17,18-Dibromo-8-methyl-4,12-ditosyl-3,4,5,6,7,8,9,10,11,12,13,14-dodecahydro-2<i>H</i>-benzo[<i>b</i>][1,4,7,11,15]dioxatriazacycloheptadecine
Keleşoğlu, Zeynep; Çelenk Kaya, Elif; Kantekin, Halit; Büyükgüngör, Orhan; Acta Crystallographica Section E 66 (2010) o1082–; doi:10.1107/S1600536810013097

data_2225868
_publ_section_title
;
 17,18-Dibromo-8-methyl-4,12-ditosyl-3,4,5,6,7,8,9,10,11,12,13,14-dodecahydro-2<i>H</i>-benzo[<i>b</i>][1,4,7,11,15]dioxatriazacycloheptadecine
;
_journal_coeditor_code           HB5401
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1082
_journal_paper_doi               10.1107/S1600536810013097
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C31 H39 Br2 N3 O6 S2'
_chemical_formula_moiety         'C31 H39 Br2 N3 O6 S2'
_chemical_formula_sum            'C31 H39 Br2 N3 O6 S2'
_chemical_formula_weight         773.59
_chemical_name_systematic
;
17,18-Dibromo-8-methyl-4,12-ditosyl-3,4,5,6,7,8,9,10,11,12,13,14-
dodecahydro-2<i>H</i>-benzo[b][1,4,7,11,15]dioxatriazacycloheptadecine
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.416(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7520(9)
_cell_length_b                   10.6864(4)
_cell_length_c                   19.9527(9)
_cell_measurement_reflns_used    22517
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      1.21
_cell_volume                     3412.2(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24321
_diffrn_reflns_theta_full        26.76
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    2.544
_exptl_absorpt_correction_T_max  0.425
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.312
_refine_diff_density_min         -1.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0629P)^2^+3.5929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                4640
_reflns_number_total             7243
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5401.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2225868
_cod_database_fobs_code          2225868