(5<i>S</i>,11a<i>S</i>)-5-Hydroperoxy-1,5,11,11a-tetrahydro[1]benzothieno[3,2-<i>f</i>]indolizin-3(2<i>H</i>)-one
Vrábel, Viktor; Švorc, Ľubomír; Marchalín, Štefan; Šafář, Peter; Acta Crystallographica Section E 68 (2012) o3327–o3328; doi:10.1107/S1600536812045394

data_2236805
_publ_section_title
;
 (5<i>S</i>,11a<i>S</i>)-5-Hydroperoxy-1,5,11,11a-tetrahydro[1]benzothieno[3,2-<i>f</i>]indolizin-3(2<i>H</i>)-one
;
_journal_coeditor_code           BG2481
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3327
_journal_page_last               o3328
_journal_paper_doi               10.1107/S1600536812045394
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C14 H13 N O3 S'
_chemical_formula_moiety         'C14 H13 N O3 S'
_chemical_formula_sum            'C14 H13 N O3 S'
_chemical_formula_weight         275.31
_chemical_name_systematic
;
(5<i>S</i>,11a<i>S</i>)-5-Hydroperoxy-1,5,11,11a-
tetrahydro[1]benzothieno[3,2-<i>f</i>]indolizin-3(2<i>H</i>)-one
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 99.458(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8040(5)
_cell_length_b                   7.9800(4)
_cell_length_c                   10.2903(5)
_cell_measurement_reflns_used    10799
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.5813
_cell_measurement_theta_min      3.2426
_cell_volume                     632.13(6)
_computing_cell_refinement
'<i>CrysAlis CCD</i> (Oxford Diffraction, 2009)'
_computing_data_collection
'<i>CrysAlis CCD</i> (Oxford Diffraction, 2009)'
_computing_data_reduction
'<i>CrysAlis RED</i> (Oxford Diffraction, 2009)'
_computing_molecular_graphics
;
DIAMOND, (Brandenburg, 2001), <i>PLATON</i> (Spek, 2009)
and <i>WinGX</i>
(Farrugia, 1999)
;
_computing_publication_material  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.4340
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur (Ruby, Gemi)'
_diffrn_measurement_method       '\w 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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21595
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         4.39
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis RED (Oxford Diffraction, 2009), based on expressions derived
by
Clark & Reid (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.126
_refine_diff_density_min         -0.137
_refine_ls_abs_structure_details 'Flack (1983), 1185 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.05(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2555
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0441P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                2162
_reflns_number_total             2555
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg2481.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2236805
_cod_database_fobs_code          2236805