10,11-Dibromo-3,6-ditosyl-3,6-diazabicyclo[6.4.0]dodeca-1(8),9,11-triene
Şamil Işık; Sema Öztürk; Hoong-Kun Fun; Erbil Ag̃ar; Selami Şaşmaz; Acta Crystallographica Section C 55 (1999) 1850–1852; doi:10.1107/S0108270199010136

data_2009122
_publ_section_title
;
 10,11-Dibromo-3,6-ditosyl-3,6-diazabicyclo[6.4.0]dodeca-1(8),9,11-triene
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1850
_journal_page_last               1852
_journal_paper_doi               10.1107/S0108270199010136
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C24 H24 Br2 N2 O4 S2'
_chemical_formula_weight         628.39
_chemical_name_systematic
;
10,11-Dibromo-3,6-ditosyl-3,6-diazabicyclo[6.4.0]dodeca-1(8),9,11-triene
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.44750(10)
_cell_length_b                   10.44750(10)
_cell_length_c                   22.8183(2)
_cell_measurement_reflns_used    7264
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.20
_cell_measurement_theta_min      2.64
_cell_volume                     2490.62(4)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1995)'
_computing_publication_material  'SHELXTL and PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\w scans'
_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  0.068
_diffrn_reflns_av_sigmaI/netI    0.068
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22912
_diffrn_reflns_theta_full        33.18
_diffrn_reflns_theta_max         33.18
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    3.46
_exptl_absorpt_correction_T_max  0.501
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_type   'empirical using SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.34
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.003(8)
_refine_ls_extinction_coef       0.0001(5)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4721
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.128
_refine_ls_R_factor_gt           0.060
_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^)+(0.0464P)^2^+3.5783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.141
_reflns_number_gt                2635
_reflns_number_total             4721
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fr1214.cif
_cod_data_source_block           I
_cod_database_code               2009122