#------------------------------------------------------------------------------ #$Date: 2025-08-19 15:49:58 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301806 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/88/2238880.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_2238880 loop_ _publ_author_name 'Chicha, Hakima' 'Rakib, El Mostapha' 'Abderrafia, Hafid' 'Saadi, Mohamed' 'El Ammari, Lahcen' _publ_section_title ; N-(1-Allyl-1H-indazol-5-yl)-4-methylbenzenesulfonamide ; _journal_coeditor_code IM2445 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1847 _journal_paper_doi 10.1107/S1600536813032091 _journal_volume 69 _journal_year 2013 _chemical_formula_iupac 'C17 H17 N3 O2 S' _chemical_formula_moiety 'C17 H17 N3 O2 S' _chemical_formula_sum 'C17 H17 N3 O2 S' _chemical_formula_weight 327.40 _chemical_name_systematic ; N-(1-Allyl-1H-indazol-5-yl)-4-methylbenzenesulfonamide ; _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 80.2110(10) _cell_angle_beta 78.9840(10) _cell_angle_gamma 69.7840(10) _cell_formula_units_Z 4 _cell_length_a 8.8200(4) _cell_length_b 10.4769(5) _cell_length_c 19.7407(10) _cell_measurement_reflns_used 6791 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.37 _cell_measurement_theta_min 2.44 _cell_volume 1669.51(14) _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'PLATON (Spek, 2009) and publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker X8 APEX' _diffrn_measurement_method '\f and \w scans' _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 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 31703 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.44 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_T_max 0.7466 _exptl_absorpt_correction_T_min 0.6934 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2009)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 688 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _refine_diff_density_max 0.315 _refine_diff_density_min -0.280 _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 415 _refine_ls_number_reflns 6791 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0420 _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^)+(0.0594P)^2^+0.4278P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1102 _refine_ls_wR_factor_ref 0.1204 _reflns_number_gt 5368 _reflns_number_total 6791 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL EL13_D371_DRX3_AA1T3 in P-1 CELL 0.71073 8.8200 10.4769 19.7407 80.211 78.984 69.784 ZERR 4.00 0.0004 0.0005 0.0010 0.001 0.001 0.001 LATT 1 SFAC C H N O S UNIT 68 68 12 8 4 MERG 2 OMIT 0 0 1 OMIT 0 1 0 OMIT 0 0 2 SHEL 40 0.8 HTAB N6 O1 HTAB N3 N5_$1 HTAB C21 O4_$2 HTAB C7 O2_$3 eqiv $1 -x, -y+2, -z+1 eqiv $2 -x+1, -y+2, -z+1 eqiv $3 -x, -y+2, -z+2 FMAP 2 PLAN 10 ACTA BOND BOND $H CONF L.S. 10 TEMP 23.00 WGHT 0.0594 0.4278 FVAR 0.40268 C1 1 -0.533094 1.410343 1.104803 11.00000 0.09207 0.16251 = 0.14920 -0.07077 0.00103 -0.01456 AFIX 93 H1A 2 -0.476230 1.346020 1.137515 11.00000 -1.20000 H1B 2 -0.536258 1.500948 1.100719 11.00000 -1.20000 AFIX 0 C2 1 -0.605387 1.374962 1.066264 11.00000 0.07873 0.10515 = 0.08886 -0.04331 0.00010 -0.00816 AFIX 43 H2 2 -0.661039 1.441933 1.034145 11.00000 -1.20000 AFIX 0 C3 1 -0.608539 1.231889 1.068265 11.00000 0.08284 0.09865 = 0.06133 -0.02025 0.01630 -0.01963 AFIX 23 H3A 2 -0.529163 1.169353 1.096626 11.00000 -1.20000 H3B 2 -0.715626 1.227599 1.089439 11.00000 -1.20000 AFIX 0 C4 1 -0.623730 1.155346 0.903725 11.00000 0.06405 0.11675 = 0.08085 -0.02138 -0.01940 -0.00962 AFIX 43 H4 2 -0.679643 1.147267 0.870071 11.00000 -1.20000 AFIX 0 C5 1 -0.452688 1.128057 0.894896 11.00000 0.05891 0.06690 = 0.05643 -0.00890 -0.01446 -0.00732 C6 1 -0.423675 1.150744 0.958418 11.00000 0.06494 0.05092 = 0.04635 -0.00463 -0.00358 -0.01171 C7 1 -0.267745 1.132331 0.971227 11.00000 0.07380 0.07488 = 0.03964 -0.01475 -0.00725 -0.02142 AFIX 43 H7 2 -0.250010 1.146005 1.013995 11.00000 -1.20000 AFIX 0 C8 1 -0.140944 1.093394 0.918857 11.00000 0.06284 0.06677 = 0.04182 -0.01041 -0.01086 -0.02118 AFIX 43 H8 2 -0.035507 1.081591 0.926017 11.00000 -1.20000 AFIX 0 C9 1 -0.167039 1.070816 0.854242 11.00000 0.05981 0.04545 = 0.03604 -0.00539 -0.00903 -0.01117 C10 1 -0.320062 1.085998 0.842258 11.00000 0.06283 0.07573 = 0.04456 -0.01411 -0.01791 -0.00905 AFIX 43 H10 2 -0.336325 1.068800 0.799964 11.00000 -1.20000 AFIX 0 C11 1 0.071418 0.758806 0.819120 11.00000 0.04998 0.05607 = 0.04609 -0.00823 -0.00393 -0.00642 C12 1 -0.005889 0.734377 0.770262 11.00000 0.07728 0.06741 = 0.05872 -0.00902 -0.01519 -0.01899 AFIX 43 H12 2 -0.031693 0.798184 0.731747 11.00000 -1.20000 AFIX 0 C13 1 -0.044348 0.616059 0.778717 11.00000 0.08099 0.07531 = 0.09057 -0.02534 -0.00895 -0.02441 AFIX 43 H13 2 -0.097715 0.601073 0.746005 11.00000 -1.20000 AFIX 0 C14 1 -0.005334 0.518544 0.834942 11.00000 0.05860 0.06018 = 0.10933 -0.02018 0.01169 -0.00977 C15 1 0.068209 0.545470 0.883451 11.00000 0.07650 0.06657 = 0.09219 0.01864 -0.00190 -0.00753 AFIX 43 H15 2 0.093510 0.481408 0.921921 11.00000 -1.20000 AFIX 0 C16 1 0.106295 0.665497 0.877061 11.00000 0.06762 0.07375 = 0.06273 0.00605 -0.01567 -0.01226 AFIX 43 H16 2 0.154273 0.682577 0.911113 11.00000 -1.20000 AFIX 0 C17 1 -0.042321 0.386197 0.843628 11.00000 0.09604 0.06561 = 0.18553 -0.02252 0.02194 -0.02416 AFIX 33 H17A 2 -0.154929 0.405407 0.839414 11.00000 -1.50000 H17B 2 -0.021397 0.338344 0.888621 11.00000 -1.50000 H17C 2 0.025788 0.330491 0.808383 11.00000 -1.50000 AFIX 0 C18 1 -0.023891 0.555301 0.403094 11.00000 0.09313 0.05645 = 0.11269 -0.00354 -0.02202 -0.02241 AFIX 93 H18A 2 -0.110332 0.566532 0.439325 11.00000 -1.20000 H18B 2 0.033178 0.468767 0.389356 11.00000 -1.20000 AFIX 0 C19 1 0.016526 0.658916 0.372144 11.00000 0.06847 0.06179 = 0.06631 -0.01305 -0.01450 -0.02436 AFIX 43 H19 2 0.103555 0.643829 0.336153 11.00000 -1.20000 AFIX 0 C20 1 -0.065882 0.802240 0.389618 11.00000 0.05215 0.05060 = 0.05893 -0.00026 -0.02058 -0.01914 AFIX 23 H20A 2 -0.127307 0.855909 0.352732 11.00000 -1.20000 H20B 2 -0.142309 0.801867 0.432048 11.00000 -1.20000 AFIX 0 C21 1 0.228155 0.969251 0.365553 11.00000 0.06523 0.05789 = 0.03780 0.00155 -0.01116 -0.03085 AFIX 43 H21 2 0.291090 1.019347 0.338252 11.00000 -1.20000 AFIX 0 C22 1 0.239101 0.919912 0.436477 11.00000 0.05221 0.04082 = 0.03679 -0.00342 -0.00810 -0.01650 C23 1 0.334647 0.923380 0.484896 11.00000 0.05279 0.04404 = 0.04014 -0.00320 -0.01022 -0.01994 AFIX 43 H23 2 0.411837 0.968438 0.472927 11.00000 -1.20000 AFIX 0 C24 1 0.310653 0.858188 0.550500 11.00000 0.05022 0.03791 = 0.03537 -0.00692 -0.00908 -0.00869 C25 1 0.190982 0.792824 0.569249 11.00000 0.05550 0.04913 = 0.03562 0.00157 -0.00530 -0.01424 AFIX 43 H25 2 0.176750 0.750692 0.614339 11.00000 -1.20000 AFIX 0 C26 1 0.095152 0.789440 0.523189 11.00000 0.05001 0.04889 = 0.04689 0.00252 -0.00625 -0.01934 AFIX 43 H26 2 0.015790 0.746713 0.536106 11.00000 -1.20000 AFIX 0 C27 1 0.121589 0.852978 0.455828 11.00000 0.04490 0.03742 = 0.03925 -0.00496 -0.00931 -0.01067 C28 1 0.535892 0.583927 0.635130 11.00000 0.04988 0.04636 = 0.04115 -0.00184 -0.01289 -0.01189 C29 1 0.539617 0.500106 0.587778 11.00000 0.06796 0.05332 = 0.04098 -0.00543 -0.01234 -0.01290 AFIX 43 H29 2 0.577270 0.518792 0.541083 11.00000 -1.20000 AFIX 0 C30 1 0.487368 0.388601 0.609887 11.00000 0.07496 0.05161 = 0.06196 -0.00719 -0.02302 -0.01675 AFIX 43 H30 2 0.488851 0.333016 0.577546 11.00000 -1.20000 AFIX 0 C31 1 0.432691 0.357136 0.679030 11.00000 0.05082 0.05174 = 0.07230 0.00555 -0.02115 -0.01310 C32 1 0.433535 0.441065 0.725914 11.00000 0.08748 0.07490 = 0.05001 0.00291 0.00034 -0.02957 AFIX 43 H32 2 0.399360 0.420657 0.772831 11.00000 -1.20000 AFIX 0 C33 1 0.483662 0.553897 0.704837 11.00000 0.09534 0.06428 = 0.04251 -0.00981 -0.00784 -0.02844 AFIX 43 H33 2 0.482489 0.609512 0.737105 11.00000 -1.20000 AFIX 0 C34 1 0.373227 0.236213 0.701948 11.00000 0.07251 0.07581 = 0.10860 0.01933 -0.03106 -0.03426 AFIX 33 H34A 2 0.256177 0.267476 0.711518 11.00000 -1.50000 H34B 2 0.417422 0.186728 0.743189 11.00000 -1.50000 H34C 2 0.408098 0.177189 0.665778 11.00000 -1.50000 AFIX 0 N1 3 -0.571796 1.189777 0.999081 11.00000 0.06785 0.06876 = 0.05989 -0.01028 0.00292 -0.01259 N2 3 -0.693854 1.193570 0.965460 11.00000 0.06312 0.09415 = 0.08482 -0.01298 -0.00434 -0.00950 N3 3 -0.033116 1.039637 0.798821 11.00000 0.06434 0.05814 = 0.03116 -0.00535 -0.01025 -0.01393 AFIX 3 H3N 2 -0.059361 1.051766 0.761133 11.00000 -1.20000 AFIX 0 N4 3 0.050296 0.865679 0.398712 11.00000 0.05369 0.04828 = 0.04318 0.00004 -0.01409 -0.02042 N5 3 0.117480 0.935105 0.343239 11.00000 0.06572 0.05843 = 0.03747 0.00080 -0.01447 -0.02608 N6 3 0.409660 0.859773 0.600818 11.00000 0.06148 0.04883 = 0.03486 -0.00741 -0.01109 -0.01339 AFIX 3 H6N 2 0.361508 0.870033 0.638795 11.00000 -1.20000 AFIX 0 O1 4 0.223631 0.910107 0.737133 11.00000 0.06624 0.08559 = 0.04763 -0.01262 0.00513 -0.02465 O2 4 0.200261 0.910928 0.863329 11.00000 0.06558 0.08845 = 0.05350 -0.01288 -0.02287 -0.01669 O3 4 0.671265 0.726574 0.537925 11.00000 0.06034 0.06866 = 0.06395 0.00175 0.00316 -0.01869 O4 4 0.651054 0.764656 0.660095 11.00000 0.08652 0.07097 = 0.08460 0.00177 -0.04754 -0.03399 S1 5 0.129538 0.907218 0.804831 11.00000 0.05288 0.06490 = 0.03710 -0.00863 -0.00790 -0.01467 S2 5 0.583439 0.735917 0.606622 11.00000 0.05540 0.05244 = 0.04957 -0.00019 -0.01650 -0.01890 HKLF 4 REM EL13_D371_DRX3_AA1T3 in P-1 REM R1 = 0.0421 for 5368 Fo > 4sig(Fo) and 0.0554 for all 6791 data REM 415 parameters refined using 0 restraints END WGHT 0.0594 0.4278 newcifs REM Highest difference peak 0.315, deepest hole -0.280, 1-sigma level 0.035 Q1 1 0.5509 0.6576 0.6227 11.00000 0.05 0.32 Q2 1 0.0749 0.8377 0.8152 11.00000 0.05 0.27 Q3 1 0.6270 0.8033 0.5628 11.00000 0.05 0.23 Q4 1 0.2117 0.8639 0.4446 11.00000 0.05 0.21 Q5 1 -0.5545 1.3030 1.1032 11.00000 0.05 0.20 Q6 1 0.3511 0.8571 0.5117 11.00000 0.05 0.20 Q7 1 0.2942 0.9175 0.5205 11.00000 0.05 0.18 Q8 1 -0.1549 1.0618 0.8889 11.00000 0.05 0.18 Q9 1 0.0750 0.7259 0.8519 11.00000 0.05 0.18 Q10 1 0.0355 0.5569 0.8032 11.00000 0.05 0.18 ; _cod_data_source_file im2445.cif _cod_data_source_block I _cod_original_sg_symbol_Hall '-p 1' _cod_database_code 2238880 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_symmetry_multiplicity C C1 -0.5331(4) 1.4103(5) 1.1048(2) 0.1376(14) Uani d . 1 1 H H1A -0.4762 1.3460 1.1375 0.165 Uiso calc R 1 1 H H1B -0.5362 1.5009 1.1007 0.165 Uiso calc R 1 1 C C2 -0.6054(3) 1.3750(3) 1.06626(16) 0.0943(8) Uani d . 1 1 H H2 -0.6610 1.4419 1.0341 0.113 Uiso calc R 1 1 C C3 -0.6085(3) 1.2319(3) 1.06826(13) 0.0859(7) Uani d . 1 1 H H3A -0.5292 1.1694 1.0966 0.103 Uiso calc R 1 1 H H3B -0.7156 1.2276 1.0894 0.103 Uiso calc R 1 1 C C4 -0.6237(3) 1.1553(3) 0.90373(15) 0.0899(8) Uani d . 1 1 H H4 -0.6796 1.1473 0.8701 0.108 Uiso calc R 1 1 C C5 -0.4527(3) 1.1281(2) 0.89489(11) 0.0631(5) Uani d . 1 1 C C6 -0.4237(3) 1.1507(2) 0.95842(10) 0.0567(5) Uani d . 1 1 C C7 -0.2677(3) 1.1323(2) 0.97123(10) 0.0626(5) Uani d . 1 1 H H7 -0.2500 1.1460 1.0140 0.075 Uiso calc R 1 1 C C8 -0.1409(3) 1.0934(2) 0.91886(9) 0.0561(5) Uani d . 1 1 H H8 -0.0355 1.0816 0.9260 0.067 Uiso calc R 1 1 C C9 -0.1670(2) 1.07082(18) 0.85424(9) 0.0483(4) Uani d . 1 1 C C10 -0.3201(3) 1.0860(2) 0.84226(10) 0.0623(5) Uani d . 1 1 H H10 -0.3363 1.0688 0.8000 0.075 Uiso calc R 1 1 C C11 0.0714(2) 0.7588(2) 0.81912(10) 0.0537(4) Uani d . 1 1 C C12 -0.0059(3) 0.7344(2) 0.77026(12) 0.0680(6) Uani d . 1 1 H H12 -0.0317 0.7982 0.7317 0.082 Uiso calc R 1 1 C C13 -0.0443(3) 0.6161(3) 0.77871(15) 0.0810(7) Uani d . 1 1 H H13 -0.0977 0.6011 0.7460 0.097 Uiso calc R 1 1 C C14 -0.0053(3) 0.5185(2) 0.83494(16) 0.0806(7) Uani d . 1 1 C C15 0.0682(3) 0.5455(3) 0.88345(15) 0.0874(8) Uani d . 1 1 H H15 0.0935 0.4814 0.9219 0.105 Uiso calc R 1 1 C C16 0.1063(3) 0.6655(2) 0.87706(12) 0.0717(6) Uani d . 1 1 H H16 0.1543 0.6826 0.9111 0.086 Uiso calc R 1 1 C C17 -0.0423(4) 0.3862(3) 0.8436(2) 0.1211(12) Uani d . 1 1 H H17A -0.1549 0.4054 0.8394 0.182 Uiso calc R 1 1 H H17B -0.0214 0.3383 0.8886 0.182 Uiso calc R 1 1 H H17C 0.0258 0.3305 0.8084 0.182 Uiso calc R 1 1 C C18 -0.0239(3) 0.5553(3) 0.40309(16) 0.0876(8) Uani d . 1 1 H H18A -0.1103 0.5665 0.4393 0.105 Uiso calc R 1 1 H H18B 0.0332 0.4688 0.3894 0.105 Uiso calc R 1 1 C C19 0.0165(3) 0.6589(2) 0.37214(12) 0.0632(5) Uani d . 1 1 H H19 0.1036 0.6438 0.3362 0.076 Uiso calc R 1 1 C C20 -0.0659(2) 0.80224(19) 0.38962(10) 0.0522(4) Uani d . 1 1 H H20A -0.1273 0.8559 0.3527 0.063 Uiso calc R 1 1 H H20B -0.1423 0.8019 0.4320 0.063 Uiso calc R 1 1 C C21 0.2282(2) 0.96925(19) 0.36555(9) 0.0511(4) Uani d . 1 1 H H21 0.2911 1.0194 0.3383 0.061 Uiso calc R 1 1 C C22 0.2391(2) 0.91991(17) 0.43648(8) 0.0428(4) Uani d . 1 1 C C23 0.3346(2) 0.92338(17) 0.48490(8) 0.0442(4) Uani d . 1 1 H H23 0.4118 0.9684 0.4729 0.053 Uiso calc R 1 1 C C24 0.3107(2) 0.85819(16) 0.55050(8) 0.0419(4) Uani d . 1 1 C C25 0.1910(2) 0.79282(18) 0.56925(9) 0.0484(4) Uani d . 1 1 H H25 0.1768 0.7507 0.6143 0.058 Uiso calc R 1 1 C C26 0.0952(2) 0.78944(18) 0.52319(9) 0.0488(4) Uani d . 1 1 H H26 0.0158 0.7467 0.5361 0.059 Uiso calc R 1 1 C C27 0.1216(2) 0.85298(16) 0.45583(8) 0.0407(4) Uani d . 1 1 C C28 0.5359(2) 0.58393(18) 0.63513(9) 0.0463(4) Uani d . 1 1 C C29 0.5396(2) 0.5001(2) 0.58778(10) 0.0552(5) Uani d . 1 1 H H29 0.5773 0.5188 0.5411 0.066 Uiso calc R 1 1 C C30 0.4874(3) 0.3886(2) 0.60989(11) 0.0619(5) Uani d . 1 1 H H30 0.4889 0.3330 0.5775 0.074 Uiso calc R 1 1 C C31 0.4327(2) 0.3571(2) 0.67903(11) 0.0590(5) Uani d . 1 1 C C32 0.4335(3) 0.4411(2) 0.72592(11) 0.0726(6) Uani d . 1 1 H H32 0.3994 0.4207 0.7728 0.087 Uiso calc R 1 1 C C33 0.4837(3) 0.5539(2) 0.70484(10) 0.0665(6) Uani d . 1 1 H H33 0.4825 0.6095 0.7371 0.080 Uiso calc R 1 1 C C34 0.3732(3) 0.2362(3) 0.70195(15) 0.0841(7) Uani d . 1 1 H H34A 0.2562 0.2675 0.7115 0.126 Uiso calc R 1 1 H H34B 0.4174 0.1867 0.7432 0.126 Uiso calc R 1 1 H H34C 0.4081 0.1772 0.6658 0.126 Uiso calc R 1 1 N N1 -0.5718(2) 1.18978(19) 0.99908(10) 0.0694(5) Uani d . 1 1 N N2 -0.6939(2) 1.1936(2) 0.96546(12) 0.0855(6) Uani d . 1 1 N N3 -0.03312(19) 1.03964(16) 0.79882(7) 0.0523(4) Uani d . 1 1 H H3N -0.0594 1.0518 0.7611 0.063 Uiso d R 1 1 N N4 0.05029(18) 0.86568(15) 0.39871(7) 0.0470(3) Uani d . 1 1 N N5 0.1175(2) 0.93510(16) 0.34324(7) 0.0521(4) Uani d . 1 1 N N6 0.40966(19) 0.85977(15) 0.60082(7) 0.0487(4) Uani d . 1 1 H H6N 0.3615 0.8700 0.6388 0.058 Uiso d R 1 1 O O1 0.22363(18) 0.91011(16) 0.73713(7) 0.0677(4) Uani d . 1 1 O O2 0.20026(17) 0.91093(16) 0.86333(7) 0.0688(4) Uani d . 1 1 O O3 0.67127(17) 0.72657(15) 0.53792(8) 0.0677(4) Uani d . 1 1 O O4 0.6511(2) 0.76466(16) 0.66010(8) 0.0748(4) Uani d . 1 1 S S1 0.12954(6) 0.90722(5) 0.80483(2) 0.05223(14) Uani d . 1 1 S S2 0.58344(6) 0.73592(5) 0.60662(2) 0.05151(14) Uani d . 1 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 C1 0.092(2) 0.163(4) 0.149(3) -0.015(2) 0.001(2) -0.071(3) C2 0.0788(17) 0.105(2) 0.0888(19) -0.0081(15) 0.0001(15) -0.0433(17) C3 0.0829(16) 0.099(2) 0.0613(14) -0.0196(14) 0.0163(12) -0.0202(13) C4 0.0640(14) 0.117(2) 0.0809(17) -0.0096(14) -0.0194(13) -0.0214(16) C5 0.0589(12) 0.0669(13) 0.0564(12) -0.0073(10) -0.0145(9) -0.0089(10) C6 0.0649(12) 0.0509(11) 0.0464(10) -0.0117(9) -0.0036(9) -0.0046(8) C7 0.0738(13) 0.0749(14) 0.0397(10) -0.0214(11) -0.0072(9) -0.0148(9) C8 0.0629(11) 0.0668(12) 0.0418(10) -0.0212(10) -0.0109(8) -0.0104(9) C9 0.0598(11) 0.0455(10) 0.0361(9) -0.0112(8) -0.0090(8) -0.0054(7) C10 0.0628(12) 0.0757(14) 0.0446(10) -0.0091(10) -0.0179(9) -0.0141(9) C11 0.0500(10) 0.0561(11) 0.0461(10) -0.0064(8) -0.0039(8) -0.0082(8) C12 0.0773(14) 0.0674(14) 0.0587(12) -0.0190(11) -0.0152(11) -0.0090(10) C13 0.0810(16) 0.0753(16) 0.0906(18) -0.0244(13) -0.0089(14) -0.0253(14) C14 0.0586(13) 0.0602(14) 0.109(2) -0.0098(11) 0.0117(13) -0.0202(14) C15 0.0765(16) 0.0666(15) 0.0922(19) -0.0075(13) -0.0019(14) 0.0186(13) C16 0.0676(13) 0.0738(15) 0.0627(13) -0.0123(11) -0.0157(11) 0.0060(11) C17 0.096(2) 0.0656(17) 0.186(4) -0.0242(15) 0.022(2) -0.0225(19) C18 0.0931(18) 0.0565(14) 0.113(2) -0.0224(13) -0.0220(16) -0.0035(13) C19 0.0685(13) 0.0618(13) 0.0663(13) -0.0244(10) -0.0145(10) -0.0131(10) C20 0.0522(10) 0.0506(10) 0.0589(11) -0.0191(8) -0.0206(9) -0.0003(8) C21 0.0652(11) 0.0579(11) 0.0378(9) -0.0308(9) -0.0112(8) 0.0015(8) C22 0.0522(9) 0.0408(9) 0.0368(8) -0.0165(7) -0.0081(7) -0.0034(7) C23 0.0528(10) 0.0440(9) 0.0401(9) -0.0199(8) -0.0102(7) -0.0032(7) C24 0.0502(9) 0.0379(8) 0.0354(8) -0.0087(7) -0.0091(7) -0.0069(6) C25 0.0555(10) 0.0491(10) 0.0356(9) -0.0142(8) -0.0053(7) 0.0016(7) C26 0.0500(10) 0.0489(10) 0.0469(10) -0.0193(8) -0.0063(8) 0.0025(8) C27 0.0449(9) 0.0374(8) 0.0393(8) -0.0107(7) -0.0093(7) -0.0050(7) C28 0.0499(10) 0.0464(9) 0.0412(9) -0.0119(8) -0.0129(7) -0.0018(7) C29 0.0680(12) 0.0533(11) 0.0410(9) -0.0129(9) -0.0123(9) -0.0054(8) C30 0.0750(13) 0.0516(11) 0.0620(12) -0.0168(10) -0.0230(10) -0.0072(9) C31 0.0508(11) 0.0517(11) 0.0723(13) -0.0131(9) -0.0212(10) 0.0055(10) C32 0.0875(16) 0.0749(15) 0.0500(12) -0.0296(13) 0.0003(11) 0.0029(10) C33 0.0954(16) 0.0643(13) 0.0425(10) -0.0284(12) -0.0078(10) -0.0098(9) C34 0.0725(15) 0.0758(16) 0.109(2) -0.0343(13) -0.0311(14) 0.0193(14) N1 0.0679(11) 0.0688(12) 0.0599(11) -0.0126(9) 0.0029(9) -0.0103(9) N2 0.0631(12) 0.0942(16) 0.0848(15) -0.0095(11) -0.0043(11) -0.0130(12) N3 0.0643(9) 0.0581(9) 0.0312(7) -0.0139(8) -0.0103(7) -0.0054(6) N4 0.0537(8) 0.0483(8) 0.0432(8) -0.0204(7) -0.0141(6) 0.0000(6) N5 0.0657(10) 0.0584(9) 0.0375(8) -0.0261(8) -0.0145(7) 0.0008(7) N6 0.0615(9) 0.0488(8) 0.0349(7) -0.0134(7) -0.0111(6) -0.0074(6) O1 0.0662(9) 0.0856(10) 0.0476(8) -0.0247(8) 0.0051(6) -0.0126(7) O2 0.0656(9) 0.0885(11) 0.0535(8) -0.0167(8) -0.0229(7) -0.0129(7) O3 0.0603(8) 0.0687(9) 0.0640(9) -0.0187(7) 0.0032(7) 0.0018(7) O4 0.0865(11) 0.0710(10) 0.0846(11) -0.0340(8) -0.0475(9) 0.0018(8) S1 0.0529(3) 0.0649(3) 0.0371(2) -0.0147(2) -0.00791(19) -0.0086(2) S2 0.0554(3) 0.0524(3) 0.0496(3) -0.0189(2) -0.0165(2) -0.0002(2) 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 C2 C1 H1A 120.0 C2 C1 H1B 120.0 H1A C1 H1B 120.0 C1 C2 C3 124.6(4) C1 C2 H2 117.7 C3 C2 H2 117.7 N1 C3 C2 111.3(2) N1 C3 H3A 109.4 C2 C3 H3A 109.4 N1 C3 H3B 109.4 C2 C3 H3B 109.4 H3A C3 H3B 108.0 N2 C4 C5 111.7(2) N2 C4 H4 124.2 C5 C4 H4 124.2 C6 C5 C10 119.11(19) C6 C5 C4 104.1(2) C10 C5 C4 136.8(2) N1 C6 C7 131.43(19) N1 C6 C5 106.56(19) C7 C6 C5 122.02(18) C8 C7 C6 117.81(18) C8 C7 H7 121.1 C6 C7 H7 121.1 C7 C8 C9 121.28(19) C7 C8 H8 119.4 C9 C8 H8 119.4 C10 C9 C8 120.84(17) C10 C9 N3 119.27(16) C8 C9 N3 119.79(17) C9 C10 C5 118.93(18) C9 C10 H10 120.5 C5 C10 H10 120.5 C16 C11 C12 120.0(2) C16 C11 S1 120.87(17) C12 C11 S1 119.12(16) C13 C12 C11 119.9(2) C13 C12 H12 120.0 C11 C12 H12 120.0 C12 C13 C14 121.3(3) C12 C13 H13 119.4 C14 C13 H13 119.4 C15 C14 C13 118.1(2) C15 C14 C17 120.2(3) C13 C14 C17 121.7(3) C14 C15 C16 122.1(2) C14 C15 H15 119.0 C16 C15 H15 119.0 C11 C16 C15 118.6(2) C11 C16 H16 120.7 C15 C16 H16 120.7 C14 C17 H17A 109.5 C14 C17 H17B 109.5 H17A C17 H17B 109.5 C14 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C19 C18 H18A 120.0 C19 C18 H18B 120.0 H18A C18 H18B 120.0 C18 C19 C20 124.7(2) C18 C19 H19 117.6 C20 C19 H19 117.6 N4 C20 C19 111.89(16) N4 C20 H20A 109.2 C19 C20 H20A 109.2 N4 C20 H20B 109.2 C19 C20 H20B 109.2 H20A C20 H20B 107.9 N5 C21 C22 111.35(15) N5 C21 H21 124.3 C22 C21 H21 124.3 C23 C22 C27 120.20(15) C23 C22 C21 135.59(16) C27 C22 C21 104.21(15) C24 C23 C22 117.89(15) C24 C23 H23 121.1 C22 C23 H23 121.1 C23 C24 C25 121.15(15) C23 C24 N6 118.47(15) C25 C24 N6 120.37(14) C26 C25 C24 122.00(16) C26 C25 H25 119.0 C24 C25 H25 119.0 C25 C26 C27 117.11(16) C25 C26 H26 121.4 C27 C26 H26 121.4 N4 C27 C26 131.53(16) N4 C27 C22 106.84(14) C26 C27 C22 121.63(15) C29 C28 C33 120.04(18) C29 C28 S2 120.13(14) C33 C28 S2 119.67(14) C30 C29 C28 119.62(18) C30 C29 H29 120.2 C28 C29 H29 120.2 C29 C30 C31 121.56(19) C29 C30 H30 119.2 C31 C30 H30 119.2 C30 C31 C32 117.79(19) C30 C31 C34 120.7(2) C32 C31 C34 121.5(2) C33 C32 C31 121.6(2) C33 C32 H32 119.2 C31 C32 H32 119.2 C32 C33 C28 119.35(19) C32 C33 H33 120.3 C28 C33 H33 120.3 C31 C34 H34A 109.5 C31 C34 H34B 109.5 H34A C34 H34B 109.5 C31 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 N2 N1 C6 111.58(18) N2 N1 C3 120.2(2) C6 N1 C3 128.1(2) C4 N2 N1 106.1(2) C9 N3 S1 123.01(12) C9 N3 H3N 114.5 S1 N3 H3N 110.5 C27 N4 N5 111.13(13) C27 N4 C20 128.27(15) N5 N4 C20 120.10(14) C21 N5 N4 106.45(14) C24 N6 S2 118.67(11) C24 N6 H6N 114.2 S2 N6 H6N 108.4 O2 S1 O1 118.84(9) O2 S1 N3 109.12(8) O1 S1 N3 104.33(8) O2 S1 C11 108.08(9) O1 S1 C11 107.75(9) N3 S1 C11 108.31(9) O4 S2 O3 120.18(10) O4 S2 N6 105.67(9) O3 S2 N6 106.80(8) O4 S2 C28 108.23(9) O3 S2 C28 108.43(9) N6 S2 C28 106.79(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.252(4) C1 H1A 0.9300 C1 H1B 0.9300 C2 C3 1.502(4) C2 H2 0.9300 C3 N1 1.450(3) C3 H3A 0.9700 C3 H3B 0.9700 C4 N2 1.317(3) C4 C5 1.417(3) C4 H4 0.9300 C5 C6 1.400(3) C5 C10 1.406(3) C6 N1 1.364(3) C6 C7 1.388(3) C7 C8 1.368(3) C7 H7 0.9300 C8 C9 1.410(2) C8 H8 0.9300 C9 C10 1.365(3) C9 N3 1.435(2) C10 H10 0.9300 C11 C16 1.380(3) C11 C12 1.384(3) C11 S1 1.762(2) C12 C13 1.370(3) C12 H12 0.9300 C13 C14 1.383(4) C13 H13 0.9300 C14 C15 1.369(4) C14 C17 1.506(4) C15 C16 1.390(4) C15 H15 0.9300 C16 H16 0.9300 C17 H17A 0.9600 C17 H17B 0.9600 C17 H17C 0.9600 C18 C19 1.280(3) C18 H18A 0.9300 C18 H18B 0.9300 C19 C20 1.493(3) C19 H19 0.9300 C20 N4 1.451(2) C20 H20A 0.9700 C20 H20B 0.9700 C21 N5 1.317(2) C21 C22 1.417(2) C21 H21 0.9300 C22 C23 1.402(2) C22 C27 1.404(2) C23 C24 1.372(2) C23 H23 0.9300 C24 C25 1.409(2) C24 N6 1.448(2) C25 C26 1.367(2) C25 H25 0.9300 C26 C27 1.398(2) C26 H26 0.9300 C27 N4 1.359(2) C28 C29 1.376(3) C28 C33 1.384(3) C28 S2 1.7592(18) C29 C30 1.375(3) C29 H29 0.9300 C30 C31 1.382(3) C30 H30 0.9300 C31 C32 1.383(3) C31 C34 1.503(3) C32 C33 1.375(3) C32 H32 0.9300 C33 H33 0.9300 C34 H34A 0.9600 C34 H34B 0.9600 C34 H34C 0.9600 N1 N2 1.355(3) N3 S1 1.6219(16) N3 H3N 0.7979 N4 N5 1.363(2) N6 S2 1.6396(16) N6 H6N 0.7925 O1 S1 1.4337(14) O2 S1 1.4253(14) O3 S2 1.4283(15) O4 S2 1.4260(14) 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 N6 H6N O1 . 0.79 2.11 2.900(2) 176.2 N3 H3N N5 2_576 0.80 2.19 2.983(2) 174.6 C21 H21 O4 2_676 0.93 2.49 3.245(2) 138.1 C7 H7 O2 2_577 0.93 2.48 3.358(2) 157.7 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 C1 C2 C3 N1 -132.5(3) N2 C4 C5 C6 1.2(3) N2 C4 C5 C10 -179.8(3) C10 C5 C6 N1 -179.90(19) C4 C5 C6 N1 -0.6(2) C10 C5 C6 C7 -0.3(3) C4 C5 C6 C7 178.9(2) N1 C6 C7 C8 -179.2(2) C5 C6 C7 C8 1.3(3) C6 C7 C8 C9 -0.8(3) C7 C8 C9 C10 -0.6(3) C7 C8 C9 N3 175.55(18) C8 C9 C10 C5 1.6(3) N3 C9 C10 C5 -174.58(18) C6 C5 C10 C9 -1.1(3) C4 C5 C10 C9 179.9(3) C16 C11 C12 C13 -1.5(3) S1 C11 C12 C13 176.62(18) C11 C12 C13 C14 -0.9(4) C12 C13 C14 C15 2.2(4) C12 C13 C14 C17 -178.1(2) C13 C14 C15 C16 -1.0(4) C17 C14 C15 C16 179.2(2) C12 C11 C16 C15 2.6(3) S1 C11 C16 C15 -175.51(17) C14 C15 C16 C11 -1.3(4) C18 C19 C20 N4 129.8(2) N5 C21 C22 C23 178.45(19) N5 C21 C22 C27 -0.7(2) C27 C22 C23 C24 0.9(2) C21 C22 C23 C24 -178.2(2) C22 C23 C24 C25 -1.6(3) C22 C23 C24 N6 179.38(14) C23 C24 C25 C26 0.9(3) N6 C24 C25 C26 179.90(16) C24 C25 C26 C27 0.5(3) C25 C26 C27 N4 178.88(17) C25 C26 C27 C22 -1.3(3) C23 C22 C27 N4 -179.55(15) C21 C22 C27 N4 -0.22(19) C23 C22 C27 C26 0.6(3) C21 C22 C27 C26 179.88(16) C33 C28 C29 C30 1.6(3) S2 C28 C29 C30 -173.83(15) C28 C29 C30 C31 -0.8(3) C29 C30 C31 C32 -0.6(3) C29 C30 C31 C34 178.9(2) C30 C31 C32 C33 1.3(3) C34 C31 C32 C33 -178.2(2) C31 C32 C33 C28 -0.5(4) C29 C28 C33 C32 -1.0(3) S2 C28 C33 C32 174.52(18) C7 C6 N1 N2 -179.6(2) C5 C6 N1 N2 0.0(2) C7 C6 N1 C3 4.1(4) C5 C6 N1 C3 -176.4(2) C2 C3 N1 N2 -100.4(3) C2 C3 N1 C6 75.7(3) C5 C4 N2 N1 -1.2(3) C6 N1 N2 C4 0.8(3) C3 N1 N2 C4 177.5(2) C10 C9 N3 S1 -124.00(18) C8 C9 N3 S1 59.8(2) C26 C27 N4 N5 -179.05(18) C22 C27 N4 N5 1.07(19) C26 C27 N4 C20 -7.3(3) C22 C27 N4 C20 172.87(17) C19 C20 N4 C27 -81.8(2) C19 C20 N4 N5 89.4(2) C22 C21 N5 N4 1.4(2) C27 N4 N5 C21 -1.5(2) C20 N4 N5 C21 -174.08(16) C23 C24 N6 S2 -90.15(17) C25 C24 N6 S2 90.84(18) C9 N3 S1 O2 -56.27(17) C9 N3 S1 O1 175.74(14) C9 N3 S1 C11 61.16(16) C16 C11 S1 O2 -4.08(19) C12 C11 S1 O2 177.84(16) C16 C11 S1 O1 125.51(17) C12 C11 S1 O1 -52.57(18) C16 C11 S1 N3 -122.18(17) C12 C11 S1 N3 59.74(18) C24 N6 S2 O4 -179.54(13) C24 N6 S2 O3 51.40(15) C24 N6 S2 C28 -64.46(14) C29 C28 S2 O4 -150.75(16) C33 C28 S2 O4 33.78(19) C29 C28 S2 O3 -18.86(18) C33 C28 S2 O3 165.67(17) C29 C28 S2 N6 95.90(16) C33 C28 S2 N6 -79.58(17) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139086223