#------------------------------------------------------------------------------ #$Date: 2024-10-09 03:51:26 +0300 (Wed, 09 Oct 2024) $ #$Revision: 295374 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/01/7160175.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7160175 loop_ _publ_author_name 'Duari, Surajit' 'Biswas, Subrata' 'Roy, Arnab' 'Maity, Srabani' 'Elsharif, Asma' 'Biswas, Srijit' _publ_section_title ; MeOTf- catalyzed Friedel-Crafts alkylation of benzoxazolones, benzothiazolones, indolinones and benzimidazolones with activated secondary alcohols ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D4OB01372G _journal_year 2024 _chemical_formula_moiety 'C15 H13 N O S' _chemical_formula_sum 'C15 H13 N O S' _chemical_formula_weight 255.32 _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-05-30 _audit_creation_method ; Olex2 1.5 (compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439) ; _audit_update_record ; 2024-06-29 deposited with the CCDC. 2024-10-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 13.3265(16) _cell_length_b 6.1652(8) _cell_length_c 31.478(4) _cell_measurement_reflns_used 5589 _cell_measurement_temperature 180.00 _cell_measurement_theta_max 26.44 _cell_measurement_theta_min 2.59 _cell_volume 2586.2(6) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 180.00 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1034 _diffrn_reflns_av_unetI/netI 0.0813 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_number 30386 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.560 _diffrn_reflns_theta_min 2.588 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4650 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1452 before and 0.0995 after correction. The Ratio of minimum to maximum transmission is 0.6237. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear whiteish white' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier whiteish _exptl_crystal_colour_primary white _exptl_crystal_density_diffrn 1.311 _exptl_crystal_description block _exptl_crystal_F_000 1072 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: 1:1 mixture of DCM and MeOH' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.365 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.049 _refine_ls_abs_structure_details ; Flack x determined using 1329 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.40(10) _refine_ls_extinction_coef 0.013(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 328 _refine_ls_number_reflns 5878 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.1179 _refine_ls_R_factor_gt 0.0562 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.7114P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1283 _refine_ls_wR_factor_ref 0.1687 _reflns_Friedel_coverage 0.946 _reflns_Friedel_fraction_full 0.982 _reflns_Friedel_fraction_max 0.977 _reflns_number_gt 3461 _reflns_number_total 5878 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob01372g2.cif _cod_data_source_block sdom186 _cod_database_code 7160175 _shelx_shelxl_version_number 2016/6 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C8(H8), C23(H23) 2.b Aromatic/amide H refined with riding coordinates: N1(H1), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), N2(H2), C19(H19), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29) 2.c Idealised Me refined as rotating group: C15(H15A,H15B,H15C), C30(H30A,H30B,H30C) ; _shelx_res_file ; TITL sdom186_a.res in Pca2(1) sdom186.res created by SHELXL-2016/6 at 19:33:14 on 30-May-2024 REM Old TITL sdom186 in Pbcm #57 REM SHELXT solution in Pca2(1) REM R1 0.218, Rweak 0.012, Alpha 0.007, Orientation as input REM Flack x = 0.476 ( 0.076 ) from Parsons' quotients REM Formula found by SHELXT: C28 N2 O4 S2 CELL 0.71073 13.3265 6.1652 31.4778 90 90 90 ZERR 8 0.0016 0.0008 0.0043 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H N O S UNIT 120 104 8 8 8 L.S. 10 0 0 PLAN 2 TEMP -113.17 CONF BOND $H list 4 fmap 2 53 ACTA MORE -1 OMIT 6 0 -3 OMIT 0 2 8 OMIT 4 0 9 OMIT 2 3 6 OMIT 0 0 26 OMIT 1 1 3 OMIT 2 4 3 OMIT 6 0 3 OMIT 6 5 -28 OMIT 12 2 16 OMIT 0 4 22 OMIT 2 3 12 OMIT 11 4 10 OMIT 0 6 18 OMIT 3 6 3 OMIT 17 1 4 OMIT 2 5 26 OMIT 1 7 -8 OMIT 14 1 -12 OMIT 14 1 7 OMIT 15 2 -4 OMIT 0 0 38 OMIT 16 3 1 OMIT 6 6 -15 OMIT 0 0 34 OMIT 9 4 25 OMIT 0 2 -8 OMIT 2 3 22 OMIT 0 3 12 OMIT 6 1 23 OMIT 8 1 19 OMIT 14 3 -15 OMIT 0 1 -16 OMIT 14 2 10 OMIT 15 2 1 OMIT 14 2 16 OMIT 2 3 -6 OMIT 14 3 15 OMIT 8 0 4 OMIT 2 5 11 OMIT 17 1 -3 OMIT 15 2 -5 OMIT 0 5 18 OMIT 5 5 4 OMIT 10 3 -1 OMIT 17 1 2 OMIT 9 2 -15 OMIT 1 5 -20 OMIT 8 7 2 OMIT 4 4 7 REM REM REM WGHT 0.065000 0.711400 EXTI 0.013441 FVAR 0.64732 S1 5 0.223047 -0.109546 0.571460 11.00000 0.03381 0.08441 = 0.07477 0.02897 0.00853 0.00016 O1 4 0.242107 0.229141 0.519583 11.00000 0.04083 0.08528 = 0.07184 0.02987 0.00689 0.00319 N1 3 0.380458 0.013308 0.531461 11.00000 0.03446 0.06605 = 0.05029 0.01123 0.00703 -0.00448 AFIX 43 H1 2 0.421649 0.084732 0.514676 11.00000 -1.20000 AFIX 0 C1 1 0.284034 0.071779 0.536709 11.00000 0.03309 0.07996 = 0.04834 0.01035 0.00502 -0.00212 C2 1 0.410239 -0.166895 0.554304 11.00000 0.03555 0.06163 = 0.04424 -0.00058 0.00146 -0.00262 C3 1 0.335068 -0.254627 0.578884 11.00000 0.03917 0.05484 = 0.05527 0.00718 0.00079 -0.00659 C4 1 0.352556 -0.431163 0.605274 11.00000 0.04529 0.06950 = 0.06143 0.00988 -0.00018 -0.01273 AFIX 43 H4 2 0.299969 -0.489210 0.622183 11.00000 -1.20000 AFIX 0 C5 1 0.447137 -0.520978 0.606608 11.00000 0.04772 0.05967 = 0.07298 0.00549 -0.01163 -0.00394 C6 1 0.522412 -0.431287 0.580262 11.00000 0.04151 0.06180 = 0.07032 0.00158 0.00261 0.00787 AFIX 43 H6 2 0.587266 -0.495248 0.580398 11.00000 -1.20000 AFIX 0 C7 1 0.505647 -0.257559 0.554811 11.00000 0.04192 0.06317 = 0.06007 0.00016 0.00977 -0.00309 AFIX 43 H7 2 0.557890 -0.199277 0.537742 11.00000 -1.20000 AFIX 0 C8 1 0.476508 -0.713219 0.634329 11.00000 0.06136 0.06026 = 0.07017 0.00418 -0.00536 -0.00068 AFIX 13 H8 2 0.505006 -0.826827 0.615131 11.00000 -1.20000 AFIX 0 C9 1 0.559089 -0.651915 0.666387 11.00000 0.05324 0.05627 = 0.06520 0.01500 0.00487 0.00074 C10 1 0.560665 -0.453988 0.686617 11.00000 0.07536 0.07003 = 0.08063 0.00634 -0.00597 0.01291 AFIX 43 H10 2 0.510390 -0.349449 0.680404 11.00000 -1.20000 AFIX 0 C11 1 0.635025 -0.405760 0.716004 11.00000 0.11111 0.06352 = 0.07292 -0.00761 0.00288 -0.00080 AFIX 43 H11 2 0.635909 -0.267195 0.729201 11.00000 -1.20000 AFIX 0 C12 1 0.707679 -0.556218 0.726322 11.00000 0.07467 0.10671 = 0.06341 0.02083 -0.00437 -0.00297 AFIX 43 H12 2 0.758444 -0.523153 0.746496 11.00000 -1.20000 AFIX 0 C13 1 0.704687 -0.757898 0.706394 11.00000 0.06271 0.09452 = 0.07342 0.00360 -0.00478 0.01509 AFIX 43 H13 2 0.753473 -0.864816 0.713156 11.00000 -1.20000 AFIX 0 C14 1 0.631368 -0.802523 0.676993 11.00000 0.05958 0.07491 = 0.05783 0.00931 0.00913 0.01738 AFIX 43 H14 2 0.630433 -0.940661 0.663627 11.00000 -1.20000 AFIX 0 C15 1 0.388638 -0.815463 0.657890 11.00000 0.07835 0.07884 = 0.09966 0.02521 -0.01540 -0.01750 AFIX 137 H15A 2 0.362879 -0.712966 0.679040 11.00000 -1.50000 H15B 2 0.411153 -0.948046 0.672176 11.00000 -1.50000 H15C 2 0.335330 -0.851180 0.637617 11.00000 -1.50000 AFIX 0 S2 5 0.522016 0.609440 0.428909 11.00000 0.03492 0.08681 = 0.07378 0.03067 0.00736 0.00006 O2 4 0.503090 0.273748 0.481211 11.00000 0.03935 0.08671 = 0.08001 0.03505 0.00961 0.00700 N2 3 0.364920 0.488929 0.469335 11.00000 0.03544 0.06456 = 0.04598 0.01269 0.00343 -0.00271 AFIX 43 H2 2 0.323806 0.419583 0.486484 11.00000 -1.20000 AFIX 0 C16 1 0.461063 0.428327 0.464340 11.00000 0.03753 0.07572 = 0.05138 0.01845 0.00087 -0.00001 C17 1 0.334105 0.669251 0.445577 11.00000 0.03502 0.05526 = 0.04367 0.00048 -0.00194 -0.00588 C18 1 0.410719 0.754736 0.421263 11.00000 0.03544 0.06114 = 0.05540 0.00885 0.00147 -0.00423 C19 1 0.392711 0.930778 0.395150 11.00000 0.04382 0.07090 = 0.06352 0.02220 0.00016 -0.00395 AFIX 43 H19 2 0.445012 0.988851 0.378086 11.00000 -1.20000 AFIX 0 C20 1 0.296624 1.022720 0.394089 11.00000 0.05042 0.05930 = 0.05552 0.00425 -0.00166 -0.00204 C21 1 0.222096 0.936373 0.419389 11.00000 0.03830 0.06504 = 0.08137 0.00144 0.00024 0.00110 AFIX 43 H21 2 0.157264 1.000408 0.418993 11.00000 -1.20000 AFIX 0 C22 1 0.239152 0.760352 0.445121 11.00000 0.03501 0.06168 = 0.05551 0.00366 0.00694 -0.00134 AFIX 43 H22 2 0.186934 0.702342 0.462239 11.00000 -1.20000 AFIX 0 C23 1 0.270096 1.216724 0.366039 11.00000 0.06514 0.05854 = 0.08489 0.01063 -0.00498 0.00221 AFIX 13 H23 2 0.243458 1.330918 0.385579 11.00000 -1.20000 AFIX 0 C24 1 0.187332 1.168336 0.335135 11.00000 0.05238 0.05574 = 0.06614 0.00726 0.00082 0.00511 C25 1 0.175876 0.974914 0.314669 11.00000 0.06482 0.06716 = 0.08645 -0.00073 -0.01380 0.01158 AFIX 43 H25 2 0.221574 0.860956 0.320864 11.00000 -1.20000 AFIX 0 C26 1 0.101018 0.937515 0.285429 11.00000 0.08086 0.08218 = 0.07228 -0.00048 -0.00461 0.00652 AFIX 43 H26 2 0.096396 0.800567 0.271734 11.00000 -1.20000 AFIX 0 C27 1 0.033733 1.096166 0.276128 11.00000 0.07145 0.09723 = 0.06639 -0.00200 -0.00854 -0.00022 AFIX 43 H27 2 -0.018966 1.070276 0.256447 11.00000 -1.20000 AFIX 0 C28 1 0.042980 1.293232 0.295477 11.00000 0.06396 0.09977 = 0.07099 0.01900 -0.00125 0.02823 AFIX 43 H28 2 -0.003369 1.405689 0.289100 11.00000 -1.20000 AFIX 0 C29 1 0.119575 1.330390 0.324379 11.00000 0.06492 0.06268 = 0.06503 0.00660 0.00799 0.01514 AFIX 43 H29 2 0.125830 1.469516 0.337079 11.00000 -1.20000 AFIX 0 C30 1 0.358604 1.317115 0.343509 11.00000 0.07603 0.08382 = 0.10270 0.03298 -0.01400 -0.02162 AFIX 137 H30A 2 0.410571 1.353981 0.364320 11.00000 -1.50000 H30B 2 0.336958 1.448920 0.328715 11.00000 -1.50000 H30C 2 0.385760 1.213638 0.322861 11.00000 -1.50000 AFIX 0 HKLF 4 REM sdom186_a.res in Pca2(1) REM R1 = 0.0562 for 3461 Fo > 4sig(Fo) and 0.1179 for all 5878 data REM 328 parameters refined using 1 restraints END WGHT 0.0650 0.7113 REM Highest difference peak 0.365, deepest hole -0.221, 1-sigma level 0.049 Q1 1 0.5336 0.3989 0.4250 11.00000 0.05 0.37 Q2 1 0.2330 0.1011 0.5762 11.00000 0.05 0.36 ; _shelx_res_checksum 91237 _shelx_hkl_file ; 0 1 0 41.90 6.70 0 1 0 44.80 6.90 0 1 0 32.80 5.80 0 -1 0 42.30 6.50 0 -1 0 51.69 7.00 0 -1 0 35.80 6.50 0 -2 0 116.79 14.70 0 -2 0 100.89 14.50 0 -2 0 140.79 14.70 0 2 0 100.69 14.10 0 2 0 121.19 15.20 0 2 0 117.09 15.00 0 -3 0 18.80 7.50 0 3 0 21.40 8.40 0 3 0 25.30 7.80 0 -3 0 8.00 5.70 0 -3 0 26.70 7.70 0 4 0 145.79 24.20 0 -4 0 179.28 22.60 0 4 0 147.89 21.80 0 -4 0 158.88 21.80 0 -4 0 150.78 21.40 0 -5 0 17.40 9.30 0 5 0 7.30 9.20 0 -5 0 -2.00 6.40 0 -6 0 71.99 19.10 0 -6 0 71.19 16.50 0 6 0 62.39 18.20 0 -7 0 0.70 8.60 0 -7 0 0.00 10.00 0 7 0 -5.00 10.40 0 7 0 -4.10 10.00 0 -8 0 -18.70 11.10 0 8 0 3.10 13.60 0 -8 0 -4.10 11.40 0 8 0 -6.90 11.60 1 1 0 265.27 26.70 -1 -1 0 245.68 27.80 -1 1 0 262.47 25.20 -1 1 0 244.48 24.30 1 -1 0 282.17 25.60 1 -1 0 282.67 25.20 -1 -1 0 285.67 26.90 1 1 0 228.08 27.50 1 1 0 260.07 25.90 -1 -1 0 255.37 25.80 1 -2 0 1107.99 95.69 -1 -2 0 1067.59 95.79 1 -2 0 983.50 93.99 1 -2 0 1112.79 95.29 -1 -2 0 1014.50 96.39 -1 2 0 873.01 94.89 -1 -2 0 950.20 97.19 -1 2 0 1043.70 95.49 1 2 0 1066.79 96.99 1 2 0 1017.10 95.69 1 3 0 124.69 17.90 1 -3 0 94.89 14.90 -1 -3 0 127.09 17.70 -1 3 0 134.29 17.10 1 -3 0 128.89 16.20 1 3 0 112.79 16.50 1 -3 0 121.49 16.40 -1 -3 0 117.69 16.80 -1 -3 0 104.59 19.20 -1 3 0 107.39 16.40 -1 -4 0 131.79 21.50 -1 -4 0 152.58 21.40 -1 4 0 149.79 20.70 1 -4 0 151.28 19.90 1 4 0 99.69 20.80 1 -4 0 156.98 20.40 -1 -4 0 213.88 23.90 -1 4 0 151.28 24.00 1 4 0 132.49 20.20 1 -4 0 138.39 18.70 -1 -5 0 19.20 9.40 -1 -5 0 20.20 8.90 1 -5 0 10.60 8.60 1 -5 0 14.30 6.90 -1 5 0 12.60 9.40 1 5 0 19.50 8.80 1 -6 0 8.80 6.90 -1 6 0 6.50 8.60 1 -6 0 14.60 10.00 -1 -6 0 18.20 12.10 1 6 0 17.40 11.00 -1 -6 0 15.80 10.40 1 7 0 26.30 11.20 -1 -7 0 16.50 11.80 1 -7 0 4.30 8.20 1 -7 0 8.80 10.50 -1 -7 0 31.90 13.00 -1 7 0 19.70 14.30 1 7 0 26.30 15.60 -1 7 0 12.20 15.10 -1 8 0 10.90 14.40 1 8 0 7.90 13.00 1 8 0 14.90 13.10 -1 -8 0 -6.40 12.90 -1 -8 0 -26.80 10.90 -1 8 0 10.70 18.00 -2 0 0 0.20 3.00 -2 0 0 3.30 2.40 2 0 0 3.00 2.00 -2 -1 0 9730.63 868.11 2 1 0 9999.00 868.31 -2 -1 0 9228.08 869.81 -2 2 0 3.30 3.00 2 -2 0 4.50 2.70 2 -2 0 2.70 1.30 2 2 0 5.30 5.30 -2 2 0 5.10 3.10 -2 -2 0 1.40 5.60 -2 -2 0 0.20 2.80 2 -2 0 7.90 3.70 2 2 0 0.10 3.70 -2 -2 0 -0.90 3.50 2 3 0 372.26 41.90 2 -3 0 415.86 41.90 -2 -3 0 383.76 43.30 2 3 0 456.65 45.20 -2 -3 0 379.36 42.10 -2 -3 0 370.56 44.60 2 -3 0 414.46 38.50 -2 3 0 399.36 42.00 -2 3 0 404.76 42.00 2 -3 0 415.86 41.20 -2 4 0 35.20 10.00 2 -4 0 30.00 7.10 2 -4 0 44.80 10.40 -2 4 0 24.80 9.60 2 4 0 40.60 12.60 -2 -4 0 20.00 9.50 2 -4 0 31.30 10.70 2 4 0 43.20 11.40 -2 -4 0 42.00 13.20 -2 -5 0 11.50 10.00 -2 -5 0 -10.60 6.30 2 5 0 4.60 7.60 2 -5 0 7.20 5.50 -2 5 0 10.20 8.10 -2 5 0 -3.30 7.60 2 -5 0 8.70 7.60 -2 6 0 0.90 6.10 2 6 0 22.90 10.80 2 -6 0 -7.10 7.30 2 -6 0 -1.10 5.30 -2 -6 0 -5.80 8.20 -2 -6 0 18.40 12.60 2 6 0 0.10 7.80 2 -7 0 7.60 6.60 2 7 0 -0.50 9.90 2 7 0 21.30 14.80 -2 -7 0 -5.50 8.50 -2 -7 0 28.80 14.10 -2 7 0 8.60 10.10 -2 7 0 3.30 12.60 -3 0 0 0.00 3.70 3 0 0 -1.10 2.70 -3 0 0 -4.60 4.80 -3 -1 0 547.65 60.89 -3 -1 0 627.54 58.69 3 -1 0 573.64 56.49 3 1 0 647.94 59.09 -3 1 0 626.54 56.69 -3 -2 0 698.43 72.99 -3 2 0 775.82 72.79 3 -2 0 769.42 72.49 -3 2 0 834.82 71.99 3 2 0 814.22 75.69 -3 -2 0 675.73 77.19 -3 -2 0 789.52 75.49 -3 3 0 872.51 81.49 3 3 0 904.11 84.99 -3 3 0 881.61 80.99 3 -3 0 911.51 81.39 -3 -3 0 748.03 82.89 -3 -3 0 922.21 82.59 3 3 0 764.42 81.69 -3 -3 0 721.93 85.09 3 4 0 20.20 7.40 -3 -4 0 0.00 6.10 -3 4 0 4.80 7.40 -3 -4 0 -5.10 3.00 -3 -4 0 -3.10 1.60 -3 4 0 -8.80 4.50 3 4 0 4.20 5.70 3 -4 0 3.40 5.90 3 -4 0 1.20 1.90 3 5 0 10.70 9.10 -3 5 0 -4.90 6.30 3 -5 0 3.00 2.50 -3 -5 0 20.60 11.10 -3 5 0 0.10 7.90 -3 -5 0 2.50 7.80 -3 -6 0 65.09 19.60 3 6 0 98.29 23.30 3 -6 0 104.19 10.40 -3 6 0 108.59 22.60 3 6 0 58.29 16.60 -3 -6 0 70.69 21.70 -3 7 0 35.30 19.90 -3 7 0 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10.90 -3 -3 37 -17.20 13.00 3 -3 -37 9.70 9.50 3 3 37 -14.50 10.80 -3 3 -37 9.60 13.00 -3 3 37 -7.10 12.50 3 3 -37 21.50 13.50 -3 -3 -37 -3.70 14.50 3 -3 37 25.50 8.90 4 0 -37 7.50 10.00 4 0 37 4.70 5.50 -4 0 -37 -3.50 8.00 -4 0 37 5.30 12.50 4 -1 -37 -18.30 7.20 -4 1 -37 15.90 10.90 4 1 37 7.50 7.70 -4 -1 37 12.20 14.40 -4 -1 37 -10.40 10.80 -4 -1 -37 -7.60 12.70 4 1 -37 -11.30 8.20 -4 1 37 -8.40 9.70 -4 -1 -37 4.40 8.50 4 -2 -37 -2.10 8.50 -4 2 -37 7.70 11.20 4 2 37 -6.60 9.20 -4 -2 37 -8.80 11.80 -4 -2 37 37.80 21.70 -4 -2 -37 -8.60 12.60 -4 2 37 6.90 15.30 -4 -2 -37 0.10 10.40 4 2 -37 0.60 10.30 -5 0 37 -8.00 10.00 -5 0 37 25.20 13.00 -5 0 -37 11.00 10.20 -5 1 -37 -5.90 9.50 5 1 37 -9.50 5.50 5 -1 -37 -24.10 8.20 -5 -1 37 3.10 14.10 -5 -1 37 -27.30 9.90 -5 -1 -37 -4.00 9.80 -5 -1 -37 3.20 15.00 5 1 -37 -24.90 10.20 -5 1 37 -7.00 12.20 5 2 37 -16.40 8.00 -5 -2 37 2.70 17.00 -5 2 -37 -7.80 10.00 5 -2 -37 -13.50 7.80 -5 -2 -37 -10.90 12.00 -5 2 37 -6.20 11.00 -5 -2 -37 7.60 11.30 5 2 -37 1.80 12.00 -6 0 -37 3.30 9.10 -6 0 37 20.90 15.00 -6 0 37 -20.40 10.00 -6 -1 37 -4.60 11.70 6 -1 -37 -4.30 9.10 -6 -1 37 -1.50 13.40 -6 1 -37 9.30 10.80 -6 -1 -37 1.20 10.20 -6 1 37 1.10 13.90 -6 -1 -37 13.40 14.70 -6 -2 37 -11.30 16.20 -6 2 37 -15.10 12.60 -7 0 -37 10.20 11.00 -7 0 -37 14.70 15.10 -7 0 37 -20.70 12.50 -7 0 37 -11.70 11.10 -7 1 -37 -7.90 10.10 -7 -1 37 -20.70 12.70 -7 -1 -37 -5.30 13.70 -7 -1 -37 -12.50 11.20 -7 1 37 -14.70 10.10 0 0 38 121.59 21.70 0 0 -38 82.59 22.70 0 1 -38 2.40 9.90 0 1 38 -8.40 10.30 0 -1 -38 0.80 9.70 0 -1 -38 -5.20 11.30 0 -2 -38 -3.20 10.90 0 2 38 -3.60 12.70 0 2 -38 -3.70 10.40 0 -2 38 -5.10 9.60 -1 0 -38 -0.40 9.10 -1 0 38 -22.30 9.40 1 0 38 -4.30 8.50 1 0 -38 7.60 12.60 1 1 38 5.10 10.40 -1 1 -38 12.70 11.40 -1 -1 38 17.20 14.00 1 -1 -38 16.00 12.10 1 -1 -38 3.20 10.10 -1 -1 -38 0.70 10.50 1 -1 38 16.60 10.70 -1 -1 -38 -29.30 11.10 1 1 -38 7.90 12.20 -1 1 38 14.30 13.20 1 2 38 -21.40 8.70 -1 -2 38 -7.00 10.10 -1 2 -38 5.00 12.10 1 -2 -38 14.40 12.50 -1 2 38 -9.20 12.50 -1 -2 -38 8.60 11.30 1 -2 38 -11.10 6.70 1 2 -38 -10.00 7.00 -2 0 -38 63.29 19.10 -2 0 38 66.59 20.50 2 0 -38 68.89 20.90 2 0 38 72.59 15.90 2 1 38 -9.50 8.50 -2 -1 38 -14.40 10.40 2 -1 -38 -7.40 10.60 -2 1 -38 11.70 11.50 -2 1 38 -2.80 11.90 -2 -1 -38 -13.80 7.20 2 -1 38 11.90 9.50 -2 -1 -38 -8.70 11.70 2 1 -38 30.00 15.30 -2 2 -38 -2.30 10.80 2 -2 -38 16.00 11.40 2 2 38 10.00 10.60 -2 -2 38 9.10 14.10 2 -2 38 -3.70 9.80 2 2 -38 17.20 12.00 -2 -2 -38 0.10 12.60 -2 2 38 -16.10 11.30 3 0 -38 -3.50 10.60 -3 0 -38 7.20 9.20 -3 0 38 -13.20 10.20 3 0 38 -15.40 7.40 -3 -1 38 -11.50 11.60 -3 1 -38 -2.90 8.90 3 -1 -38 -16.60 9.10 3 1 38 0.80 8.60 -3 -1 -38 -22.00 9.60 3 -1 38 -15.20 6.90 -3 1 38 4.00 13.30 3 1 -38 3.20 10.00 -3 -1 -38 -6.50 8.00 -3 -2 38 8.90 14.50 3 -2 -38 5.00 10.80 3 2 38 2.10 10.90 -3 -2 38 4.60 12.50 -3 2 -38 -15.40 12.50 -3 2 38 -6.40 13.90 -3 -2 -38 21.90 16.00 3 2 -38 1.10 10.30 -3 -2 -38 -5.00 8.00 3 -2 38 11.40 9.40 -4 0 38 3.10 14.50 4 0 38 -6.10 6.50 -4 0 -38 -5.00 8.80 -4 1 -38 9.30 13.50 -4 -1 38 13.10 13.90 -4 -1 38 -5.40 10.60 4 1 38 7.20 8.90 4 -1 -38 14.60 10.20 -4 -1 -38 8.00 9.90 -4 1 38 -2.70 12.10 -4 -1 -38 0.60 12.10 4 1 -38 -6.40 9.60 4 -2 -38 17.80 9.50 -4 -2 38 -21.40 11.40 4 2 38 -6.30 8.90 -4 2 -38 -12.90 8.20 -4 -2 38 12.90 15.60 -4 -2 -38 5.50 11.40 4 2 -38 6.10 10.70 -4 2 38 7.90 13.30 -4 -2 -38 3.80 14.70 -5 0 38 -24.90 10.40 -5 0 -38 -3.30 8.90 -5 -1 38 -4.00 12.40 5 -1 -38 -11.80 9.30 -5 -1 38 4.90 13.60 -5 1 -38 18.80 13.30 -5 -1 -38 20.80 13.80 -5 -1 -38 -4.50 8.40 -5 1 38 -18.90 11.90 5 1 -38 15.30 13.10 -6 0 -38 28.60 14.00 -6 0 -38 -17.30 9.90 -6 0 38 -1.80 13.30 -6 0 38 13.20 14.10 -6 -1 38 1.90 15.40 6 -1 -38 9.90 8.80 -6 1 -38 -9.80 9.30 -6 -1 38 4.20 16.00 -6 1 38 11.40 13.30 -6 -1 -38 8.60 10.60 -6 -1 -38 -3.90 13.60 0 0 39 -11.80 9.30 0 0 -39 32.50 14.70 0 -1 -39 -6.00 9.80 0 1 -39 -6.30 8.60 0 -1 -39 5.90 12.10 0 -1 39 -9.70 10.00 0 1 39 16.50 13.10 0 -2 39 -13.70 12.00 0 2 39 -15.20 11.60 0 2 -39 7.30 12.60 0 -2 -39 -19.90 10.80 1 0 39 7.70 9.60 -1 0 39 -8.70 10.70 1 0 -39 4.20 9.10 -1 0 -39 -2.00 9.10 -1 -1 39 8.10 12.40 1 1 39 14.60 12.50 -1 1 -39 17.80 10.80 1 -1 -39 13.90 13.00 1 -1 -39 -20.40 11.90 -1 -1 -39 6.70 14.20 1 -1 39 18.40 11.90 -1 1 39 3.50 12.20 1 1 -39 8.40 15.00 -1 -1 -39 16.60 12.00 1 -2 -39 -3.30 12.30 -1 -2 39 -1.80 12.80 1 2 39 -12.70 12.80 -1 2 -39 8.60 11.60 1 2 -39 5.80 10.60 -1 2 39 -10.10 11.50 -1 -2 -39 14.20 14.30 2 0 -39 19.10 13.90 2 0 39 0.90 9.20 -2 0 39 16.80 13.90 -2 0 -39 14.20 13.40 -2 1 -39 29.70 14.20 -2 -1 39 30.90 15.80 2 1 39 21.80 11.20 2 -1 -39 -15.00 12.00 -2 -1 -39 10.70 12.50 2 -1 39 10.80 10.20 -2 -1 -39 -19.00 10.90 2 1 -39 18.10 12.00 -2 1 39 14.00 14.10 -2 2 -39 -2.90 10.40 2 -2 -39 21.20 12.90 2 2 39 -18.30 10.70 -2 -2 39 7.80 11.70 2 2 -39 5.80 10.30 -2 2 39 -11.50 9.90 2 -2 39 2.10 10.00 -2 -2 -39 25.90 18.20 3 0 -39 1.00 9.10 -3 0 -39 0.80 11.20 3 0 39 -7.50 7.50 3 -1 -39 65.49 19.40 -3 1 -39 1.00 8.60 -3 -1 39 -5.40 13.00 3 1 39 -12.90 8.30 -3 1 39 1.30 11.90 -3 -1 -39 1.00 11.10 3 -1 39 -1.30 7.30 -3 -1 -39 -7.00 14.20 3 1 -39 -9.70 10.80 -3 -2 39 -21.80 14.20 3 2 39 -0.50 12.10 3 -2 39 6.30 9.20 -3 2 39 -6.50 12.20 -4 0 -39 16.10 11.60 -4 0 39 11.70 16.80 4 0 39 8.10 11.50 4 1 39 -3.70 7.70 -4 -1 39 -1.60 14.50 4 -1 -39 -14.50 9.40 -4 1 -39 3.40 10.50 -4 -1 39 -15.80 11.00 -4 1 39 66.29 21.00 -4 -1 -39 -31.20 13.40 -4 -1 -39 -6.70 9.80 4 1 -39 -7.60 10.80 -5 0 39 -2.90 13.70 -5 0 -39 -5.40 9.50 0 0 -40 9.40 13.00 0 0 40 0.00 12.60 0 -1 -40 -0.30 13.50 0 -1 -40 -7.30 11.30 0 1 40 -14.90 12.20 0 1 -40 4.20 13.10 0 -1 40 -23.60 11.30 1 0 40 -17.70 10.30 -1 0 -40 -3.00 10.30 -1 0 40 -6.40 9.30 1 0 -40 0.40 12.30 1 1 40 -17.30 11.40 1 -1 -40 4.10 11.40 -1 -1 40 0.90 14.20 -1 1 -40 -3.10 10.20 1 -1 -40 3.60 11.60 -1 -1 -40 22.50 15.20 -1 1 40 -20.90 10.50 -1 -1 -40 -2.00 10.90 1 -1 40 2.40 10.50 1 1 -40 -2.70 10.30 -2 0 40 17.40 14.70 -2 0 -40 28.20 15.80 2 0 40 17.50 11.30 2 0 -40 84.09 22.80 2 -1 -40 -33.40 10.80 -2 1 -40 10.80 12.40 -2 -1 40 -2.40 11.30 2 1 40 -5.50 10.20 2 1 -40 5.60 10.10 -2 -1 -40 -1.20 12.90 -2 -1 -40 16.40 16.60 2 -1 40 -9.90 8.80 -2 1 40 -8.40 13.10 3 0 -40 -13.90 9.10 -3 0 40 1.50 14.90 -3 0 -40 -12.20 9.30 3 0 40 3.00 8.70 -3 -1 40 -14.60 11.20 3 1 40 -4.80 9.90 -3 1 40 -12.10 11.30 3 -1 40 -9.10 8.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 38302 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.22305(11) -0.1095(3) 0.57146(6) 0.0643(6) Uani 1 1 d . . . . . O1 O 0.2421(3) 0.2291(8) 0.51958(15) 0.0660(14) Uani 1 1 d . . . . . N1 N 0.3805(5) 0.0133(8) 0.5315(3) 0.050(2) Uani 1 1 d . . . . . H1 H 0.421649 0.084732 0.514676 0.060 Uiso 1 1 calc R U . . . C1 C 0.2840(4) 0.0718(13) 0.5367(2) 0.0538(16) Uani 1 1 d . . . . . C2 C 0.4102(4) -0.1669(11) 0.5543(2) 0.0471(15) Uani 1 1 d . . . . . C3 C 0.3351(4) -0.2546(10) 0.5789(2) 0.0498(15) Uani 1 1 d . . . . . C4 C 0.3526(5) -0.4312(13) 0.6053(3) 0.0587(18) Uani 1 1 d . . . . . H4 H 0.299969 -0.489210 0.622183 0.070 Uiso 1 1 calc R U . . . C5 C 0.4471(7) -0.5210(12) 0.6066(4) 0.060(3) Uani 1 1 d . . . . . C6 C 0.5224(5) -0.4313(12) 0.5803(3) 0.0579(19) Uani 1 1 d . . . . . H6 H 0.587266 -0.495248 0.580398 0.069 Uiso 1 1 calc R U . . . C7 C 0.5056(4) -0.2576(11) 0.5548(2) 0.0551(17) Uani 1 1 d . . . . . H7 H 0.557890 -0.199277 0.537742 0.066 Uiso 1 1 calc R U . . . C8 C 0.4765(6) -0.7132(12) 0.6343(2) 0.0639(18) Uani 1 1 d . . . . . H8 H 0.505006 -0.826827 0.615131 0.077 Uiso 1 1 calc R U . . . C9 C 0.5591(5) -0.6519(12) 0.6664(3) 0.0582(17) Uani 1 1 d . . . . . C10 C 0.5607(7) -0.4540(16) 0.6866(4) 0.075(3) Uani 1 1 d . . . . . H10 H 0.510390 -0.349449 0.680404 0.090 Uiso 1 1 calc R U . . . C11 C 0.6350(7) -0.4058(14) 0.7160(3) 0.083(2) Uani 1 1 d . . . . . H11 H 0.635909 -0.267195 0.729201 0.099 Uiso 1 1 calc R U . . . C12 C 0.7077(7) -0.5562(18) 0.7263(3) 0.082(3) Uani 1 1 d . . . . . H12 H 0.758444 -0.523153 0.746496 0.098 Uiso 1 1 calc R U . . . C13 C 0.7047(6) -0.7579(16) 0.7064(3) 0.077(2) Uani 1 1 d . . . . . H13 H 0.753473 -0.864816 0.713156 0.092 Uiso 1 1 calc R U . . . C14 C 0.6314(5) -0.8025(13) 0.6770(2) 0.0641(19) Uani 1 1 d . . . . . H14 H 0.630433 -0.940661 0.663627 0.077 Uiso 1 1 calc R U . . . C15 C 0.3886(6) -0.8155(14) 0.6579(3) 0.086(3) Uani 1 1 d . . . . . H15A H 0.362879 -0.712966 0.679040 0.128 Uiso 1 1 calc R U . . . H15B H 0.411153 -0.948046 0.672176 0.128 Uiso 1 1 calc R U . . . H15C H 0.335330 -0.851180 0.637617 0.128 Uiso 1 1 calc R U . . . S2 S 0.52202(11) 0.6094(3) 0.42891(6) 0.0652(6) Uani 1 1 d . . . . . O2 O 0.5031(3) 0.2737(9) 0.48121(16) 0.0687(15) Uani 1 1 d . . . . . N2 N 0.3649(5) 0.4889(8) 0.4693(3) 0.0487(19) Uani 1 1 d . . . . . H2 H 0.323806 0.419583 0.486484 0.058 Uiso 1 1 calc R U . . . C16 C 0.4611(5) 0.4283(13) 0.4643(2) 0.0549(16) Uani 1 1 d . . . . . C17 C 0.3341(4) 0.6693(11) 0.44558(19) 0.0446(14) Uani 1 1 d . . . . . C18 C 0.4107(4) 0.7547(10) 0.4213(2) 0.0507(16) Uani 1 1 d . . . . . C19 C 0.3927(5) 0.9308(14) 0.3952(3) 0.0594(18) Uani 1 1 d . . . . . H19 H 0.445012 0.988851 0.378086 0.071 Uiso 1 1 calc R U . . . C20 C 0.2966(7) 1.0227(11) 0.3941(4) 0.055(2) Uani 1 1 d . . . . . C21 C 0.2221(5) 0.9364(13) 0.4194(3) 0.062(2) Uani 1 1 d . . . . . H21 H 0.157264 1.000408 0.418993 0.074 Uiso 1 1 calc R U . . . C22 C 0.2392(4) 0.7604(11) 0.4451(2) 0.0507(16) Uani 1 1 d . . . . . H22 H 0.186934 0.702342 0.462239 0.061 Uiso 1 1 calc R U . . . C23 C 0.2701(6) 1.2167(12) 0.3660(3) 0.070(2) Uani 1 1 d . . . . . H23 H 0.243458 1.330918 0.385579 0.083 Uiso 1 1 calc R U . . . C24 C 0.1873(5) 1.1683(11) 0.3351(2) 0.0581(17) Uani 1 1 d . . . . . C25 C 0.1759(7) 0.9749(14) 0.3147(4) 0.073(3) Uani 1 1 d . . . . . H25 H 0.221574 0.860956 0.320864 0.087 Uiso 1 1 calc R U . . . C26 C 0.1010(7) 0.9375(17) 0.2854(3) 0.078(2) Uani 1 1 d . . . . . H26 H 0.096396 0.800567 0.271734 0.094 Uiso 1 1 calc R U . . . C27 C 0.0337(6) 1.0962(15) 0.2761(3) 0.078(2) Uani 1 1 d . . . . . H27 H -0.018966 1.070276 0.256447 0.094 Uiso 1 1 calc R U . . . C28 C 0.0430(6) 1.2932(17) 0.2955(3) 0.078(2) Uani 1 1 d . . . . . H28 H -0.003369 1.405689 0.289100 0.094 Uiso 1 1 calc R U . . . C29 C 0.1196(5) 1.3304(12) 0.3244(2) 0.0642(19) Uani 1 1 d . . . . . H29 H 0.125830 1.469516 0.337079 0.077 Uiso 1 1 calc R U . . . C30 C 0.3586(6) 1.3171(15) 0.3435(3) 0.088(3) Uani 1 1 d . . . . . H30A H 0.410571 1.353981 0.364320 0.131 Uiso 1 1 calc R U . . . H30B H 0.336958 1.448920 0.328715 0.131 Uiso 1 1 calc R U . . . H30C H 0.385760 1.213638 0.322861 0.131 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0338(7) 0.0844(13) 0.0748(13) 0.0290(11) 0.0085(7) 0.0002(8) O1 0.041(2) 0.085(3) 0.072(4) 0.030(3) 0.007(2) 0.003(2) N1 0.034(3) 0.066(4) 0.050(6) 0.011(3) 0.007(3) -0.004(2) C1 0.033(3) 0.080(4) 0.048(4) 0.010(4) 0.005(3) -0.002(4) C2 0.036(3) 0.062(4) 0.044(3) -0.001(3) 0.001(3) -0.003(3) C3 0.039(3) 0.055(4) 0.055(4) 0.007(3) 0.001(3) -0.007(3) C4 0.045(4) 0.069(4) 0.061(5) 0.010(4) 0.000(3) -0.013(4) C5 0.048(4) 0.060(5) 0.073(8) 0.005(4) -0.012(5) -0.004(3) C6 0.042(4) 0.062(4) 0.070(6) 0.002(5) 0.003(3) 0.008(3) C7 0.042(3) 0.063(4) 0.060(4) 0.000(4) 0.010(3) -0.003(3) C8 0.061(4) 0.060(4) 0.070(5) 0.004(4) -0.005(4) -0.001(4) C9 0.053(4) 0.056(4) 0.065(5) 0.015(4) 0.005(3) 0.001(3) C10 0.075(5) 0.070(5) 0.081(8) 0.006(5) -0.006(5) 0.013(5) C11 0.111(7) 0.064(5) 0.073(6) -0.008(5) 0.003(5) -0.001(5) C12 0.075(5) 0.107(7) 0.063(6) 0.021(6) -0.004(5) -0.003(5) C13 0.063(4) 0.095(6) 0.073(5) 0.004(5) -0.005(4) 0.015(4) C14 0.060(4) 0.075(5) 0.058(5) 0.009(4) 0.009(3) 0.017(4) C15 0.078(5) 0.079(5) 0.100(7) 0.025(5) -0.015(5) -0.018(5) S2 0.0349(7) 0.0868(14) 0.0738(13) 0.0307(12) 0.0074(7) 0.0001(8) O2 0.039(2) 0.087(4) 0.080(4) 0.035(3) 0.010(2) 0.007(2) N2 0.035(3) 0.065(4) 0.046(5) 0.013(3) 0.003(3) -0.003(2) C16 0.038(3) 0.076(4) 0.051(4) 0.018(4) 0.001(3) 0.000(4) C17 0.035(3) 0.055(4) 0.044(3) 0.000(3) -0.002(3) -0.006(3) C18 0.035(3) 0.061(4) 0.055(4) 0.009(3) 0.001(3) -0.004(3) C19 0.044(4) 0.071(4) 0.064(5) 0.022(5) 0.000(3) -0.004(4) C20 0.050(4) 0.059(5) 0.056(6) 0.004(4) -0.002(4) -0.002(3) C21 0.038(4) 0.065(4) 0.081(6) 0.001(5) 0.000(3) 0.001(3) C22 0.035(3) 0.062(4) 0.056(4) 0.004(3) 0.007(3) -0.001(3) C23 0.065(4) 0.059(4) 0.085(5) 0.011(4) -0.005(4) 0.002(4) C24 0.052(4) 0.056(4) 0.066(5) 0.007(4) 0.001(3) 0.005(3) C25 0.065(5) 0.067(5) 0.086(8) -0.001(5) -0.014(5) 0.012(4) C26 0.081(5) 0.082(5) 0.072(6) 0.000(5) -0.005(5) 0.007(5) C27 0.071(5) 0.097(7) 0.066(6) -0.002(6) -0.009(4) 0.000(5) C28 0.064(4) 0.100(6) 0.071(6) 0.019(5) -0.001(4) 0.028(5) C29 0.065(4) 0.063(4) 0.065(5) 0.007(4) 0.008(4) 0.015(4) C30 0.076(5) 0.084(6) 0.103(7) 0.033(5) -0.014(5) -0.022(5) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 S1 C1 90.8(3) . . ? C1 N1 H1 122.4 . . ? C1 N1 C2 115.2(6) . . ? C2 N1 H1 122.4 . . ? O1 C1 S1 123.9(5) . . ? O1 C1 N1 125.9(6) . . ? N1 C1 S1 110.3(6) . . ? N1 C2 C7 126.3(6) . . ? C3 C2 N1 113.5(6) . . ? C3 C2 C7 120.1(6) . . ? C2 C3 S1 110.1(5) . . ? C2 C3 C4 121.5(6) . . ? C4 C3 S1 128.4(5) . . ? C3 C4 H4 120.4 . . ? C5 C4 C3 119.1(7) . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 118.3(8) . . ? C4 C5 C8 124.4(9) . . ? C6 C5 C8 117.3(7) . . ? C5 C6 H6 118.7 . . ? C7 C6 C5 122.6(6) . . ? C7 C6 H6 118.7 . . ? C2 C7 H7 120.8 . . ? C6 C7 C2 118.4(6) . . ? C6 C7 H7 120.8 . . ? C5 C8 H8 107.2 . . ? C5 C8 C9 111.6(6) . . ? C9 C8 H8 107.2 . . ? C15 C8 C5 113.8(7) . . ? C15 C8 H8 107.2 . . ? C15 C8 C9 109.4(6) . . ? C10 C9 C8 122.1(7) . . ? C10 C9 C14 118.3(8) . . ? C14 C9 C8 119.5(7) . . ? C9 C10 H10 119.7 . . ? C9 C10 C11 120.6(9) . . ? C11 C10 H10 119.7 . . ? C10 C11 H11 119.5 . . ? C12 C11 C10 120.9(9) . . ? C12 C11 H11 119.5 . . ? C11 C12 H12 120.9 . . ? C11 C12 C13 118.3(9) . . ? C13 C12 H12 120.9 . . ? C12 C13 H13 119.9 . . ? C14 C13 C12 120.2(8) . . ? C14 C13 H13 119.9 . . ? C9 C14 H14 119.2 . . ? C13 C14 C9 121.7(8) . . ? C13 C14 H14 119.2 . . ? C8 C15 H15A 109.5 . . ? C8 C15 H15B 109.5 . . ? C8 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 S2 C16 91.2(3) . . ? C16 N2 H2 122.0 . . ? C16 N2 C17 115.9(6) . . ? C17 N2 H2 122.0 . . ? O2 C16 S2 123.5(5) . . ? O2 C16 N2 126.9(6) . . ? N2 C16 S2 109.6(5) . . ? C18 C17 N2 112.5(5) . . ? C18 C17 C22 121.0(6) . . ? C22 C17 N2 126.5(6) . . ? C17 C18 S2 110.8(5) . . ? C17 C18 C19 120.1(6) . . ? C19 C18 S2 129.1(5) . . ? C18 C19 H19 120.3 . . ? C18 C19 C20 119.4(7) . . ? C20 C19 H19 120.3 . . ? C19 C20 C23 122.8(8) . . ? C21 C20 C19 119.2(7) . . ? C21 C20 C23 118.0(7) . . ? C20 C21 H21 119.1 . . ? C22 C21 C20 121.8(6) . . ? C22 C21 H21 119.1 . . ? C17 C22 H22 120.7 . . ? C21 C22 C17 118.6(6) . . ? C21 C22 H22 120.7 . . ? C20 C23 H23 106.1 . . ? C24 C23 C20 112.9(6) . . ? C24 C23 H23 106.1 . . ? C24 C23 C30 110.6(7) . . ? C30 C23 C20 114.3(7) . . ? C30 C23 H23 106.1 . . ? C25 C24 C23 124.2(7) . . ? C25 C24 C29 116.2(8) . . ? C29 C24 C23 119.5(7) . . ? C24 C25 H25 118.5 . . ? C24 C25 C26 122.9(9) . . ? C26 C25 H25 118.5 . . ? C25 C26 H26 119.9 . . ? C27 C26 C25 120.1(10) . . ? C27 C26 H26 119.9 . . ? C26 C27 H27 120.5 . . ? C26 C27 C28 119.0(9) . . ? C28 C27 H27 120.5 . . ? C27 C28 H28 119.8 . . ? C27 C28 C29 120.4(7) . . ? C29 C28 H28 119.8 . . ? C24 C29 H29 119.3 . . ? C28 C29 C24 121.3(8) . . ? C28 C29 H29 119.3 . . ? C23 C30 H30A 109.5 . . ? C23 C30 H30B 109.5 . . ? C23 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.763(7) . ? S1 C3 1.756(6) . ? O1 C1 1.243(8) . ? N1 H1 0.8800 . ? N1 C1 1.345(9) . ? N1 C2 1.382(9) . ? C2 C3 1.377(8) . ? C2 C7 1.389(8) . ? C3 C4 1.389(10) . ? C4 H4 0.9500 . ? C4 C5 1.377(10) . ? C5 C6 1.414(12) . ? C5 C8 1.523(11) . ? C6 H6 0.9500 . ? C6 C7 1.356(10) . ? C7 H7 0.9500 . ? C8 H8 1.0000 . ? C8 C9 1.540(10) . ? C8 C15 1.523(10) . ? C9 C10 1.377(12) . ? C9 C14 1.379(9) . ? C10 H10 0.9500 . ? C10 C11 1.388(14) . ? C11 H11 0.9500 . ? C11 C12 1.380(13) . ? C12 H12 0.9500 . ? C12 C13 1.393(14) . ? C13 H13 0.9500 . ? C13 C14 1.374(11) . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? S2 C16 1.775(7) . ? S2 C18 1.749(6) . ? O2 C16 1.226(8) . ? N2 H2 0.8800 . ? N2 C16 1.344(9) . ? N2 C17 1.401(9) . ? C17 C18 1.381(8) . ? C17 C22 1.385(8) . ? C18 C19 1.382(10) . ? C19 H19 0.9500 . ? C19 C20 1.401(10) . ? C20 C21 1.380(12) . ? C20 C23 1.528(11) . ? C21 H21 0.9500 . ? C21 C22 1.373(11) . ? C22 H22 0.9500 . ? C23 H23 1.0000 . ? C23 C24 1.501(10) . ? C23 C30 1.509(11) . ? C24 C25 1.364(11) . ? C24 C29 1.389(9) . ? C25 H25 0.9500 . ? C25 C26 1.377(14) . ? C26 H26 0.9500 . ? C26 C27 1.359(12) . ? C27 H27 0.9500 . ? C27 C28 1.365(13) . ? C28 H28 0.9500 . ? C28 C29 1.386(12) . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C3 C4 C5 -179.5(7) . . . . ? N1 C2 C3 S1 1.9(7) . . . . ? N1 C2 C3 C4 -177.4(7) . . . . ? N1 C2 C7 C6 177.9(7) . . . . ? C1 S1 C3 C2 -2.1(5) . . . . ? C1 S1 C3 C4 177.1(7) . . . . ? C1 N1 C2 C3 -0.4(10) . . . . ? C1 N1 C2 C7 -179.1(7) . . . . ? C2 N1 C1 S1 -1.3(9) . . . . ? C2 N1 C1 O1 179.3(8) . . . . ? C2 C3 C4 C5 -0.4(11) . . . . ? C3 S1 C1 O1 -178.6(7) . . . . ? C3 S1 C1 N1 1.9(6) . . . . ? C3 C2 C7 C6 -0.7(10) . . . . ? C3 C4 C5 C6 -1.1(13) . . . . ? C3 C4 C5 C8 179.5(8) . . . . ? C4 C5 C6 C7 1.9(13) . . . . ? C4 C5 C8 C9 -118.6(9) . . . . ? C4 C5 C8 C15 5.8(13) . . . . ? C5 C6 C7 C2 -0.9(12) . . . . ? C5 C8 C9 C10 38.5(11) . . . . ? C5 C8 C9 C14 -144.8(8) . . . . ? C6 C5 C8 C9 62.1(11) . . . . ? C6 C5 C8 C15 -173.5(8) . . . . ? C7 C2 C3 S1 -179.4(5) . . . . ? C7 C2 C3 C4 1.4(10) . . . . ? C8 C5 C6 C7 -178.8(8) . . . . ? C8 C9 C10 C11 178.6(8) . . . . ? C8 C9 C14 C13 -177.9(7) . . . . ? C9 C10 C11 C12 -1.4(15) . . . . ? C10 C9 C14 C13 -1.1(12) . . . . ? C10 C11 C12 C13 0.2(14) . . . . ? C11 C12 C13 C14 0.6(14) . . . . ? C12 C13 C14 C9 -0.2(13) . . . . ? C14 C9 C10 C11 1.9(14) . . . . ? C15 C8 C9 C10 -88.3(10) . . . . ? C15 C8 C9 C14 88.4(8) . . . . ? S2 C18 C19 C20 -179.9(7) . . . . ? N2 C17 C18 S2 -0.7(7) . . . . ? N2 C17 C18 C19 178.6(7) . . . . ? N2 C17 C22 C21 -179.3(7) . . . . ? C16 S2 C18 C17 1.5(5) . . . . ? C16 S2 C18 C19 -177.8(7) . . . . ? C16 N2 C17 C18 -0.8(10) . . . . ? C16 N2 C17 C22 179.4(7) . . . . ? C17 N2 C16 S2 1.9(9) . . . . ? C17 N2 C16 O2 -178.4(8) . . . . ? C17 C18 C19 C20 0.8(12) . . . . ? C18 S2 C16 O2 178.4(8) . . . . ? C18 S2 C16 N2 -1.9(6) . . . . ? C18 C17 C22 C21 1.0(10) . . . . ? C18 C19 C20 C21 0.4(13) . . . . ? C18 C19 C20 C23 -179.7(8) . . . . ? C19 C20 C21 C22 -1.0(13) . . . . ? C19 C20 C23 C24 120.8(9) . . . . ? C19 C20 C23 C30 -6.8(13) . . . . ? C20 C21 C22 C17 0.3(12) . . . . ? C20 C23 C24 C25 -37.5(13) . . . . ? C20 C23 C24 C29 145.8(7) . . . . ? C21 C20 C23 C24 -59.4(11) . . . . ? C21 C20 C23 C30 173.0(8) . . . . ? C22 C17 C18 S2 179.1(5) . . . . ? C22 C17 C18 C19 -1.6(10) . . . . ? C23 C20 C21 C22 179.1(8) . . . . ? C23 C24 C25 C26 -177.8(9) . . . . ? C23 C24 C29 C28 179.0(7) . . . . ? C24 C25 C26 C27 -0.7(16) . . . . ? C25 C24 C29 C28 2.1(13) . . . . ? C25 C26 C27 C28 1.4(14) . . . . ? C26 C27 C28 C29 -0.4(14) . . . . ? C27 C28 C29 C24 -1.4(13) . . . . ? C29 C24 C25 C26 -1.0(15) . . . . ? C30 C23 C24 C25 92.0(10) . . . . ? C30 C23 C24 C29 -84.7(9) . . . . ?