalyzed asymmetric [3 + 2]-cycloadditions of γ-1-ethoxyethoxy-propiolates and aldehydes
Liu, Feng; Wang, Yidong; Ye, Weiming; Zhang, Junliang; Organic Chemistry Frontiers 2 (2015) 221–; doi:10.1039/C4QO00261J

data_1553040
_publ_section_title
;
 Gold(i)-catalyzed asymmetric [3 + 2]-cycloadditions of
 \g-1-ethoxyethoxy-propiolates and aldehydes
;
_journal_issue                   3
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              221
_journal_paper_doi               10.1039/C4QO00261J
_journal_volume                  2
_journal_year                    2015
_chemical_formula_sum            'C27 H31 N O6 S'
_chemical_formula_weight         497.59
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-02-26 deposited with the CCDC.
2015-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.251(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.2388(11)
_cell_length_b                   14.6418(8)
_cell_length_c                   20.7375(12)
_cell_measurement_temperature    296(2)
_cell_volume                     5537.9(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1230
_diffrn_reflns_av_sigmaI/netI    0.1520
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65292
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.9666
_exptl_absorpt_correction_T_min  0.9319
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1261
_refine_ls_number_reflns         19094
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.2011
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0543P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                7917
_reflns_number_total             19094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qo00261j2.cif
_cod_data_source_block           z
_cod_database_code               1553040