(<i>Z</i>)-2-(Benzo[<i>b</i>]thiophen-3-ylmethylene)-1-azabicyclo[2.2.2]octan-3-one
Sonar, Vijayakumar N.; Parkin, Sean; Crooks, Peter A.; Acta Crystallographica Section E 59 (2003) o1726–o1728; doi:10.1107/S1600536803022797

data_2202871
_publ_section_title
(<i>Z</i>)-2-(Benzo[<i>b</i>]thiophen-3-ylmethylene)-1-azabicyclo[2.2.2]octan-3-one
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1726
_journal_page_last               o1728
_journal_paper_doi               10.1107/S1600536803022797
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C16 H15 N O S'
_chemical_formula_moiety         'C16 H15 N O S'
_chemical_formula_sum            'C16 H15 N O S'
_chemical_formula_weight         269.35
_chemical_name_systematic
;
(Z)-(2-Benzo[b]thiophen-3-ylmethylene)-1-azabicyclo[2.2.2]octan-3-one
;
_space_group_IT_number           1
_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                102.8959(9)
_cell_angle_beta                 94.7214(9)
_cell_angle_gamma                110.2617(10)
_cell_formula_units_Z            1
_cell_length_a                   6.21440(10)
_cell_length_b                   6.80780(10)
_cell_length_c                   8.4492(2)
_cell_measurement_reflns_used    1439
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     321.861(11)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1995)'
_computing_publication_material
;
SHELX97-2 (Sheldrick, 1997) and local procedures
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7534
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.9647
_exptl_absorpt_correction_T_min  0.9311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             142
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.181
_refine_ls_abs_structure_details 'Flack (1983), 1389 Friedel pairs '
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2858
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0582P)^2^+0.0899P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                2811
_reflns_number_total             2858
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6181.cif
_cod_data_source_block           I
_cod_original_cell_volume        321.860(10)
_cod_database_code               2202871
_cod_database_fobs_code          2202871