(6<i>R</i>*,16<i>R</i>*)-9,14-Dihydro-6-methyl-6,16-methano-6<i>H</i>,16<i>H</i>-[2,4]benzothiazepino[3,4-<i>d</i>][1,3,5]benzoxadiazocine hydrobromide dimethylformamide hemisolvate
Kettmann, Viktor; Svetlik, Jan; Acta Crystallographica Section C 56 (2000) 1115–1116; doi:10.1107/S0108270100006727

data_2011379
_publ_section_title
;(6<i>R</i>*,16<i>R</i>*)-9,14-Dihydro-6-methyl-6,16-methano-6<i>H</i>,16<i>H</i>-[2,4]benzothiazepino[3,4-<i>d</i>][1,3,5]benzoxadiazocine
 hydrobromide dimethylformamide hemisolvate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1115
_journal_page_last               1116
_journal_paper_doi               10.1107/S0108270100006727
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          'C19 H19 N2 O S , Br , 0.5C3 H7 N O'
_chemical_formula_moiety         'C19 H19 N2 O S , Br , 0.5C3 H7 N O'
_chemical_formula_structural     'C19 H19 N2 O S+ , Br- , 0.5C3 H7 N O'
_chemical_formula_sum            'C20.5 H22.5 Br N2.5 O1.5 S'
_chemical_formula_weight         439.89
_chemical_melting_point          511
_chemical_name_systematic
;
(6R*,16R*)-9,14-Dihydro-6-methyl-6,16-methano-6H,16H-[2,4]benzo-
thiazepino[3,4-d][1,3,5]benzoxadiazocine hydrobromide 0.5 dimethylformamide
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.94(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.612(8)
_cell_length_b                   19.807(9)
_cell_length_c                   11.087(5)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      10
_cell_volume                     4065(3)
_computing_cell_refinement       'Syntex P2~1~ diffractometer software '
_computing_data_collection       'Syntex P2~1~ diffractometer software '
_computing_data_reduction        'XP21 (Pavel\<c\'ik, 1987)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976) '
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Syntex P2~1~ '
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .024
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7534
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_T_max  .810
_exptl_absorpt_correction_T_min  .495
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_meas      1.440(10)
_exptl_crystal_density_method    'flotation in bromoform/c-hexane '
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .10
_refine_diff_density_max         .39
_refine_diff_density_min         -.31
_refine_ls_extinction_coef       .0017(3)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   .896
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .896
_refine_ls_R_factor_all          .181
_refine_ls_R_factor_gt           .063
_refine_ls_shift/su_max          .002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0758P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .157
_reflns_number_gt                3573
_reflns_number_total             7166
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1354.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C20.5 H22.5 Br1 N2.5 O1.5 S1 '
_cod_database_code               2011379
_cod_database_fobs_code          2011379