#------------------------------------------------------------------------------ #$Date: 2008-04-05 09:13:02 +0100 (Sat, 05 Apr 2008) $ #$Revision: 340 $ #$URL: svn://www.crystallography.net/cod/cif/2/2102050.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2102050 loop_ _publ_author_name 'Nagel, Norbert' 'Bock, Hans' 'Eller, Peter' _publ_section_title ; Dimorphism and inclusion compounds of N,N'-di(benzenesulfonyl)-p-phenylenediamine ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 234 _journal_page_last 244 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac 'C18 H16 N2 O4 S2,C O (C H3)2' _chemical_formula_moiety 'C18 H16 N2 O4 S2,C3 H6 O' _chemical_formula_sum 'C21 H22 N2 O5 S2' _chemical_formula_weight 446.53 _chemical_name_systematic ; ? ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M Pbcn _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.503(2) _cell_length_b 7.7310(9) _cell_length_c 15.188(2) _cell_measurement_reflns_used 90 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 19 _cell_measurement_theta_min 10 _cell_volume 2055.1(4) _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measurement_device 'Siemens P4 four circle' _diffrn_measurement_method '\w scan' _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 .0202 _diffrn_reflns_av_sigmaI/netI .0268 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 2658 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.33 _diffrn_standards_interval_count 100 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu .296 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.443 _exptl_crystal_description block _exptl_crystal_F_000 936 _exptl_crystal_size_max .70 _exptl_crystal_size_mid .65 _exptl_crystal_size_min .40 _refine_diff_density_max .386 _refine_diff_density_min -.331 _refine_ls_extinction_coef .0071(7) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_matrix_type full _refine_ls_number_parameters 144 _refine_ls_number_reflns 2013 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.055 _refine_ls_restrained_S_obs 1.072 _refine_ls_R_factor_all .0595 _refine_ls_R_factor_obs .0422 _refine_ls_shift/esd_max .000 _refine_ls_shift/esd_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+2.2606P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all .1136 _refine_ls_wR_factor_obs .1007 _reflns_number_observed 1564 _reflns_number_total 2016 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file se0270.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol S1 .16553(3) .14541(7) .50034(4) .0244(2) Uani d . 1 . S O1 .24182(9) .1232(2) .46828(12) .0342(4) Uani d . 1 . O O2 .10893(9) .0208(2) .47845(11) .0313(4) Uani d . 1 . O N1 .13919(10) .3334(2) .46212(13) .0224(4) Uani d . 1 . N H1N .1759(14) .401(3) .4564(16) .024(7) Uiso d . 1 . H C1 .06814(11) .4140(3) .48302(13) .0201(4) Uani d . 1 . C C2 .06696(12) .5911(3) .4939(2) .0257(5) Uani d . 1 . C H2 .11325(12) .6547(3) .4896(2) .031 Uiso calc R 1 . H C3 .00039(13) .3229(3) .4891(2) .0280(5) Uani d . 1 . C H3 .00027(13) .2009(3) .4816(2) .034 Uiso calc R 1 . H C10 .16958(14) .1617(3) .6154(2) .0310(6) Uani d . 1 . C C11 .1123(2) .0894(4) .6663(2) .0403(6) Uani d . 1 . C H11 .0704(2) .0321(4) .6394(2) .048 Uiso calc R 1 . H C12 .1170(2) .1018(4) .7566(2) .0561(9) Uani d . 1 . C H12 .0780(2) .0535(4) .7925(2) .067 Uiso calc R 1 . H C13 .1782(2) .1838(4) .7948(2) .0636(10) Uani d . 1 . C H13 .1814(2) .1909(4) .8572(2) .076 Uiso calc R 1 . H C14 .2345(2) .2552(4) .7444(2) .0612(10) Uani d . 1 . C H14 .2762(2) .3126(4) .7718(2) .073 Uiso calc R 1 . H C15 .2311(2) .2443(4) .6536(2) .0451(7) Uani d . 1 . C H15 .2704(2) .2929(4) .6181(2) .054 Uiso calc R 1 . H C20 .5000 .1442(4) .7500 .0374(9) Uani d SD 1 . C O3 .5259(7) .2894(11) .7307(8) .043(2) Uiso d PD .25 1 O C21 .4197(3) .1024(8) .7301(4) .0487(14) Uiso d PD .50 1 C H21A .4085(3) -.0160(8) .7493(4) .073 Uiso calc PR .50 1 H H21B .4110(3) .1120(8) .6665(4) .073 Uiso calc PR .50 1 H H21C .3861(3) .1834(8) .7612(4) .073 Uiso calc PR .50 1 H O3' .4786(7) .2927(11) .7365(8) .046(3) Uiso d PD .25 2 O C21' .4481(4) -.0029(9) .7343(5) .062(2) Uiso d PD .50 2 C H21D .4780(4) -.1093(9) .7281(5) .093 Uiso calc PR .50 2 H H21E .4189(4) .0174(9) .6801(5) .093 Uiso calc PR .50 2 H H21F .4128(4) -.0144(9) .7840(5) .093 Uiso calc PR .50 2 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 .0180(3) .0195(3) .0356(3) .0028(2) .0004(2) -.0003(2) O1 .0191(8) .0290(8) .0544(10) .0058(7) .0052(8) -.0013(8) O2 .0242(8) .0228(8) .0467(10) -.0009(7) .0012(7) -.0054(7) N1 .0142(9) .0215(9) .0314(10) -.0006(8) .0015(8) .0038(8) C1 .0154(10) .0226(10) .0222(10) .0023(8) -.0003(8) .0028(8) C2 .0145(10) .0228(11) .0399(13) -.0030(8) .0008(9) .0028(10) C3 .0211(11) .0186(10) .0441(14) -.0011(9) -.0010(10) -.0006(10) C10 .0355(13) .0230(11) .0345(13) .0035(10) -.0060(11) .0065(10) C11 .0404(15) .0383(14) .0424(15) .0006(12) -.0027(12) .0119(12) C12 .069(2) .055(2) .044(2) .001(2) -.001(2) .018(2) C13 .102(3) .052(2) .036(2) .001(2) -.020(2) .0156(14) C14 .087(3) .046(2) .051(2) -.011(2) -.030(2) .008(2) C15 .051(2) .0332(14) .051(2) -.0082(13) -.0154(14) .0097(13) C20 .047(2) .024(2) .042(2) .000 -.002(2) .000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance S1 O2 . 1.421(2) S1 O1 . 1.432(2) S1 N1 . 1.631(2) S1 C10 . 1.754(3) N1 C1 . 1.427(3) C1 C2 . 1.379(3) C1 C3 . 1.382(3) C2 C3 5_566 1.378(3) C3 C2 5_566 1.378(3) C10 C15 . 1.380(4) C10 C11 . 1.383(4) C11 C12 . 1.377(4) C12 C13 . 1.373(5) C13 C14 . 1.365(5) C14 C15 . 1.383(4) C20 O3' 3_656 1.225(9) C20 O3' . 1.225(9) C20 O3 . 1.246(9) C20 O3 3_656 1.246(9) C20 C21 . 1.474(6) C20 C21 3_656 1.474(6) C20 C21' . 1.475(7) C20 C21' 3_656 1.475(7) O3 O3 3_656 1.08(2) O3 C21 3_656 1.831(13) O3' O3' 3_656 .85(2) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O2 S1 O1 . . 119.30(10) O2 S1 N1 . . 108.87(10) O1 S1 N1 . . 104.44(10) O2 S1 C10 . . 108.05(11) O1 S1 C10 . . 108.06(11) N1 S1 C10 . . 107.59(11) C1 N1 S1 . . 123.8(2) C2 C1 C3 . . 119.0(2) C2 C1 N1 . . 118.2(2) C3 C1 N1 . . 122.7(2) C3 C2 C1 5_566 . 121.0(2) C2 C3 C1 5_566 . 120.0(2) C15 C10 C11 . . 121.2(3) C15 C10 S1 . . 118.9(2) C11 C10 S1 . . 119.9(2) C12 C11 C10 . . 119.0(3) C13 C12 C11 . . 120.0(3) C14 C13 C12 . . 120.9(3) C13 C14 C15 . . 120.2(3) C10 C15 C14 . . 118.7(3) O3' C20 O3' 3_656 . 40.7(9) O3 C20 O3 . 3_656 51.4(10) O3 C20 C21 . . 119.8(7) O3 C20 C21 3_656 . 84.2(6) O3 C20 C21 . 3_656 84.2(6) O3 C20 C21 3_656 3_656 119.8(7) C21 C20 C21 . 3_656 154.7(6) O3' C20 C21' 3_656 . 159.7(7) O3' C20 C21' . . 120.5(6) O3' C20 C21' 3_656 3_656 120.5(6) O3' C20 C21' . 3_656 159.7(7) C21' C20 C21' . 3_656 79.1(6) O3 O3 C20 3_656 . 64.3(5) O3 O3 C21 3_656 3_656 105.1(9) C20 O3 C21 . 3_656 53.2(4) O3' O3' C20 3_656 . 69.6(5) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion O2 S1 N1 C1 . . 56.0(2) O1 S1 N1 C1 . . -175.5(2) C10 S1 N1 C1 . . -60.8(2) S1 N1 C1 C2 . . 142.8(2) S1 N1 C1 C3 . . -40.0(3) C3 C1 C2 C3 . 5_566 .2(4) N1 C1 C2 C3 . 5_566 177.6(2) C2 C1 C3 C2 . 5_566 -.2(4) N1 C1 C3 C2 . 5_566 -177.4(2) O2 S1 C10 C15 . . 165.7(2) O1 S1 C10 C15 . . 35.3(2) N1 S1 C10 C15 . . -76.9(2) O2 S1 C10 C11 . . -13.2(2) O1 S1 C10 C11 . . -143.5(2) N1 S1 C10 C11 . . 104.2(2) C15 C10 C11 C12 . . .4(4) S1 C10 C11 C12 . . 179.2(2) C10 C11 C12 C13 . . -.5(5) C11 C12 C13 C14 . . .6(5) C12 C13 C14 C15 . . -.7(5) C11 C10 C15 C14 . . -.5(4) S1 C10 C15 C14 . . -179.3(2) C13 C14 C15 C10 . . .6(5) O3' C20 O3 O3 3_656 3_656 -50.0(18) O3' C20 O3 O3 . 3_656 28.8(9) O3 C20 O3 O3 3_656 3_656 .000(3) C21 C20 O3 O3 . 3_656 52.6(15) C21 C20 O3 O3 3_656 3_656 -136.1(13) C21' C20 O3 O3 . 3_656 83.6(17) C21' C20 O3 O3 3_656 3_656 -146.9(10) O3' C20 O3 C21 3_656 3_656 86(3) O3' C20 O3 C21 . 3_656 164.9(14) O3 C20 O3 C21 3_656 3_656 136.1(13) C21 C20 O3 C21 . 3_656 -171.3(3) C21 C20 O3 C21 3_656 3_656 .0 C21' C20 O3 C21 . 3_656 -140.3(12) C21' C20 O3 C21 3_656 3_656 -10.8(6) O3' C20 O3' O3' 3_656 3_656 .000(4) O3 C20 O3' O3' . 3_656 -36.9(11) O3 C20 O3' O3' 3_656 3_656 73(2) C21 C20 O3' O3' . 3_656 163.8(19) C21 C20 O3' O3' 3_656 3_656 -19(2) C21' C20 O3' O3' . 3_656 169.7(15) C21' C20 O3' O3' 3_656 3_656 -26(4)