The diene-transmissive hetero-Diels-Alder reaction of 2-vinyl α,β-unsaturated aldimines: stereoselective synthesis of hexahydroquinazolin-2-ones.
Kobayashi, Satoru; Kudo, Kenji; Ito, Ai; Hirama, Satoru; Otani, Takashi; Saito, Takao; Organic & biomolecular chemistry 12 (2014) 4061–4064; doi:10.1039/c4ob00224e

data_7153743
_publ_section_title
;
 The diene-transmissive hetero-Diels-Alder reaction of 2-vinyl
 \a,\b-unsaturated aldimines: stereoselective synthesis of
 hexahydroquinazolin-2-ones.
;
_journal_issue                   24
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4061
_journal_page_last               4064
_journal_paper_doi               10.1039/c4ob00224e
_journal_volume                  12
_journal_year                    2014
_chemical_formula_sum            'C36 H34 N2 O4 S'
_chemical_formula_weight         590.71
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                73.96(3)
_cell_angle_beta                 81.78(3)
_cell_angle_gamma                81.29(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9250(16)
_cell_length_b                   11.508(2)
_cell_length_c                   17.714(4)
_cell_measurement_temperature    173(2)
_cell_volume                     1526.0(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8416
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.9497
_exptl_absorpt_correction_type   analytical
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1643
_reflns_number_gt                4747
_reflns_number_total             6503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ob00224e2.cif
_cod_data_source_block           ydkr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7153743.cif.
;
_cod_original_cell_volume        1526.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7153743