A thiophene-based azacryptand Mannich base: 18,24-bis(<i>p</i>-tolylsulfonamido)-2,5,8,11,21-pentaoxa-15,27-dithia-18,24-diazatricyclo[24.3.0.0]nonacosa-1(26),12(16),13,28-tetraene
Gaël Labat; Joan Halfpenny; Acta Crystallographica Section E 62 (2006) o3087–o3089; doi:10.1107/S1600536806024317

data_2209622
_publ_section_title
;A thiophene-based azacryptand Mannich base:
 18,24-bis(<i>p</i>-tolylsulfonamido)-2,5,8,11,21-pentaoxa-15,27-dithia-18,24-diazatricyclo[24.3.0.0]nonacosa-1(26),12(16),13,28-tetraene
;
_journal_coeditor_code           OB2031
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3087
_journal_page_last               o3089
_journal_paper_doi               10.1107/S1600536806024317
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C34 H42 N2 O9 S4'
_chemical_formula_moiety         'C34 H42 N2 O9 S4'
_chemical_formula_sum            'C34 H42 N2 O9 S4'
_chemical_formula_weight         750.94
_chemical_name_systematic
;
18,24-bis(p-tolylsulfonamide)-2,5,8,11,21-pentaoxa-15,27-dithia-18,24-
diazatricyclo[24.3.0.0]nonacosa-1(26),12(16),13,28-tetraene
;
_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                 105.619(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2875(13)
_cell_length_b                   9.0910(5)
_cell_length_c                   22.6813(17)
_cell_measurement_reflns_used    8001
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     3631.6(5)
_computing_cell_refinement       IPDS-I
_computing_data_collection       'IPDS-I (Stoe & Cie, 2000)'
_computing_data_reduction        IPDS-I
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f oscillation'
_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  0.1156
_diffrn_reflns_av_sigmaI/netI    0.0868
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27910
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.426
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.876
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                4692
_reflns_number_total             7077
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob2031.cif
_cod_data_source_block           I
_cod_original_cell_volume        3631.6(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2209622
_cod_database_fobs_code          2209622