5,6,7,8,9,10-Hexahydro-10-hydroxy-5,9-methano-4<i>H</i>-thieno[3,2-<i>c</i>]azonine
Kozísek, J.; Berkes, D.; Svoboda, I.; Decroix, B.; Acta Crystallographica Section C 52 (1996) 1825–1826; doi:10.1107/S0108270196002612

data_2005152
_publ_section_title
5,6,7,8,9,10-Hexahydro-10-hydroxy-5,9-methano-4<i>H</i>-thieno[3,2-<i>c</i>]azonine
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1825
_journal_page_last               1826
_journal_paper_doi               10.1107/S0108270196002612
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          'C11 H15 N1 O1 S1'
_chemical_formula_moiety         'C11 H15 N1 O1 S1'
_chemical_formula_sum            'C11 H15 N O S'
_chemical_formula_weight         209.30
_chemical_name_systematic
;
4,5,6,7,8,9-Hexahydro-10-hydroxy-5,9-methano-4H-thieno[3,2-c]azonine,
C~11~H~15~NOS
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 109.400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.150(3)
_cell_length_b                   6.257(2)
_cell_length_c                   12.433(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      4.4
_cell_volume                     1038.3(4)
_computing_cell_refinement       SDP-Plus
_computing_data_collection       'SDP-Plus (Frenz, 1985)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1971)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2880
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.277
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.16
_refine_ls_extinction_coef       0.020(2)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.082
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment
'H14 refined freely, others refined as riding on their associated C atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_obs          0.0305
_refine_ls_shift/esd_max         -0.090
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0358P)^2^ + 0.4479P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0831
_refine_ls_wR_factor_obs         0.0812
_reflns_number_observed          1351
_reflns_number_total             1442
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            mu1226.cif
_cod_data_source_block           koz11
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2005152