7-Bromo-4b-methyl-7,8-dihydro-4b<i>H</i>-9-thia-8a-azafluorene 9,9-dioxide
Gallucci, Judith C.; Dura, Robert D.; Paquette, Leo A.; Acta Crystallographica Section E 64 (2008) o1303–; doi:10.1107/S1600536808017972

data_2218798
_publ_section_title
;
 7-Bromo-4b-methyl-7,8-dihydro-4b<i>H</i>-9-thia-8a-azafluorene
 9,9-dioxide
;
_journal_coeditor_code           RT2018
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1303
_journal_paper_doi               10.1107/S1600536808017972
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C12 H12 Br1 N1 O2 S1'
_chemical_formula_moiety         'C12 H12 Br1 N1 O2 S1'
_chemical_formula_sum            'C12 H12 Br N O2 S'
_chemical_formula_weight         314.2
_chemical_name_common            'Paquette 1603'
_chemical_name_systematic
;
7-Bromo-4b-methyl-7,8-dihydro-4b<i>H</i>-9-thia-8a-azafluorene 9,9-dioxide
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.0090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3970(3)
_cell_length_b                   7.89120(10)
_cell_length_c                   11.4652(2)
_cell_measurement_reflns_used    2393
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     1269.13(4)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
;
DENZO (Otwinowski & Minor, 1997) and SCALEPACK (Otwinowski & Minor,
1997)
;
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.677
_diffrn_measured_fraction_theta_max 0.677
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18122
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.9
_exptl_absorpt_coefficient_mu    3.392
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.487
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         1509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.487
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0519P)^2^+1.4699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                2401
_reflns_number_total             2835
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rt2018.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2218798
_cod_database_fobs_code          2218798