10,13-Bis(<i>p</i>-tolylsulfonyl)-1,4,7-trithia-10,13-diazacyclopentadecane
Blake, Alexander J.; Lippolis, Vito; Schröder, Martin; Acta Crystallographica Section E 60 (2004) o901–o903; doi:10.1107/S1600536804009201

data_2203693
_publ_section_title
;
 10,13-Bis(<i>p</i>-tolylsulfonyl)-1,4,7-trithia-10,13-diazacyclopentadecane
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o901
_journal_page_last               o903
_journal_paper_doi               10.1107/S1600536804009201
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C24 H34 N2 O4 S5'
_chemical_formula_moiety         'C24 H34 N2 O4 S5'
_chemical_formula_sum            'C24 H34 N2 O4 S5'
_chemical_formula_weight         574.83
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.377(3)
_cell_length_b                   12.377(3)
_cell_length_c                   18.2960(10)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      10.1
_cell_volume                     2802.8(10)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe & Cie, 1997)'
_computing_data_reduction        'X-RED  (Stoe, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material
'enCIFer (Allen et al., 2004) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       \w
_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  0.115
_diffrn_reflns_av_sigmaI/netI    0.068
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3449
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.1
_diffrn_reflns_theta_min         2.6
_diffrn_standards_decay_%        7.4
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.45
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.20
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         1491
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.129
_refine_ls_R_factor_gt           0.070
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.017P)^2^+7.15P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.117
_refine_ls_wR_factor_ref         0.149
_reflns_number_gt                911
_reflns_number_total             1491
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ya6205.cif
_cod_data_source_block           I
_cod_database_code               2203693
_cod_database_fobs_code          2203693