β,γ-Regioselective Inverse-Electron-Demand Aza-Diels-Alder Reactions with α,β-Unsaturated Aldehydes via Dienamine Catalysis.
Gu, Jing; Ma, Chao; Li, Qing-Zhu; Du, Wei; Chen, Ying-Chun; Organic letters 16 (2014) 3986–3989; doi:10.1021/ol501814p

data_1517193
_publ_section_title
;
 \b,\g-Regioselective Inverse-Electron-Demand Aza-Diels-Alder Reactions
 with \a,\b-Unsaturated Aldehydes via Dienamine Catalysis.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              3986
_journal_page_last               3989
_journal_paper_doi               10.1021/ol501814p
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C31 H36 Cl N O6 S2'
_chemical_formula_weight         618.18
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.7416(5)
_cell_length_b                   11.7295(2)
_cell_length_c                   7.44950(10)
_cell_measurement_reflns_used    13786
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      69.9770
_cell_measurement_theta_min      3.7653
_cell_volume                     3035.68(8)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Gemini S Ultra, Agilent Technologies'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            27271
_diffrn_reflns_theta_full        70.11
_diffrn_reflns_theta_max         70.11
_diffrn_reflns_theta_min         3.98
_exptl_absorpt_coefficient_mu    2.765
_exptl_absorpt_correction_T_max  0.4532
_exptl_absorpt_correction_T_min  0.3968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         5651
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.9109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                5417
_reflns_number_total             5651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol501814p_si_002.cif
_cod_data_source_block           3j
_cod_depositor_comments          'Adding full bibliography for 1517193.cif.'
_cod_database_code               1517193