Cross-Diels-Alder Reactions of 6-Oxo-1-Sulfonyl-1,6-Dihydropyridine-3-Carboxylates
Marie-Laure Teyssot; Anh-Tuan Lormier; Isabelle Chataigner; Serge R. Piettre; Journal of Organic Chemistry 72 (2007) 2364–2373; doi:10.1021/jo062186b

data_4022695
_publ_section_title
;
 Cross-Diels-Alder Reactions of
 6-Oxo-1-Sulfonyl-1,6-Dihydropyridine-3-Carboxylates
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2364
_journal_page_last               2373
_journal_paper_doi               10.1021/jo062186b
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C27 H37 N O9 S Si'
_chemical_formula_sum            'C27 H37 N O9 S Si'
_chemical_formula_weight         579.73
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 105.3770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.8232(13)
_cell_length_b                   8.6831(4)
_cell_length_c                   27.9690(14)
_cell_measurement_temperature    296(2)
_cell_volume                     6046.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            23572
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Saint+ V6.02)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.130
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^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         0.1224
_reflns_number_gt                3994
_reflns_number_total             6184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo062186bsi20061020_023956.cif
_cod_data_source_block           disal3m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4022695