#------------------------------------------------------------------------------ #$Date: 2011-04-07 13:48:30 +0300 (Thu, 07 Apr 2011) $ #$Revision: 17414 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2229367.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_2229367 loop_ _publ_author_name 'Bortoluzzi, Adailton J.' 'Policarpi, Everton B.' 'Mora, Cristiano' 'Oliveira, Kely N.' 'Nunes, Ricardo J.' _publ_section_title ; 4-[(1,3-Dioxo-2,3-dihydro-1H-benzo[de]isoquinolin-2-yl)methyl]-N'-[(E)-4-nitrobenzylidene]benzenesulfonohydrazide dimethyl sulfoxide monosolvate ; _journal_coeditor_code FF2001 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o627 _journal_page_last o628 _journal_volume 67 _journal_year 2011 _chemical_formula_iupac 'C26 H18 N4 O6 S, C2 H6 O S' _chemical_formula_moiety 'C26 H18 N4 O6 S, C2 H6 O S' _chemical_formula_sum 'C28 H24 N4 O7 S2' _chemical_formula_weight 592.63 _chemical_name_systematic ; 4-[(1,3-Dioxo-2,3-dihydro-1H-benzo[de]isoquinolin-2-yl)methyl]- N'-[(E)-4-nitrobenzylidene]benzenesulfonohydrazide dimethyl sulfoxide monosolvate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 107.268(7) _cell_angle_beta 101.789(7) _cell_angle_gamma 96.319(8) _cell_formula_units_Z 2 _cell_length_a 9.1520(10) _cell_length_b 11.9710(10) _cell_length_c 13.9100(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 13.41 _cell_measurement_theta_min 8.53 _cell_volume 1400.6(2) _computing_cell_refinement 'CAD-4 Software (Enraf--Nonius, 1989)' _computing_data_collection 'CAD-4 Software (Enraf--Nonius, 1989)' _computing_data_reduction 'HELENA (Spek, 1996)' _computing_molecular_graphics ; PLATON (Spek, 2009) and Mercury (Macrae et al., 2006) ; _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.952 _diffrn_measured_fraction_theta_max 0.952 _diffrn_measurement_device_type 'Enraf--Nonius CAD-4' _diffrn_measurement_method \w--2\q _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 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 5055 _diffrn_reflns_theta_full 25.07 _diffrn_reflns_theta_max 25.07 _diffrn_reflns_theta_min 2.31 _diffrn_standards_decay_% 1 _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.244 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prismatic _exptl_crystal_F_000 616 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.727 _refine_diff_density_min -0.425 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 371 _refine_ls_number_reflns 4737 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0524 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.6130P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1380 _refine_ls_wR_factor_ref 0.1626 _reflns_number_gt 3075 _reflns_number_total 4737 _reflns_threshold_expression I>2sigma(I) _[local]_cod_data_source_file ff2001.cif _[local]_cod_data_source_block I _cod_database_code 2229367 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S S1 0.34031(11) 0.73620(8) 0.53120(6) 0.0597(3) Uani d . 1 . . N N1 0.8354(3) 1.1992(2) 0.8805(2) 0.0571(7) Uani d . 1 . . N N2 0.4477(3) 0.6426(2) 0.55446(19) 0.0540(7) Uani d . 1 . . H H2N 0.5170 0.6398 0.5273 0.058(12) Uiso d R 1 . . N N3 0.4776(3) 0.6399(2) 0.65605(19) 0.0501(6) Uani d . 1 . . O O1 0.6771(4) 1.2526(3) 0.9840(2) 0.1026(11) Uani d . 1 . . O O2 0.9903(3) 1.1379(3) 0.7756(2) 0.0987(10) Uani d . 1 . . O O3 0.3260(3) 0.7192(2) 0.42331(18) 0.0797(8) Uani d . 1 . . O O4 0.2088(3) 0.7188(2) 0.5685(2) 0.0766(8) Uani d . 1 . . C C2 0.7994(4) 1.2237(3) 0.9760(3) 0.0626(9) Uani d . 1 . . C C3 0.9105(4) 1.2127(3) 1.0630(2) 0.0547(8) Uani d . 1 . . C C4 0.8859(5) 1.2441(4) 1.1612(3) 0.0767(11) Uani d . 1 . . H H4 0.7994 1.2747 1.1724 0.092 Uiso calc R 1 . . C C5 0.9881(6) 1.2309(4) 1.2432(3) 0.0864(13) Uani d . 1 . . H H5 0.9706 1.2547 1.3092 0.104 Uiso calc R 1 . . C C6 1.1117(6) 1.1846(4) 1.2296(3) 0.0803(13) Uani d . 1 . . H H6 1.1779 1.1753 1.2858 0.096 Uiso calc R 1 . . C C7 1.1429(4) 1.1495(3) 1.1304(3) 0.0645(10) Uani d . 1 . . C C8 1.2697(5) 1.1010(4) 1.1103(5) 0.0918(15) Uani d . 1 . . H H8 1.3383 1.0895 1.1643 0.110 Uiso calc R 1 . . C C9 1.2953(5) 1.0705(4) 1.0149(6) 0.1053(19) Uani d . 1 . . H H9 1.3799 1.0370 1.0038 0.126 Uiso calc R 1 . . C C10 1.1970(5) 1.0884(4) 0.9325(4) 0.0845(13) Uani d . 1 . . H H10 1.2170 1.0683 0.8672 0.101 Uiso calc R 1 . . C C11 1.0701(4) 1.1359(3) 0.9479(3) 0.0547(8) Uani d . 1 . . C C12 1.0410(4) 1.1663(3) 1.0464(3) 0.0492(8) Uani d . 1 . . C C13 0.9662(4) 1.1572(3) 0.8612(3) 0.0636(10) Uani d . 1 . . C C14 0.7269(5) 1.2149(3) 0.7930(3) 0.0737(11) Uani d . 1 . . H H14A 0.7827 1.2462 0.7515 0.088 Uiso calc R 1 . . H H14B 0.6660 1.2723 0.8202 0.088 Uiso calc R 1 . . C C15 0.6233(4) 1.0984(3) 0.7248(3) 0.0602(9) Uani d . 1 . . C C16 0.6623(5) 1.0275(3) 0.6388(3) 0.0680(10) Uani d . 1 . . H H16 0.7496 1.0539 0.6214 0.082 Uiso calc R 1 . . C C17 0.5738(4) 0.9184(3) 0.5784(3) 0.0636(9) Uani d . 1 . . H H17 0.6009 0.8715 0.5208 0.076 Uiso calc R 1 . . C C18 0.4443(4) 0.8797(3) 0.6049(2) 0.0535(8) Uani d . 1 . . C C19 0.4011(4) 0.9501(4) 0.6880(3) 0.0714(10) Uani d . 1 . . H H19 0.3127 0.9246 0.7045 0.086 Uiso calc R 1 . . C C20 0.4909(5) 1.0596(4) 0.7469(3) 0.0765(11) Uani d . 1 . . H H20 0.4611 1.1079 0.8027 0.092 Uiso calc R 1 . . C C21 0.5844(4) 0.5873(3) 0.6806(2) 0.0500(8) Uani d . 1 . . H H21 0.6372 0.5541 0.6320 0.060 Uiso calc R 1 . . C C22 0.6255(4) 0.5781(3) 0.7849(2) 0.0475(7) Uani d . 1 . . C C23 0.7517(4) 0.5304(3) 0.8140(3) 0.0580(9) Uani d . 1 . . H H23 0.8057 0.4994 0.7655 0.070 Uiso calc R 1 . . C C24 0.7984(4) 0.5285(3) 0.9143(3) 0.0613(9) Uani d . 1 . . H H24 0.8839 0.4973 0.9341 0.074 Uiso calc R 1 . . C C25 0.7162(4) 0.5734(3) 0.9838(2) 0.0550(8) Uani d . 1 . . C C26 0.5894(4) 0.6196(3) 0.9578(3) 0.0638(9) Uani d . 1 . . H H26 0.5356 0.6495 1.0067 0.077 Uiso calc R 1 . . C C27 0.5431(4) 0.6209(3) 0.8576(3) 0.0615(9) Uani d . 1 . . H H27 0.4561 0.6507 0.8382 0.074 Uiso calc R 1 . . N N4 0.7691(4) 0.5767(3) 1.0923(3) 0.0733(9) Uani d . 1 . . O O5 0.6974(4) 0.6209(4) 1.1535(2) 0.1111(12) Uani d . 1 . . O O6 0.8819(4) 0.5387(4) 1.1166(2) 0.1188(13) Uani d . 1 . . S S2 0.74498(12) 0.64956(10) 0.39415(8) 0.0747(3) Uani d . 1 . . O O1S 0.7208(3) 0.6673(3) 0.5003(2) 0.0830(8) Uani d . 1 . . C C1S 0.8748(5) 0.5522(4) 0.3777(3) 0.0833(12) Uani d . 1 . . H H1S1 0.8257 0.4734 0.3689 0.125 Uiso calc R 1 . . H H1S2 0.9591 0.5784 0.4379 0.125 Uiso calc R 1 . . H H1S3 0.9105 0.5515 0.3173 0.125 Uiso calc R 1 . . C C2S 0.8693(6) 0.7814(4) 0.4070(4) 0.1081(17) Uani d . 1 . . H H2S1 0.8157 0.8468 0.4170 0.162 Uiso calc R 1 . . H H2S2 0.9049 0.7705 0.3451 0.162 Uiso calc R 1 . . H H2S3 0.9542 0.7979 0.4657 0.162 Uiso calc R 1 . . 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 0.0667(6) 0.0595(5) 0.0449(5) -0.0013(4) -0.0036(4) 0.0219(4) N1 0.0665(19) 0.0523(16) 0.0478(16) 0.0087(14) 0.0064(14) 0.0155(13) N2 0.0696(19) 0.0552(16) 0.0371(14) 0.0016(14) 0.0122(14) 0.0193(12) N3 0.0566(16) 0.0536(15) 0.0412(14) 0.0033(13) 0.0094(12) 0.0217(12) O1 0.084(2) 0.137(3) 0.079(2) 0.060(2) 0.0151(16) 0.0140(19) O2 0.103(2) 0.127(3) 0.0623(18) -0.0099(19) 0.0389(17) 0.0240(17) O3 0.113(2) 0.0723(17) 0.0391(13) -0.0025(15) -0.0086(13) 0.0230(12) O4 0.0539(15) 0.0878(19) 0.0830(19) 0.0021(13) 0.0062(13) 0.0319(15) C2 0.064(2) 0.062(2) 0.055(2) 0.0181(18) 0.0125(18) 0.0088(17) C3 0.059(2) 0.055(2) 0.0449(19) 0.0089(16) 0.0094(16) 0.0111(15) C4 0.077(3) 0.085(3) 0.059(2) 0.014(2) 0.019(2) 0.010(2) C5 0.103(4) 0.097(3) 0.046(2) -0.003(3) 0.011(2) 0.019(2) C6 0.094(3) 0.068(3) 0.062(3) -0.011(2) -0.012(2) 0.028(2) C7 0.058(2) 0.0424(18) 0.079(3) -0.0036(16) -0.0068(19) 0.0200(17) C8 0.062(3) 0.057(2) 0.136(5) 0.007(2) -0.012(3) 0.028(3) C9 0.053(3) 0.075(3) 0.170(6) 0.020(2) 0.022(3) 0.015(3) C10 0.062(3) 0.068(3) 0.111(4) 0.003(2) 0.038(3) 0.004(2) C11 0.0454(19) 0.0446(17) 0.066(2) -0.0026(15) 0.0159(17) 0.0083(16) C12 0.0477(19) 0.0370(16) 0.057(2) -0.0010(14) 0.0091(15) 0.0119(14) C13 0.073(3) 0.054(2) 0.058(2) -0.0128(18) 0.0226(19) 0.0129(17) C14 0.099(3) 0.054(2) 0.058(2) 0.008(2) -0.003(2) 0.0214(17) C15 0.083(3) 0.0477(19) 0.0437(19) 0.0127(18) -0.0020(18) 0.0186(15) C16 0.082(3) 0.060(2) 0.059(2) -0.0055(19) 0.014(2) 0.0247(18) C17 0.080(3) 0.056(2) 0.051(2) 0.0032(19) 0.0152(19) 0.0167(16) C18 0.062(2) 0.0540(19) 0.0415(18) 0.0084(16) 0.0002(15) 0.0211(15) C19 0.067(2) 0.080(3) 0.061(2) 0.007(2) 0.0146(19) 0.017(2) C20 0.080(3) 0.072(3) 0.060(2) 0.009(2) 0.012(2) 0.004(2) C21 0.061(2) 0.0471(17) 0.0396(17) 0.0028(16) 0.0122(15) 0.0141(14) C22 0.0561(19) 0.0409(16) 0.0446(17) 0.0047(14) 0.0108(15) 0.0152(13) C23 0.073(2) 0.053(2) 0.051(2) 0.0212(17) 0.0210(17) 0.0152(16) C24 0.069(2) 0.062(2) 0.055(2) 0.0231(18) 0.0075(18) 0.0227(17) C25 0.064(2) 0.055(2) 0.0431(18) 0.0007(17) 0.0074(16) 0.0192(15) C26 0.068(2) 0.081(3) 0.053(2) 0.017(2) 0.0235(18) 0.0292(19) C27 0.057(2) 0.083(3) 0.057(2) 0.0212(19) 0.0184(17) 0.0352(19) N4 0.080(2) 0.087(2) 0.052(2) 0.0088(19) 0.0094(18) 0.0279(17) O5 0.115(3) 0.171(3) 0.0557(18) 0.032(2) 0.0289(19) 0.043(2) O6 0.121(3) 0.182(4) 0.072(2) 0.070(3) 0.0121(19) 0.062(2) S2 0.0732(7) 0.1007(8) 0.0565(6) 0.0068(6) 0.0234(5) 0.0332(5) O1S 0.103(2) 0.095(2) 0.0608(16) 0.0099(16) 0.0414(15) 0.0291(14) C1S 0.080(3) 0.094(3) 0.077(3) 0.010(2) 0.028(2) 0.025(2) C2S 0.130(4) 0.101(4) 0.115(4) 0.005(3) 0.060(3) 0.053(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _geom_angle_publ_flag O4 S1 O3 . . 120.25(16) ? O4 S1 N2 . . 108.61(16) ? O3 S1 N2 . . 103.64(16) ? O4 S1 C18 . . 107.94(17) ? O3 S1 C18 . . 109.03(15) ? N2 S1 C18 . . 106.58(15) ? C2 N1 C13 . . 123.8(3) ? C2 N1 C14 . . 118.4(3) ? C13 N1 C14 . . 117.7(3) ? N3 N2 S1 . . 115.3(2) ? N3 N2 H2N . . 117.1 ? S1 N2 H2N . . 114.1 ? C21 N3 N2 . . 115.5(3) ? O1 C2 N1 . . 119.3(3) ? O1 C2 C3 . . 122.8(3) ? N1 C2 C3 . . 117.9(3) ? C4 C3 C12 . . 119.4(3) ? C4 C3 C2 . . 120.4(3) ? C12 C3 C2 . . 120.1(3) ? C3 C4 C5 . . 120.8(4) ? C3 C4 H4 . . 119.6 ? C5 C4 H4 . . 119.6 ? C6 C5 C4 . . 121.3(4) ? C6 C5 H5 . . 119.4 ? C4 C5 H5 . . 119.4 ? C5 C6 C7 . . 120.7(4) ? C5 C6 H6 . . 119.6 ? C7 C6 H6 . . 119.6 ? C8 C7 C6 . . 124.0(4) ? C8 C7 C12 . . 117.6(4) ? C6 C7 C12 . . 118.3(4) ? C9 C8 C7 . . 121.7(5) ? C9 C8 H8 . . 119.1 ? C7 C8 H8 . . 119.1 ? C8 C9 C10 . . 120.9(4) ? C8 C9 H9 . . 119.6 ? C10 C9 H9 . . 119.6 ? C11 C10 C9 . . 119.9(5) ? C11 C10 H10 . . 120.1 ? C9 C10 H10 . . 120.1 ? C10 C11 C12 . . 119.8(4) ? C10 C11 C13 . . 120.2(4) ? C12 C11 C13 . . 119.9(3) ? C11 C12 C3 . . 120.5(3) ? C11 C12 C7 . . 120.1(3) ? C3 C12 C7 . . 119.4(3) ? O2 C13 N1 . . 120.1(4) ? O2 C13 C11 . . 122.6(4) ? N1 C13 C11 . . 117.3(3) ? N1 C14 C15 . . 111.5(3) ? N1 C14 H14A . . 109.3 ? C15 C14 H14A . . 109.3 ? N1 C14 H14B . . 109.3 ? C15 C14 H14B . . 109.3 ? H14A C14 H14B . . 108.0 ? C20 C15 C16 . . 118.5(3) ? C20 C15 C14 . . 121.5(4) ? C16 C15 C14 . . 120.0(4) ? C17 C16 C15 . . 121.1(4) ? C17 C16 H16 . . 119.5 ? C15 C16 H16 . . 119.5 ? C16 C17 C18 . . 119.1(4) ? C16 C17 H17 . . 120.4 ? C18 C17 H17 . . 120.4 ? C19 C18 C17 . . 120.7(3) ? C19 C18 S1 . . 121.3(3) ? C17 C18 S1 . . 118.0(3) ? C18 C19 C20 . . 119.2(4) ? C18 C19 H19 . . 120.4 ? C20 C19 H19 . . 120.4 ? C15 C20 C19 . . 121.4(4) ? C15 C20 H20 . . 119.3 ? C19 C20 H20 . . 119.3 ? N3 C21 C22 . . 120.5(3) ? N3 C21 H21 . . 119.7 ? C22 C21 H21 . . 119.7 ? C23 C22 C27 . . 118.9(3) ? C23 C22 C21 . . 119.9(3) ? C27 C22 C21 . . 121.1(3) ? C24 C23 C22 . . 120.7(3) ? C24 C23 H23 . . 119.6 ? C22 C23 H23 . . 119.6 ? C25 C24 C23 . . 118.5(3) ? C25 C24 H24 . . 120.7 ? C23 C24 H24 . . 120.7 ? C24 C25 C26 . . 122.6(3) ? C24 C25 N4 . . 118.9(3) ? C26 C25 N4 . . 118.5(3) ? C25 C26 C27 . . 118.6(3) ? C25 C26 H26 . . 120.7 ? C27 C26 H26 . . 120.7 ? C26 C27 C22 . . 120.6(3) ? C26 C27 H27 . . 119.7 ? C22 C27 H27 . . 119.7 ? O6 N4 O5 . . 123.1(4) ? O6 N4 C25 . . 119.1(4) ? O5 N4 C25 . . 117.7(4) ? O1S S2 C1S . . 106.61(19) ? O1S S2 C2S . . 104.8(2) ? C1S S2 C2S . . 97.5(2) ? S2 C1S H1S1 . . 109.5 ? S2 C1S H1S2 . . 109.5 ? H1S1 C1S H1S2 . . 109.5 ? S2 C1S H1S3 . . 109.5 ? H1S1 C1S H1S3 . . 109.5 ? H1S2 C1S H1S3 . . 109.5 ? S2 C2S H2S1 . . 109.5 ? S2 C2S H2S2 . . 109.5 ? H2S1 C2S H2S2 . . 109.5 ? S2 C2S H2S3 . . 109.5 ? H2S1 C2S H2S3 . . 109.5 ? H2S2 C2S H2S3 . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 O4 . 1.423(3) ? S1 O3 . 1.429(2) ? S1 N2 . 1.630(3) ? S1 C18 . 1.762(3) ? N1 C2 . 1.388(4) ? N1 C13 . 1.394(5) ? N1 C14 . 1.478(4) ? N2 N3 . 1.394(3) ? N2 H2N . 0.8006 ? N3 C21 . 1.263(4) ? O1 C2 . 1.224(4) ? O2 C13 . 1.214(4) ? C2 C3 . 1.461(5) ? C3 C4 . 1.377(5) ? C3 C12 . 1.404(5) ? C4 C5 . 1.380(6) ? C4 H4 . 0.9300 ? C5 C6 . 1.336(6) ? C5 H5 . 0.9300 ? C6 C7 . 1.415(6) ? C6 H6 . 0.9300 ? C7 C8 . 1.395(6) ? C7 C12 . 1.418(5) ? C8 C9 . 1.344(7) ? C8 H8 . 0.9300 ? C9 C10 . 1.391(7) ? C9 H9 . 0.9300 ? C10 C11 . 1.375(5) ? C10 H10 . 0.9300 ? C11 C12 . 1.399(5) ? C11 C13 . 1.481(5) ? C14 C15 . 1.517(5) ? C14 H14A . 0.9700 ? C14 H14B . 0.9700 ? C15 C20 . 1.375(5) ? C15 C16 . 1.384(5) ? C16 C17 . 1.381(5) ? C16 H16 . 0.9300 ? C17 C18 . 1.383(5) ? C17 H17 . 0.9300 ? C18 C19 . 1.373(5) ? C19 C20 . 1.383(5) ? C19 H19 . 0.9300 ? C20 H20 . 0.9300 ? C21 C22 . 1.462(4) ? C21 H21 . 0.9300 ? C22 C23 . 1.383(4) ? C22 C27 . 1.394(4) ? C23 C24 . 1.381(5) ? C23 H23 . 0.9300 ? C24 C25 . 1.367(5) ? C24 H24 . 0.9300 ? C25 C26 . 1.369(5) ? C25 N4 . 1.474(4) ? C26 C27 . 1.377(5) ? C26 H26 . 0.9300 ? C27 H27 . 0.9300 ? N4 O6 . 1.200(4) ? N4 O5 . 1.213(4) ? S2 O1S . 1.494(3) ? S2 C1S . 1.755(4) ? S2 C2S . 1.781(5) ? C1S H1S1 . 0.9600 ? C1S H1S2 . 0.9600 ? C1S H1S3 . 0.9600 ? C2S H2S1 . 0.9600 ? C2S H2S2 . 0.9600 ? C2S H2S3 . 0.9600 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N2 H2N O1S . 0.80 1.99 2.764(4) 163 y C8 H8 Cg 2_777 0.93 2.903 3.799(6) 162 y 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O4 S1 N2 N3 . . . . -49.9(3) ? O3 S1 N2 N3 . . . . -178.9(2) ? C18 S1 N2 N3 . . . . 66.1(3) ? S1 N2 N3 C21 . . . . -165.8(2) ? C13 N1 C2 O1 . . . . -175.1(3) ? C14 N1 C2 O1 . . . . 2.9(5) ? C13 N1 C2 C3 . . . . 4.6(5) ? C14 N1 C2 C3 . . . . -177.4(3) ? O1 C2 C3 C4 . . . . -5.1(6) ? N1 C2 C3 C4 . . . . 175.2(3) ? O1 C2 C3 C12 . . . . 172.8(4) ? N1 C2 C3 C12 . . . . -6.8(5) ? C12 C3 C4 C5 . . . . 0.2(6) ? C2 C3 C4 C5 . . . . 178.1(4) ? C3 C4 C5 C6 . . . . -1.7(7) ? C4 C5 C6 C7 . . . . 1.1(7) ? C5 C6 C7 C8 . . . . 179.7(4) ? C5 C6 C7 C12 . . . . 0.8(5) ? C6 C7 C8 C9 . . . . -179.1(4) ? C12 C7 C8 C9 . . . . -0.2(6) ? C7 C8 C9 C10 . . . . 1.2(7) ? C8 C9 C10 C11 . . . . -1.2(7) ? C9 C10 C11 C12 . . . . 0.2(5) ? C9 C10 C11 C13 . . . . 179.0(4) ? C10 C11 C12 C3 . . . . -178.8(3) ? C13 C11 C12 C3 . . . . 2.5(4) ? C10 C11 C12 C7 . . . . 0.7(5) ? C13 C11 C12 C7 . . . . -178.0(3) ? C4 C3 C12 C11 . . . . -178.7(3) ? C2 C3 C12 C11 . . . . 3.3(5) ? C4 C3 C12 C7 . . . . 1.8(5) ? C2 C3 C12 C7 . . . . -176.2(3) ? C8 C7 C12 C11 . . . . -0.7(5) ? C6 C7 C12 C11 . . . . 178.2(3) ? C8 C7 C12 C3 . . . . 178.8(3) ? C6 C7 C12 C3 . . . . -2.3(5) ? C2 N1 C13 O2 . . . . -179.9(3) ? C14 N1 C13 O2 . . . . 2.1(5) ? C2 N1 C13 C11 . . . . 1.1(5) ? C14 N1 C13 C11 . . . . -176.9(3) ? C10 C11 C13 O2 . . . . -2.5(5) ? C12 C11 C13 O2 . . . . 176.2(3) ? C10 C11 C13 N1 . . . . 176.5(3) ? C12 C11 C13 N1 . . . . -4.8(4) ? C2 N1 C14 C15 . . . . -96.1(4) ? C13 N1 C14 C15 . . . . 82.0(4) ? N1 C14 C15 C20 . . . . 86.5(5) ? N1 C14 C15 C16 . . . . -92.5(4) ? C20 C15 C16 C17 . . . . -2.3(5) ? C14 C15 C16 C17 . . . . 176.8(3) ? C15 C16 C17 C18 . . . . -0.1(5) ? C16 C17 C18 C19 . . . . 2.1(5) ? C16 C17 C18 S1 . . . . -176.1(3) ? O4 S1 C18 C19 . . . . 5.1(3) ? O3 S1 C18 C19 . . . . 137.3(3) ? N2 S1 C18 C19 . . . . -111.5(3) ? O4 S1 C18 C17 . . . . -176.8(3) ? O3 S1 C18 C17 . . . . -44.6(3) ? N2 S1 C18 C17 . . . . 66.7(3) ? C17 C18 C19 C20 . . . . -1.6(5) ? S1 C18 C19 C20 . . . . 176.6(3) ? C16 C15 C20 C19 . . . . 2.8(6) ? C14 C15 C20 C19 . . . . -176.2(3) ? C18 C19 C20 C15 . . . . -0.9(6) ? N2 N3 C21 C22 . . . . -179.6(2) ? N3 C21 C22 C23 . . . . -173.8(3) ? N3 C21 C22 C27 . . . . 3.6(5) ? C27 C22 C23 C24 . . . . -2.0(5) ? C21 C22 C23 C24 . . . . 175.5(3) ? C22 C23 C24 C25 . . . . 0.7(5) ? C23 C24 C25 C26 . . . . 0.3(5) ? C23 C24 C25 N4 . . . . -177.2(3) ? C24 C25 C26 C27 . . . . -0.1(5) ? N4 C25 C26 C27 . . . . 177.5(3) ? C25 C26 C27 C22 . . . . -1.2(5) ? C23 C22 C27 C26 . . . . 2.2(5) ? C21 C22 C27 C26 . . . . -175.3(3) ? C24 C25 N4 O6 . . . . -0.8(5) ? C26 C25 N4 O6 . . . . -178.5(4) ? C24 C25 N4 O5 . . . . 177.4(4) ? C26 C25 N4 O5 . . . . -0.3(5) ?