Gold catalyzed stereoselective tandem hydroamination-formal aza-Diels-Alder reaction of propargylic amino esters.
Fustero, Santos; Bello, Paula; Miró, Javier; Sánchez-Roselló, María; Maestro, Miguel A.; González, Javier; del Pozo, Carlos; Chemical communications (Cambridge, England) 49 (2013) 1336–1338; doi:10.1039/c2cc37796a

data_7112294
_publ_section_title
;
 Gold catalyzed stereoselective tandem hydroamination-formal
 aza-Diels-Alder reaction of propargylic amino esters.
;
_journal_issue                   13
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1336
_journal_page_last               1338
_journal_paper_doi               10.1039/c2cc37796a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C30 H56 F6 N2 O6'
_chemical_formula_weight         650.74
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.0850(10)
_cell_angle_beta                 68.8250(10)
_cell_angle_gamma                71.2380(10)
_cell_formula_units_Z            4
_cell_length_a                   13.3817(3)
_cell_length_b                   13.4222(3)
_cell_length_c                   18.3938(4)
_cell_measurement_temperature    100(2)
_cell_volume                     2879.44(11)
_computing_cell_refinement       'SAINT V7.12A (Bruker 2004)'
_computing_data_collection       'Apex2 V.1.0-27(Bruker 2005)'
_computing_data_reduction        'SAINT and XPREP Version 6.14, 2003'
_computing_molecular_graphics    'Bruker SHELXTL suite ver. 6.12, 2001'
_computing_publication_material  'Bruker SHELXTL suite ver. 6.12, 2001'
_computing_structure_refinement  'SHELXL-97 in SHELXTL ver. 6.12, 2001'
_computing_structure_solution    'SHELXS-97 in SHELXTL ver. 6.12, 2001'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55997
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_correction_T_min  0.9364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS program multi-scan
Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         14251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0588
_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^)+(0.1176P)^2^+2.0165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1779
_refine_ls_wR_factor_ref         0.1932
_reflns_number_gt                11292
_reflns_number_total             14251
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7108830
_cod_data_source_file            c2cc37796a.txt
_cod_data_source_block           anc1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7112294