#------------------------------------------------------------------------------ #$Date: 2024-08-07 01:08:30 +0300 (Wed, 07 Aug 2024) $ #$Revision: 294010 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023155.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_2023155 loop_ _publ_author_name 'Yennawar, Hemant P.' 'Mal, Tapas K.' 'Olsen, Mark A.' 'Lagalante, Anthony F.' 'Louca, Evelyn M.' 'Gavalis, Aloura D.' 'Silverberg, Lee J.' _publ_section_title ; Synthesis and crystal structures of two racemic 2-heteroaryl-3-phenyl-2,3-di-hydro-4H-pyrido[3,2-e][1,3]thia-zin-4-ones. ; _journal_issue 'Pt 7' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 699 _journal_page_last 703 _journal_paper_doi 10.1107/S2056989024005103 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C21 H15 N3 O S, 0.438H2 O' _chemical_formula_moiety 'C21 H15 N3 O S, 0.438(H2 O)' _chemical_formula_sum 'C21 H15.438 N3 O1.44 S' _chemical_formula_weight 364.85 _chemical_name_systematic '2-(1H-Indol-3-yl)-3-phenyl-2,3-dihydro-4H-pyrido[3,2-e][1,3]thiazin-4-one 0.438-hydrate' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5-ac5-024 (compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 111.952(2) _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 28.2424(4) _cell_length_b 11.03070(10) _cell_length_c 28.6936(4) _cell_measurement_reflns_used 15647 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 74.5880 _cell_measurement_theta_min 3.3150 _cell_volume 8290.9(2) _computing_cell_refinement ; CrysAlisPro 1.171.42.93a (Rigaku OD, 2023) ; _computing_data_collection ; CrysAlisPro 1.171.42.93a (Rigaku OD, 2023) ; _computing_data_reduction ; CrysAlisPro 1.171.42.93a (Rigaku OD, 2023) ; _computing_molecular_graphics ; Olex2 1.5-ac5-024 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5-ac5-024 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 173(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.936 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'ROD, Synergy Custom system, HyPix-Arc 150' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_unetI/netI 0.0258 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 26357 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.133 _diffrn_reflns_theta_min 3.321 _diffrn_source 'Rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 1.510 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.65151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2023) ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_density_diffrn 1.168 _exptl_crystal_description block _exptl_crystal_F_000 3032 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.17 _refine_diff_density_max 0.927 _refine_diff_density_min -0.252 _refine_ls_extinction_coef 0.00059(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2018/3 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 492 _refine_ls_number_reflns 8118 _refine_ls_number_restraints 560 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0677 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1597P)^2^+0.3431P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2064 _refine_ls_wR_factor_ref 0.2179 _reflns_number_gt 6592 _reflns_number_total 8118 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL ljs68_auto_a.res in C2/c ljs68_auto.res created by SHELXL-2018/3 at 11:16:40 on 14-May-2024 REM Old TITL ljs68_auto in C2/c REM SHELXT solution in C2/c: R1 0.197, Rweak 0.044, Alpha 0.025 REM 0.774 for 440 systematic absences, Orientation as input REM Formula found by SHELXT: C31 C14 O2 S2 CELL 1.54184 28.2424 11.0307 28.6936 90 111.952 90 ZERR 16 0.0004 0.0001 0.0004 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O S UNIT 336 240 48 23 16 EQIV $1 1-X,1-Y,1-Z EQIV $2 -0.5+X,1.5-Y,-0.5+Z ISOR 0.005 0.01 O3 O6 O4 O5 C10 C11 C38 C39 SIMU DELU TEMP 173 L.S. 50 PLAN 18 SIZE 0.2 0.2 0.17 HTAB N3 O2_$2 HTAB C26 N6_$1 fmap 2 acta OMIT -2 0 4 OMIT -2 2 1 OMIT 0 2 2 OMIT 5 1 3 OMIT 2 2 0 OMIT -5 1 3 OMIT -8 2 6 OMIT 0 2 4 REM REM REM WGHT 0.159700 0.343100 EXTI 0.000592 FVAR 1.89229 S1 5 0.267245 1.022575 0.465863 11.00000 0.05960 0.06340 = 0.05230 -0.00959 0.01295 -0.00496 O1 4 0.293266 0.675868 0.409169 11.00000 0.07916 0.05440 = 0.06892 -0.00551 0.02546 -0.00078 N1 3 0.303010 0.879568 0.409075 11.00000 0.05067 0.05175 = 0.05933 0.00019 0.01695 -0.00031 N2 3 0.189731 0.906490 0.473919 11.00000 0.05679 0.08098 = 0.06566 0.01432 0.02171 0.00638 N3 3 0.174764 1.012087 0.286656 11.00000 0.06906 0.05668 = 0.05414 -0.00161 0.00535 -0.00525 AFIX 43 H3 2 0.154615 0.980900 0.258841 11.00000 -1.20000 AFIX 0 C1 1 0.281977 1.000781 0.409207 11.00000 0.04787 0.05054 = 0.05513 -0.00441 0.01452 -0.00690 AFIX 13 H1 2 0.308920 1.058872 0.411199 11.00000 -1.20000 AFIX 0 C2 1 0.278940 0.777493 0.414887 11.00000 0.05587 0.05286 = 0.04847 -0.00249 0.01010 -0.00285 C3 1 0.234297 0.794348 0.430767 11.00000 0.05010 0.06063 = 0.05157 0.00292 0.00895 -0.00456 C4 1 0.226589 0.896641 0.455172 11.00000 0.04938 0.06393 = 0.04766 0.00598 0.00919 0.00096 C5 1 0.158197 0.812439 0.466945 11.00000 0.05846 0.09243 = 0.08530 0.02486 0.02595 0.00633 AFIX 43 H5 2 0.132288 0.817730 0.479478 11.00000 -1.20000 AFIX 0 C6 1 0.161781 0.707702 0.442205 11.00000 0.05768 0.08517 = 0.09284 0.02167 0.01648 -0.01357 AFIX 43 H6 2 0.138430 0.645049 0.437607 11.00000 -1.20000 AFIX 0 C7 1 0.200935 0.697863 0.424348 11.00000 0.06571 0.06441 = 0.06879 0.00721 0.01289 -0.01133 AFIX 43 H7 2 0.204796 0.627491 0.408270 11.00000 -1.20000 AFIX 0 C8 1 0.349271 0.872710 0.398583 11.00000 0.05397 0.04946 = 0.05659 -0.00261 0.01829 -0.00059 C9 1 0.348170 0.902749 0.351460 11.00000 0.07260 0.07034 = 0.05990 -0.00096 0.02384 0.00402 AFIX 43 H9 2 0.317518 0.921538 0.325509 11.00000 -1.20000 AFIX 0 C10 1 0.394172 0.904300 0.343613 11.00000 0.09991 0.07356 = 0.07558 -0.00498 0.04892 -0.00176 AFIX 43 H10 2 0.394180 0.923974 0.312100 11.00000 -1.20000 AFIX 0 C11 1 0.439558 0.876795 0.382382 11.00000 0.06848 0.07152 = 0.09835 -0.00983 0.04365 0.00196 AFIX 43 H11 2 0.470041 0.878957 0.377004 11.00000 -1.20000 AFIX 0 C12 1 0.439785 0.846928 0.427835 11.00000 0.05765 0.08973 = 0.08891 -0.00373 0.02358 0.01080 AFIX 43 H12 2 0.470460 0.827601 0.453652 11.00000 -1.20000 AFIX 0 C13 1 0.394559 0.844589 0.436728 11.00000 0.05727 0.07818 = 0.06212 0.00212 0.01837 0.00483 AFIX 43 H13 2 0.395056 0.824079 0.468345 11.00000 -1.20000 AFIX 0 C14 1 0.237515 1.029152 0.362485 11.00000 0.05234 0.04643 = 0.05160 0.00133 0.01491 -0.00418 C15 1 0.213853 0.953105 0.323115 11.00000 0.06344 0.04608 = 0.05771 -0.00311 0.01237 -0.00263 AFIX 43 H15 2 0.222979 0.872738 0.321317 11.00000 -1.20000 AFIX 0 C16 1 0.173127 1.129229 0.301926 11.00000 0.06680 0.05438 = 0.05707 0.00634 0.01682 -0.00055 C17 1 0.140683 1.223324 0.276835 11.00000 0.09103 0.07253 = 0.06807 0.01714 0.01665 0.01404 AFIX 43 H17 2 0.114825 1.211520 0.245580 11.00000 -1.20000 AFIX 0 C18 1 0.148468 1.333208 0.300035 11.00000 0.12644 0.06015 = 0.08560 0.02153 0.02871 0.02375 AFIX 43 H18 2 0.127790 1.398271 0.284149 11.00000 -1.20000 AFIX 0 C19 1 0.187248 1.350258 0.347648 11.00000 0.13042 0.04575 = 0.08955 0.00358 0.05013 0.00605 AFIX 43 H19 2 0.191610 1.426651 0.362375 11.00000 -1.20000 AFIX 0 C20 1 0.218963 1.257114 0.373115 11.00000 0.08492 0.04829 = 0.06519 -0.00145 0.03222 -0.00925 AFIX 43 H20 2 0.244057 1.269320 0.404791 11.00000 -1.20000 AFIX 0 C21 1 0.212097 1.143139 0.349601 11.00000 0.05898 0.04616 = 0.05597 0.00116 0.02288 -0.00590 S2 5 0.532076 0.808920 0.579384 11.00000 0.06116 0.05780 = 0.06573 0.00008 0.02338 0.00432 O2 4 0.602559 0.532591 0.688859 11.00000 0.08670 0.06567 = 0.05874 0.00799 -0.00213 -0.02045 N4 3 0.613107 0.707658 0.653076 11.00000 0.06477 0.05551 = 0.04438 -0.00630 0.00998 -0.01529 N5 3 0.469616 0.630955 0.536231 11.00000 0.04682 0.08489 = 0.06928 -0.00542 0.01110 -0.00122 N6 3 0.663289 0.609647 0.535219 11.00000 0.04870 0.08725 = 0.07790 -0.03150 0.01996 -0.00761 AFIX 43 H6A 2 0.681683 0.551779 0.530967 11.00000 -1.20000 AFIX 0 C22 1 0.601063 0.780691 0.607376 11.00000 0.05796 0.05285 = 0.04542 -0.00814 0.01444 -0.01000 AFIX 13 H22 2 0.617659 0.859538 0.617745 11.00000 -1.20000 AFIX 0 C23 1 0.589281 0.599956 0.652500 11.00000 0.06036 0.05585 = 0.05094 -0.00619 0.00930 -0.01201 C24 1 0.544431 0.569350 0.606364 11.00000 0.05142 0.05737 = 0.05326 -0.00792 0.01079 -0.00891 C25 1 0.513947 0.655996 0.573458 11.00000 0.04701 0.06490 = 0.05306 -0.00667 0.01573 -0.00137 C26 1 0.455933 0.513476 0.530470 11.00000 0.05040 0.09417 = 0.07701 -0.01554 0.00411 -0.01739 AFIX 43 H26 2 0.425467 0.493622 0.504472 11.00000 -1.20000 AFIX 0 C27 1 0.483370 0.421387 0.559874 11.00000 0.06199 0.07061 = 0.09334 -0.02149 0.00884 -0.02008 AFIX 43 H27 2 0.471970 0.341705 0.553716 11.00000 -1.20000 AFIX 0 C28 1 0.528673 0.449006 0.599195 11.00000 0.06206 0.05810 = 0.07352 -0.00794 0.00785 -0.01177 AFIX 43 H28 2 0.548071 0.388435 0.620286 11.00000 -1.20000 AFIX 0 C29 1 0.648641 0.756490 0.699092 11.00000 0.06914 0.05462 = 0.04615 -0.00643 0.00875 -0.01557 C30 1 0.629626 0.793123 0.735870 11.00000 0.08214 0.07059 = 0.06024 -0.01132 0.01753 0.00443 AFIX 43 H30 2 0.595434 0.781919 0.730879 11.00000 -1.20000 AFIX 0 C31 1 0.662891 0.846037 0.779494 11.00000 0.11628 0.06894 = 0.05785 -0.01523 0.01997 0.00032 AFIX 43 H31 2 0.651188 0.868089 0.804590 11.00000 -1.20000 AFIX 0 C32 1 0.711962 0.866036 0.786108 11.00000 0.11465 0.06399 = 0.05985 -0.00652 0.00608 -0.02777 AFIX 43 H32 2 0.733482 0.904643 0.815103 11.00000 -1.20000 AFIX 0 C33 1 0.730479 0.830106 0.750578 11.00000 0.08438 0.11354 = 0.08106 -0.00717 0.01492 -0.04782 AFIX 43 H33 2 0.764686 0.842240 0.755844 11.00000 -1.20000 AFIX 0 C34 1 0.697843 0.774981 0.706227 11.00000 0.07511 0.11082 = 0.06046 -0.01065 0.02245 -0.03430 AFIX 43 H34 2 0.710222 0.751269 0.681804 11.00000 -1.20000 AFIX 0 C35 1 0.621903 0.727417 0.570692 11.00000 0.04501 0.06019 = 0.05120 -0.01457 0.01158 -0.01350 C36 1 0.650849 0.624818 0.576404 11.00000 0.04820 0.06990 = 0.06281 -0.01513 0.01232 -0.00917 AFIX 43 H36 2 0.660523 0.573444 0.604098 11.00000 -1.20000 AFIX 0 C37 1 0.641766 0.701529 0.501550 11.00000 0.04982 0.08710 = 0.06253 -0.02516 0.01903 -0.02458 C38 1 0.642399 0.720390 0.453736 11.00000 0.07639 0.11801 = 0.07190 -0.02733 0.03844 -0.02543 AFIX 43 H38 2 0.659817 0.668545 0.440134 11.00000 -1.20000 AFIX 0 C39 1 0.616101 0.819059 0.427772 11.00000 0.09721 0.13907 = 0.07076 -0.01053 0.04058 -0.03752 AFIX 43 H39 2 0.616231 0.834870 0.395984 11.00000 -1.20000 AFIX 0 C40 1 0.589008 0.897018 0.447412 11.00000 0.09070 0.09704 = 0.07062 0.00298 0.02927 -0.02974 AFIX 43 H40 2 0.570973 0.962260 0.428514 11.00000 -1.20000 AFIX 0 C41 1 0.589236 0.876520 0.494778 11.00000 0.06685 0.07300 = 0.06261 -0.00493 0.02167 -0.02223 AFIX 43 H41 2 0.571843 0.928847 0.508220 11.00000 -1.20000 AFIX 0 C42 1 0.615518 0.777374 0.522641 11.00000 0.05083 0.06560 = 0.05231 -0.01580 0.01654 -0.02115 PART 3 O3 4 10.435729 10.497409 10.668991 10.25000 0.20457 0.21898 = 0.21272 0.01138 0.10796 -0.02683 PART 2 O4 4 10.474029 10.693590 10.701120 10.25000 0.23106 0.21624 = 0.20324 0.02386 0.06223 0.01758 PART 1 O6 4 10.420529 10.560530 10.655540 10.25000 0.18111 0.18378 = 0.16601 0.04715 0.07074 0.02386 PART 3 O5 4 10.500000 10.050190 10.750000 10.12500 0.21137 0.23728 = 0.24004 0.00000 0.08095 0.00000 HKLF 4 REM ljs68_auto_a.res in C2/c REM wR2 = 0.2179, GooF = S = 1.091, Restrained GooF = 1.084 for all data REM R1 = 0.0677 for 6592 Fo > 4sig(Fo) and 0.0757 for all 8118 data REM 492 parameters refined using 560 restraints END WGHT 0.1597 0.3431 REM Highest difference peak 0.927, deepest hole -0.252, 1-sigma level 0.113 Q1 1 0.4485 0.6382 0.6707 11.00000 0.05 0.93 Q2 1 0.5098 0.0074 0.7871 11.00000 0.05 0.78 Q3 1 0.4529 0.5832 0.6957 11.00000 0.05 0.78 Q4 1 0.5011 0.1261 0.7728 11.00000 0.05 0.61 Q5 1 0.4660 0.8928 0.6641 11.00000 0.05 0.53 Q6 1 0.5000 0.5250 0.7500 10.50000 0.05 0.53 Q7 1 0.7111 0.6870 0.7042 11.00000 0.05 0.44 Q8 1 0.7498 0.7396 0.7432 11.00000 0.05 0.43 Q9 1 0.6581 0.8238 0.7258 11.00000 0.05 0.35 Q10 1 0.2478 0.9518 0.4604 11.00000 0.05 0.30 Q11 1 0.7466 0.8277 0.7805 11.00000 0.05 0.30 Q12 1 0.5296 0.6196 0.5839 11.00000 0.05 0.29 Q13 1 0.5228 0.7222 0.5754 11.00000 0.05 0.26 Q14 1 0.5991 0.8619 0.4385 11.00000 0.05 0.26 Q15 1 0.6299 0.7657 0.4430 11.00000 0.05 0.25 Q16 1 0.6716 0.7196 0.7045 11.00000 0.05 0.24 Q17 1 0.5611 0.7941 0.5973 11.00000 0.05 0.22 Q18 1 0.2493 1.0031 0.3822 11.00000 0.05 0.22 REM The information below was added by Olex2. REM REM R1 = 0.0677 for 6592 Fo > 4sig(Fo) and 0.0757 for all 27308 data REM 492 parameters refined using n/a restraints REM Highest difference peak 0.93, deepest hole -0.25 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0757 REM R1_gt = 0.0677 REM wR_ref = 0.2179 REM GOOF = 1.091 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 27308 REM Reflections_gt = 6592 REM Parameters = 492 REM Hole = -0.25 REM Peak = 0.93 REM Flack = n/a ; _cod_data_source_file tx2086.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 2023154--2023155.cif.' _cod_database_code 2023155 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.752 _shelx_estimated_absorpt_t_max 0.783 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S S1 0.26724(2) 1.02257(5) 0.46586(2) 0.0607(2) Uani d 1 . . O O1 0.29327(7) 0.67587(14) 0.40917(7) 0.0681(4) Uani d 1 . . N N1 0.30301(7) 0.87957(16) 0.40907(7) 0.0550(4) Uani d 1 . . N N2 0.18973(8) 0.9065(2) 0.47392(8) 0.0682(5) Uani d 1 . . N N3 0.17476(8) 1.01209(17) 0.28666(7) 0.0651(5) Uani d 1 . . H H3 0.154615 0.980900 0.258841 0.078 Uiso calc 1 . . C C1 0.28198(8) 1.00078(19) 0.40921(8) 0.0526(5) Uani d 1 . . H H1 0.308920 1.058872 0.411199 0.063 Uiso calc 1 . . C C2 0.27894(9) 0.77749(19) 0.41489(8) 0.0551(5) Uani d 1 . . C C3 0.23430(8) 0.7943(2) 0.43077(8) 0.0570(5) Uani d 1 . . C C4 0.22659(8) 0.8966(2) 0.45517(8) 0.0563(5) Uani d 1 . . C C5 0.15820(11) 0.8124(3) 0.46694(12) 0.0790(7) Uani d 1 . . H H5 0.132288 0.817730 0.479478 0.095 Uiso calc 1 . . C C6 0.16178(11) 0.7077(3) 0.44220(12) 0.0819(8) Uani d 1 . . H H6 0.138430 0.645049 0.437607 0.098 Uiso calc 1 . . C C7 0.20094(10) 0.6979(2) 0.42435(10) 0.0699(6) Uani d 1 . . H H7 0.204796 0.627491 0.408270 0.084 Uiso calc 1 . . C C8 0.34927(8) 0.87271(19) 0.39858(8) 0.0540(5) Uani d 1 . . C C9 0.34817(11) 0.9027(2) 0.35146(9) 0.0679(6) Uani d 1 . . H H9 0.317518 0.921538 0.325509 0.081 Uiso calc 1 . . C C10 0.39417(13) 0.9043(3) 0.34361(11) 0.0783(7) Uani d 1 . . H H10 0.394180 0.923974 0.312100 0.094 Uiso calc 1 . . C C11 0.43956(11) 0.8768(2) 0.38238(12) 0.0758(7) Uani d 1 . . H H11 0.470041 0.878957 0.377004 0.091 Uiso calc 1 . . C C12 0.43979(11) 0.8469(3) 0.42784(12) 0.0799(7) Uani d 1 . . H H12 0.470460 0.827601 0.453652 0.096 Uiso calc 1 . . C C13 0.39456(9) 0.8446(2) 0.43673(10) 0.0670(6) Uani d 1 . . H H13 0.395056 0.824079 0.468345 0.080 Uiso calc 1 . . C C14 0.23751(8) 1.02915(18) 0.36249(8) 0.0514(5) Uani d 1 . . C C15 0.21385(9) 0.9531(2) 0.32312(8) 0.0587(5) Uani d 1 . . H H15 0.222979 0.872738 0.321317 0.070 Uiso calc 1 . . C C16 0.17313(10) 1.1292(2) 0.30193(9) 0.0612(5) Uani d 1 . . C C17 0.14068(13) 1.2233(3) 0.27683(11) 0.0810(8) Uani d 1 . . H H17 0.114825 1.211520 0.245580 0.097 Uiso calc 1 . . C C18 0.14847(15) 1.3332(3) 0.30004(13) 0.0939(10) Uani d 1 . . H H18 0.127790 1.398271 0.284149 0.113 Uiso calc 1 . . C C19 0.18725(15) 1.3503(2) 0.34765(12) 0.0860(9) Uani d 1 . . H H19 0.191610 1.426651 0.362375 0.103 Uiso calc 1 . . C C20 0.21896(11) 1.2571(2) 0.37311(9) 0.0649(6) Uani d 1 . . H H20 0.244057 1.269320 0.404791 0.078 Uiso calc 1 . . C C21 0.21210(9) 1.14314(18) 0.34960(8) 0.0533(5) Uani d 1 . . S S2 0.53208(2) 0.80892(5) 0.57938(2) 0.0617(2) Uani d 1 . . O O2 0.60256(8) 0.53259(16) 0.68886(7) 0.0789(6) Uani d 1 . . N N4 0.61311(8) 0.70766(16) 0.65308(6) 0.0579(5) Uani d 1 . . N N5 0.46962(7) 0.6310(2) 0.53623(8) 0.0701(5) Uani d 1 . . N N6 0.66329(8) 0.6096(2) 0.53522(9) 0.0724(6) Uani d 1 . . H H6A 0.681683 0.551779 0.530967 0.087 Uiso calc 1 . . C C22 0.60106(8) 0.78069(19) 0.60738(7) 0.0535(5) Uani d 1 . . H H22 0.617659 0.859538 0.617745 0.064 Uiso calc 1 . . C C23 0.58928(9) 0.6000(2) 0.65250(8) 0.0590(5) Uani d 1 . . C C24 0.54443(8) 0.5693(2) 0.60636(8) 0.0566(5) Uani d 1 . . C C25 0.51395(8) 0.6560(2) 0.57346(8) 0.0558(5) Uani d 1 . . C C26 0.45593(10) 0.5135(3) 0.53047(11) 0.0796(8) Uani d 1 . . H H26 0.425467 0.493622 0.504472 0.095 Uiso calc 1 . . C C27 0.48337(11) 0.4214(3) 0.55987(11) 0.0812(8) Uani d 1 . . H H27 0.471970 0.341705 0.553716 0.097 Uiso calc 1 . . C C28 0.52867(10) 0.4490(2) 0.59919(10) 0.0696(6) Uani d 1 . . H H28 0.548071 0.388435 0.620286 0.084 Uiso calc 1 . . C C29 0.64864(9) 0.7565(2) 0.69909(8) 0.0603(6) Uani d 1 . . C C30 0.62963(12) 0.7931(2) 0.73587(10) 0.0736(7) Uani d 1 . . H H30 0.595434 0.781919 0.730879 0.088 Uiso calc 1 . . C C31 0.66289(15) 0.8460(3) 0.77949(10) 0.0847(8) Uani d 1 . . H H31 0.651188 0.868089 0.804590 0.102 Uiso calc 1 . . C C32 0.71196(15) 0.8660(3) 0.78611(11) 0.0872(9) Uani d 1 . . H H32 0.733482 0.904643 0.815103 0.105 Uiso calc 1 . . C C33 0.73048(14) 0.8301(3) 0.75058(13) 0.0976(10) Uani d 1 . . H H33 0.764686 0.842240 0.755844 0.117 Uiso calc 1 . . C C34 0.69784(12) 0.7750(3) 0.70623(10) 0.0830(8) Uani d 1 . . H H34 0.710222 0.751269 0.681804 0.100 Uiso calc 1 . . C C35 0.62190(8) 0.7274(2) 0.57069(8) 0.0540(5) Uani d 1 . . C C36 0.65085(9) 0.6248(2) 0.57640(9) 0.0627(6) Uani d 1 . . H H36 0.660523 0.573444 0.604098 0.075 Uiso calc 1 . . C C37 0.64177(9) 0.7015(3) 0.50155(9) 0.0671(6) Uani d 1 . . C C38 0.64240(12) 0.7204(3) 0.45374(11) 0.0857(8) Uani d 1 . . H H38 0.659817 0.668545 0.440134 0.103 Uiso calc 1 . . C C39 0.61610(14) 0.8191(4) 0.42777(12) 0.0997(10) Uani d 1 . . H H39 0.616231 0.834870 0.395984 0.120 Uiso calc 1 . . C C40 0.58901(13) 0.8970(3) 0.44741(11) 0.0864(8) Uani d 1 . . H H40 0.570973 0.962260 0.428514 0.104 Uiso calc 1 . . C C41 0.58924(10) 0.8765(2) 0.49478(9) 0.0682(6) Uani d 1 . . H H41 0.571843 0.928847 0.508220 0.082 Uiso calc 1 . . C C42 0.61552(8) 0.7774(2) 0.52264(8) 0.0570(5) Uani d 1 . . O O3 0.435729 0.497409 0.668991 0.203(7) Uani d 0.25 A 3 O O4 0.474029 0.693590 0.701120 0.222(8) Uani d 0.25 B 2 O O6 0.420529 0.560530 0.655540 0.175(6) Uani d 0.25 C 1 O O5 0.500000 0.050190 0.750000 0.231(12) Uani d 0.25 D 3 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 0.0596(4) 0.0634(4) 0.0523(3) -0.0050(2) 0.0130(2) -0.0096(2) O1 0.0792(11) 0.0544(9) 0.0689(10) -0.0008(8) 0.0255(9) -0.0055(7) N1 0.0507(10) 0.0517(9) 0.0593(10) -0.0003(7) 0.0169(8) 0.0002(8) N2 0.0568(11) 0.0810(13) 0.0657(11) 0.0064(10) 0.0217(9) 0.0143(10) N3 0.0691(12) 0.0567(10) 0.0541(10) -0.0052(9) 0.0053(9) -0.0016(8) C1 0.0479(11) 0.0505(10) 0.0551(11) -0.0069(8) 0.0145(9) -0.0044(9) C2 0.0559(12) 0.0529(11) 0.0485(10) -0.0029(9) 0.0101(9) -0.0025(9) C3 0.0501(11) 0.0606(12) 0.0516(11) -0.0046(9) 0.0089(9) 0.0029(9) C4 0.0494(11) 0.0639(12) 0.0477(10) 0.0010(9) 0.0092(8) 0.0060(9) C5 0.0585(14) 0.0924(19) 0.0853(18) 0.0063(13) 0.0260(13) 0.0249(15) C6 0.0577(14) 0.0852(18) 0.0928(19) -0.0136(13) 0.0165(13) 0.0217(15) C7 0.0657(14) 0.0644(14) 0.0688(14) -0.0113(11) 0.0129(11) 0.0072(11) C8 0.0540(11) 0.0495(10) 0.0566(11) -0.0006(9) 0.0183(9) -0.0026(9) C9 0.0726(15) 0.0703(14) 0.0599(13) 0.0040(12) 0.0238(11) -0.0010(11) C10 0.0999(19) 0.0736(15) 0.0756(15) -0.0018(14) 0.0489(14) -0.0050(13) C11 0.0685(15) 0.0715(15) 0.0983(18) 0.0020(12) 0.0436(14) -0.0098(13) C12 0.0576(14) 0.0897(19) 0.0889(18) 0.0108(13) 0.0236(13) -0.0037(15) C13 0.0573(13) 0.0782(15) 0.0621(13) 0.0048(11) 0.0184(10) 0.0021(11) C14 0.0523(11) 0.0464(10) 0.0516(10) -0.0042(8) 0.0149(9) 0.0013(8) C15 0.0634(13) 0.0461(10) 0.0577(12) -0.0026(9) 0.0124(10) -0.0031(9) C16 0.0668(14) 0.0544(12) 0.0571(12) -0.0005(10) 0.0168(10) 0.0063(9) C17 0.091(2) 0.0725(16) 0.0681(15) 0.0140(14) 0.0166(14) 0.0171(12) C18 0.126(3) 0.0602(15) 0.0856(19) 0.0237(17) 0.0287(18) 0.0215(14) C19 0.130(3) 0.0457(12) 0.0895(19) 0.0061(14) 0.0501(19) 0.0036(12) C20 0.0849(17) 0.0483(11) 0.0652(13) -0.0093(11) 0.0322(12) -0.0015(10) C21 0.0590(12) 0.0462(10) 0.0560(11) -0.0059(9) 0.0229(9) 0.0012(8) S2 0.0612(4) 0.0578(3) 0.0657(4) 0.0043(2) 0.0234(3) 0.0001(2) O2 0.0867(13) 0.0657(10) 0.0587(9) -0.0204(9) -0.0021(9) 0.0080(8) N4 0.0648(11) 0.0555(10) 0.0444(8) -0.0153(8) 0.0100(8) -0.0063(7) N5 0.0468(10) 0.0849(14) 0.0693(12) -0.0012(9) 0.0111(9) -0.0054(10) N6 0.0487(10) 0.0872(14) 0.0779(13) -0.0076(10) 0.0200(9) -0.0315(11) C22 0.0580(12) 0.0528(11) 0.0454(10) -0.0100(9) 0.0144(9) -0.0081(8) C23 0.0604(13) 0.0559(11) 0.0509(11) -0.0120(10) 0.0093(9) -0.0062(9) C24 0.0514(11) 0.0574(11) 0.0533(11) -0.0089(9) 0.0108(9) -0.0079(9) C25 0.0470(11) 0.0649(12) 0.0531(11) -0.0014(9) 0.0157(9) -0.0067(9) C26 0.0504(13) 0.0942(19) 0.0770(17) -0.0174(13) 0.0041(12) -0.0155(14) C27 0.0620(15) 0.0706(15) 0.0933(19) -0.0201(13) 0.0088(13) -0.0215(14) C28 0.0621(14) 0.0581(12) 0.0735(15) -0.0118(11) 0.0078(11) -0.0079(11) C29 0.0691(14) 0.0546(12) 0.0462(10) -0.0156(10) 0.0087(9) -0.0064(9) C30 0.0821(17) 0.0706(15) 0.0602(13) 0.0044(13) 0.0175(12) -0.0113(11) C31 0.116(2) 0.0689(16) 0.0579(14) 0.0003(16) 0.0200(15) -0.0152(12) C32 0.115(2) 0.0640(15) 0.0599(14) -0.0278(15) 0.0061(15) -0.0065(12) C33 0.084(2) 0.114(3) 0.0811(19) -0.0478(19) 0.0149(15) -0.0072(17) C34 0.0751(17) 0.111(2) 0.0605(14) -0.0343(16) 0.0224(12) -0.0107(14) C35 0.0450(10) 0.0602(12) 0.0512(10) -0.0135(9) 0.0116(8) -0.0146(9) C36 0.0482(11) 0.0699(14) 0.0628(12) -0.0092(10) 0.0123(10) -0.0151(10) C37 0.0498(12) 0.0871(16) 0.0625(13) -0.0246(11) 0.0190(10) -0.0252(12) C38 0.0764(17) 0.118(2) 0.0719(15) -0.0254(16) 0.0384(14) -0.0273(15) C39 0.097(2) 0.139(3) 0.0708(16) -0.0375(19) 0.0406(16) -0.0105(17) C40 0.091(2) 0.097(2) 0.0706(16) -0.0297(16) 0.0293(15) 0.0030(15) C41 0.0668(14) 0.0730(15) 0.0626(13) -0.0222(12) 0.0217(11) -0.0049(11) C42 0.0508(11) 0.0656(12) 0.0523(10) -0.0211(10) 0.0165(9) -0.0158(9) O3 0.205(10) 0.219(11) 0.213(11) -0.027(8) 0.108(8) 0.011(8) O4 0.231(12) 0.216(11) 0.203(11) 0.018(9) 0.062(9) 0.024(8) O6 0.181(9) 0.184(9) 0.166(9) 0.024(8) 0.071(7) 0.047(7) O5 0.211(15) 0.237(15) 0.240(15) 0.000 0.081(10) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l 0 0 2 0 0 3 0 0 -4 0 0 4 0 0 5 0 0 -5 0 0 -6 0 0 6 0 0 7 0 0 -7 0 0 -8 0 0 8 0 0 -9 0 0 9 0 0 10 0 0 10 0 0 11 0 0 11 0 0 -11 0 0 12 0 0 12 0 0 -12 0 0 12 0 0 13 0 0 13 0 0 14 0 0 -14 0 0 14 0 0 -15 0 0 15 0 0 -16 0 0 16 0 0 -17 0 0 17 0 0 18 0 0 -19 0 0 19 0 0 -20 0 0 20 0 0 21 0 0 22 0 0 22 0 0 23 0 0 23 0 0 24 0 0 24 0 0 25 0 0 25 0 0 26 0 0 -26 0 0 -27 0 0 27 0 0 -28 0 0 28 0 0 29 0 0 29 0 0 30 0 0 31 0 0 32 0 0 33 0 -2 0 0 -2 0 0 -2 0 0 -2 0 0 -2 1 0 -2 1 0 -2 1 0 -2 -1 0 -2 1 0 -2 -1 0 -2 -1 0 -2 -1 0 -2 1 0 -2 1 0 -2 -2 0 -2 2 0 -2 -2 0 -2 2 0 -2 2 0 -2 -2 0 -2 2 0 -2 2 0 -2 2 0 2 -2 0 -2 3 0 -2 3 0 -2 3 0 2 -3 0 -2 3 0 -2 -3 0 -2 3 0 2 -3 0 -2 3 0 -2 -3 0 -2 3 0 -2 3 0 2 -4 0 -2 -4 0 -2 4 0 -2 4 0 -2 4 0 -2 -4 0 -2 4 0 -2 4 0 -2 4 0 -2 4 0 2 -4 0 -2 4 0 -2 4 0 -2 4 0 -2 -5 0 -2 5 0 -2 5 0 -2 5 0 -2 5 0 -2 5 0 -2 5 0 -2 5 0 -2 5 0 -2 6 0 -2 6 0 -2 -6 0 -2 6 0 -2 6 0 -2 6 0 -2 6 0 -2 6 0 -2 7 0 -2 7 0 -2 7 0 -2 -7 0 -2 7 0 -2 7 0 -2 7 0 -2 8 0 -2 8 0 -2 8 0 -2 8 0 -2 -8 0 2 -8 0 -2 8 0 -2 8 0 -2 9 0 -2 9 0 -2 -9 0 2 -9 0 -2 9 0 -2 9 0 -2 9 0 -2 10 0 -2 -10 0 2 -10 0 -2 10 0 -2 10 0 -2 10 0 -2 10 0 -2 10 0 -2 -11 0 2 -11 0 -2 11 0 -2 11 0 -2 12 0 -2 12 0 -2 -12 0 -2 12 0 2 -12 0 -2 12 0 -2 -13 0 -2 13 0 -2 13 0 -2 13 0 -2 13 0 -2 -14 0 -2 14 0 -2 15 0 -2 15 0 -2 15 0 -2 16 0 -2 16 0 -2 17 0 -2 17 0 -2 17 0 -2 -17 0 2 18 0 -2 18 0 -2 18 0 -2 18 0 -2 -18 0 -2 19 0 2 19 0 -2 19 0 -2 19 0 -2 -19 0 -2 20 0 -2 20 0 -2 -20 0 -2 20 0 2 20 0 -2 21 0 2 21 0 -2 21 0 -2 -21 0 -2 21 0 -2 22 0 -2 22 0 -2 -22 0 -2 22 0 -2 23 0 -2 23 0 -2 23 0 -2 24 0 -2 24 0 -2 24 0 -2 25 0 -2 26 0 -2 26 0 -2 26 0 -2 27 0 -2 27 0 -2 -28 0 -2 28 0 2 28 0 -2 28 0 -2 -29 0 -2 29 0 2 29 0 -2 29 0 2 30 0 -2 30 0 -2 -30 0 -2 31 0 -2 -31 0 2 31 0 -2 32 0 2 32 0 -4 0 0 -4 0 0 -4 0 0 -4 1 0 -4 -1 0 -4 1 0 -4 -1 0 -4 1 0 -4 -1 0 -4 1 0 -4 -1 0 4 -2 0 -4 -2 0 -4 2 0 -4 2 0 -4 -2 0 -4 2 0 -4 2 0 -4 -2 0 -4 -2 0 -4 -3 0 -4 3 0 -4 -3 0 -4 3 0 -4 3 0 -4 3 0 -4 -3 0 -4 3 0 4 -3 0 4 -4 0 -4 4 0 -4 4 0 -4 -4 0 -4 4 0 -4 4 0 -4 4 0 -4 -4 0 -4 4 0 -4 4 0 4 -4 0 -4 -4 0 -4 5 0 -4 5 0 -4 5 0 -4 5 0 -4 5 0 -4 -5 0 -4 5 0 -4 5 0 -4 5 0 -4 6 0 -4 6 0 -4 6 0 -4 6 0 -4 6 0 -4 6 0 -4 -6 0 -4 6 0 -4 6 0 -4 7 0 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32 2 -16 32 -2 -16 -32 2 16 -32 -2 15 32 -2 -15 -32 2 15 -32 -2 14 -32 2 14 -32 -2 13 -32 2 13 -32 2 12 -32 -2 12 -32 2 11 -32 -2 11 -32 2 10 -32 -2 10 32 -2 -10 -32 -2 9 -32 2 9 32 -2 -9 -32 2 8 -32 -2 8 32 -2 -8 -32 2 7 -32 -2 7 32 -2 -7 -32 2 6 -32 -2 6 32 -2 -6 -32 2 5 -32 -2 5 32 -2 -5 -32 2 4 -32 -2 4 32 -2 -4 -32 -2 3 -32 -2 2 -32 -2 1 -32 -4 20 32 4 -20 -32 -4 19 32 4 -19 -32 -4 18 32 4 -18 32 4 -17 -32 4 17 32 -4 -16 32 4 -16 -32 4 16 -32 4 15 32 -4 -15 -32 4 14 32 -4 -14 -32 4 13 32 -4 -13 -32 4 12 32 -4 -12 -32 4 11 32 -4 -11 32 4 -10 32 -4 -10 32 4 -9 32 -4 -9 -32 -4 8 32 4 -8 32 -4 -8 -32 -4 7 32 4 -7 32 -4 -7 -32 -4 6 32 4 -6 -32 -4 5 32 4 -5 33 1 -24 33 -1 -24 33 1 -23 33 -1 -23 33 1 -22 33 -1 -22 -33 1 21 33 -1 -21 33 1 -21 -33 -1 20 -33 1 20 33 -1 -20 33 1 -20 -33 -1 19 -33 1 19 33 1 -19 33 -1 -19 -33 -1 18 -33 1 18 33 -1 -18 33 1 -18 -33 -1 17 -33 1 17 33 -1 -17 33 1 -17 33 -1 -16 33 1 -16 -33 1 16 -33 -1 16 33 -1 -15 33 1 -15 -33 -1 15 -33 1 15 33 1 -14 33 -1 -14 -33 1 14 -33 -1 14 33 -1 -13 -33 -1 13 -33 1 13 -33 1 12 -33 -1 12 33 -1 -11 -33 -1 11 -33 1 11 33 -1 -10 -33 1 10 -33 -1 10 33 -1 -9 -33 1 9 -33 -1 9 33 -1 -8 -33 1 8 -33 -1 8 -33 1 7 -33 -1 7 -33 1 6 -33 -1 6 -33 -1 5 -33 1 5 -33 -1 4 -33 -1 3 33 3 -21 33 3 -20 -33 -3 19 33 3 -19 -33 3 18 33 3 -18 -33 3 17 33 3 -17 33 -3 -16 -33 3 16 33 3 -16 33 -3 -15 -33 3 15 33 3 -15 33 -3 -14 -33 3 14 33 -3 -13 -33 3 13 33 -3 -12 -33 3 12 -33 -3 12 33 -3 -11 -33 3 11 -33 -3 11 33 -3 -10 -33 -3 10 -33 -3 9 -33 -3 8 -33 -3 7 -33 -3 6 34 0 -22 34 0 -21 34 0 -20 34 0 -19 -34 0 18 34 0 -18 -34 0 17 34 0 -17 -34 0 16 34 0 -16 -34 0 15 34 0 -15 -34 0 14 34 0 -14 -34 0 13 34 0 -13 -34 0 12 34 0 -12 -34 0 11 -34 0 10 -34 0 9 -34 0 8 -34 0 7 34 2 -21 34 2 -20 34 2 -19 34 2 -18 -34 2 17 34 2 -17 -34 2 16 34 2 -16 -34 2 15 34 2 -15 -34 2 14 -34 -2 14 34 2 -14 -34 2 13 -34 -2 13 34 2 -13 -34 2 12 34 2 -12 -34 -2 12 -34 -2 11 -34 -2 10 -34 -2 9 34 4 -13 34 4 -12 34 4 -11 35 1 -18 35 1 -17 35 1 -16 35 1 -15 35 1 -14 35 1 -13 35 1 -12 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 C4 S1 C1 . . 95.25(10) ? C2 N1 C1 . . 122.35(18) ? C2 N1 C8 . . 120.96(17) ? C8 N1 C1 . . 116.54(16) ? C5 N2 C4 . . 116.8(2) ? C15 N3 C16 . . 108.53(19) ? N1 C1 S1 . . 110.37(14) ? N1 C1 C14 . . 113.36(17) ? C14 C1 S1 . . 112.06(15) ? O1 C2 N1 . . 122.5(2) ? O1 C2 C3 . . 120.7(2) ? N1 C2 C3 . . 116.73(19) ? C4 C3 C2 . . 124.1(2) ? C7 C3 C2 . . 118.0(2) ? C7 C3 C4 . . 117.6(2) ? N2 C4 S1 . . 114.87(18) ? N2 C4 C3 . . 124.0(2) ? C3 C4 S1 . . 121.08(17) ? N2 C5 C6 . . 123.8(3) ? C5 C6 C7 . . 118.6(3) ? C6 C7 C3 . . 119.1(3) ? C9 C8 N1 . . 119.9(2) ? C13 C8 N1 . . 119.4(2) ? C13 C8 C9 . . 120.5(2) ? C8 C9 C10 . . 118.6(2) ? C11 C10 C9 . . 120.4(3) ? C12 C11 C10 . . 120.2(3) ? C11 C12 C13 . . 120.7(3) ? C8 C13 C12 . . 119.6(2) ? C15 C14 C1 . . 127.15(19) ? C15 C14 C21 . . 106.50(19) ? C21 C14 C1 . . 126.33(19) ? C14 C15 N3 . . 110.2(2) ? N3 C16 C17 . . 129.1(2) ? N3 C16 C21 . . 107.8(2) ? C17 C16 C21 . . 123.0(2) ? C18 C17 C16 . . 117.1(3) ? C17 C18 C19 . . 121.2(3) ? C20 C19 C18 . . 122.0(3) ? C19 C20 C21 . . 117.8(3) ? C16 C21 C14 . . 106.90(19) ? C20 C21 C14 . . 134.3(2) ? C20 C21 C16 . . 118.8(2) ? C25 S2 C22 . . 95.91(10) ? C23 N4 C22 . . 121.32(17) ? C23 N4 C29 . . 120.80(18) ? C29 N4 C22 . . 117.79(17) ? C25 N5 C26 . . 116.0(2) ? C36 N6 C37 . . 109.2(2) ? N4 C22 S2 . . 109.75(15) ? N4 C22 C35 . . 112.98(19) ? C35 C22 S2 . . 112.90(14) ? O2 C23 N4 . . 121.9(2) ? O2 C23 C24 . . 120.6(2) ? N4 C23 C24 . . 117.4(2) ? C25 C24 C23 . . 123.5(2) ? C28 C24 C23 . . 117.8(2) ? C28 C24 C25 . . 118.2(2) ? N5 C25 S2 . . 115.41(18) ? N5 C25 C24 . . 123.9(2) ? C24 C25 S2 . . 120.72(16) ? N5 C26 C27 . . 124.9(2) ? C26 C27 C28 . . 118.6(3) ? C27 C28 C24 . . 118.5(2) ? C30 C29 N4 . . 117.8(2) ? C34 C29 N4 . . 121.8(2) ? C34 C29 C30 . . 120.3(2) ? C31 C30 C29 . . 118.6(3) ? C32 C31 C30 . . 120.8(3) ? C31 C32 C33 . . 120.6(3) ? C32 C33 C34 . . 119.9(3) ? C29 C34 C33 . . 119.8(3) ? C36 C35 C22 . . 127.7(2) ? C36 C35 C42 . . 106.7(2) ? C42 C35 C22 . . 125.6(2) ? N6 C36 C35 . . 109.5(2) ? N6 C37 C38 . . 129.5(3) ? N6 C37 C42 . . 107.7(2) ? C38 C37 C42 . . 122.8(3) ? C39 C38 C37 . . 116.7(3) ? C38 C39 C40 . . 122.4(3) ? C41 C40 C39 . . 119.7(3) ? C40 C41 C42 . . 120.0(3) ? C37 C42 C35 . . 106.9(2) ? C41 C42 C35 . . 134.6(2) ? C41 C42 C37 . . 118.5(2) ? 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 C1 . 1.838(2) ? S1 C4 . 1.755(2) ? O1 C2 . 1.223(3) ? N1 C1 . 1.464(3) ? N1 C2 . 1.357(3) ? N1 C8 . 1.448(3) ? N2 C4 . 1.343(3) ? N2 C5 . 1.333(4) ? N3 C15 . 1.369(3) ? N3 C16 . 1.371(3) ? C1 C14 . 1.488(3) ? C2 C3 . 1.504(3) ? C3 C4 . 1.387(3) ? C3 C7 . 1.387(3) ? C5 C6 . 1.379(5) ? C6 C7 . 1.386(4) ? C8 C9 . 1.381(3) ? C8 C13 . 1.372(3) ? C9 C10 . 1.399(4) ? C10 C11 . 1.381(4) ? C11 C12 . 1.343(4) ? C12 C13 . 1.393(4) ? C14 C15 . 1.365(3) ? C14 C21 . 1.426(3) ? C16 C17 . 1.394(3) ? C16 C21 . 1.407(3) ? C17 C18 . 1.361(4) ? C18 C19 . 1.408(5) ? C19 C20 . 1.379(4) ? C20 C21 . 1.406(3) ? S2 C22 . 1.835(2) ? S2 C25 . 1.753(2) ? O2 C23 . 1.220(3) ? N4 C22 . 1.467(3) ? N4 C23 . 1.362(3) ? N4 C29 . 1.432(3) ? N5 C25 . 1.336(3) ? N5 C26 . 1.345(4) ? N6 C36 . 1.363(3) ? N6 C37 . 1.375(4) ? C22 C35 . 1.504(3) ? C23 C24 . 1.489(3) ? C24 C25 . 1.392(3) ? C24 C28 . 1.391(3) ? C26 C27 . 1.362(4) ? C27 C28 . 1.387(3) ? C29 C30 . 1.410(4) ? C29 C34 . 1.342(4) ? C30 C31 . 1.382(4) ? C31 C32 . 1.345(5) ? C32 C33 . 1.367(5) ? C33 C34 . 1.401(4) ? C35 C36 . 1.370(3) ? C35 C42 . 1.432(3) ? C37 C38 . 1.394(4) ? C37 C42 . 1.397(3) ? C38 C39 . 1.370(5) ? C39 C40 . 1.402(5) ? C40 C41 . 1.375(4) ? C41 C42 . 1.394(4) ? 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 N3 H3 O2 8_465 0.86 2.00 2.828(3) 160.7 yes C26 H26 N6 5_666 0.93 2.60 3.463(3) 155.1 yes