1-(8-Bromo-2-methyl-4-thioxo-3,4,5,6-tetrahydro-2<i>H</i>-2,6-methano-1,3-benzoxazocin-11-yl)ethanone
Palamarchuk, G. V.; Borisov, O. V.; Kovalenko, S. S.; Chernykh, V. P.; Kovalenko, S. M.; Baumer, V. N.; Shishkin, O. V.; Acta Crystallographica Section E 65 (2009) o461–; doi:10.1107/S160053680900347X

data_2220972
_publ_section_title
1-(8-Bromo-2-methyl-4-thioxo-3,4,5,6-tetrahydro-2<i>H</i>-2,6-methano-1,3-benzoxazocin-11-yl)ethanone
_journal_coeditor_code           BG2221
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o461
_journal_paper_doi               10.1107/S160053680900347X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C14 H14 Br N O2 S'
_chemical_formula_moiety         'C14 H14 Br N O2 S'
_chemical_formula_sum            'C14 H14 Br N O2 S'
_chemical_formula_weight         340.23
_chemical_name_systematic
;
1-(8-Bromo-2-methyl-4-thioxo-3,4,5,6-tetrahydro-2<i>H</i>-2,6-methano-1,3-
benzoxazocin-11-yl)ethanone
;
_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           SHELXL97
_cell_angle_alpha                98.67(5)
_cell_angle_beta                 99.09(5)
_cell_angle_gamma                101.81(5)
_cell_formula_units_Z            4
_cell_length_a                   8.213(5)
_cell_length_b                   11.625(7)
_cell_length_c                   15.156(10)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1373.3(16)
_computing_cell_refinement       'P3 (Siemens, 1991)'
_computing_data_collection       'P3 (Siemens, 1991)'
_computing_data_reduction        'XDISK and XPREP (Siemens, 1991)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Siemens P3/PC'
_diffrn_measurement_method       2\q/\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7869
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.142
_exptl_absorpt_correction_T_max  0.8550
_exptl_absorpt_correction_T_min  0.6112
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(XPREP; Siemens, 1991)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.427
_refine_ls_extinction_coef       0.0026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.9457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                3383
_reflns_number_total             4773
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            bg2221.cif
_cod_data_source_block           I
_cod_original_cell_volume        1373.1(15)
_cod_database_code               2220972
_cod_database_fobs_code          2220972