Diastereotopic group selective intramolecular cycloadditions of sulfenic acids to 1,4-dienes.
Grainger, Richard S.; Tisselli, Patrizia; Steed, Jonathan W.; Organic & biomolecular chemistry 2 (2004) 151–153; doi:10.1039/b314176d

data_7150334
_publ_section_title
;
 Diastereotopic group selective intramolecular cycloadditions of
 sulfenic acids to 1,4-dienes.
;
_journal_issue                   2
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              151
_journal_page_last               153
_journal_paper_doi               10.1039/b314176d
_journal_volume                  2
_journal_year                    2004
_chemical_formula_sum            'C9 H15 O2.5 S'
_chemical_formula_weight         195.27
_chemical_name_common            pt062a
_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                109.079(2)
_cell_angle_beta                 92.0540(10)
_cell_angle_gamma                100.681(2)
_cell_formula_units_Z            4
_cell_length_a                   7.1304(3)
_cell_length_b                   10.9979(4)
_cell_length_c                   13.4699(6)
_cell_measurement_temperature    120(2)
_cell_volume                     975.68(7)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.590
_diffrn_measured_fraction_theta_max 0.590
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3808
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.9429
_exptl_absorpt_correction_T_min  0.7967
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0251P)^2^+0.6204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                2203
_reflns_number_total             2637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b314176d.txt
_cod_data_source_block           PT062A.CIF
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C9 H15 O2.50 S'
_cod_database_code               7150334