#------------------------------------------------------------------------------ #$Date: 2024-07-18 01:12:23 +0300 (Thu, 18 Jul 2024) $ #$Revision: 293448 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572141.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_1572141 loop_ _publ_author_name 'Gong, Jian-Ye' 'Wang, Xiaopeng' 'Zhang, Weijing' 'Wu, Yifan' 'Li, Kai' 'Sha, Renmanduhu' 'Liu, Lingxiu' 'Li, Chunbin' 'Feng, Lina' 'Jiang, Guoyu' 'Wang, Jianguo' 'Tang, Ben Zhong' _publ_section_title ; Sulfur oxidation states manipulate excited state electronic configurations for constructing highly efficient organic type I photosensitizer ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03039G _journal_year 2024 _chemical_formula_moiety 'C48 H34 N2 O2 S' _chemical_formula_sum 'C48 H34 N2 O2 S' _chemical_formula_weight 702.83 _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_date 2020-07-11 _audit_creation_method ; Olex2 1.3 (compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132) ; _audit_update_record ; 2024-01-13 deposited with the CCDC. 2024-07-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.842(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.6095(11) _cell_length_b 17.9909(12) _cell_length_c 14.0147(10) _cell_measurement_reflns_used 3388 _cell_measurement_temperature 100.0(2) _cell_measurement_theta_max 28.1830 _cell_measurement_theta_min 2.5710 _cell_volume 3560.7(5) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -10.00 22.00 1.00 6.00 -- -11.59 -99.00 90.00 32 2 \w -40.00 52.00 1.00 6.00 -- -11.59 57.00-150.00 92 3 \w -64.00 18.00 1.00 6.00 -- -11.59 -77.00 -60.00 82 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0168835000 _diffrn_orient_matrix_UB_12 0.0153030000 _diffrn_orient_matrix_UB_13 -0.0389297000 _diffrn_orient_matrix_UB_21 0.0095308500 _diffrn_orient_matrix_UB_22 0.0340654500 _diffrn_orient_matrix_UB_23 0.0260768000 _diffrn_orient_matrix_UB_31 0.0463550500 _diffrn_orient_matrix_UB_32 -0.0126185500 _diffrn_orient_matrix_UB_33 0.0233195000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_unetI/netI 0.0617 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 7994 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.124 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.56893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.311 _exptl_crystal_description block _exptl_crystal_F_000 1472 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.247 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 240 _refine_ls_number_reflns 3145 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0508 _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^)+(0.0609P)^2^+1.1840P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1224 _refine_ls_wR_factor_ref 0.1338 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2524 _reflns_number_total 3145 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03039g2.cif _cod_data_source_block tpa_2 _cod_database_code 1572141 _shelx_shelxl_version_number 2018/3 _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. ; _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C20(H20), C21(H21), C24(H24) ; _shelx_res_file ; TITL tpa_2_a.res in C2/c tpa_2.res created by SHELXL-2018/3 at 09:26:07 on 11-Jul-2020 REM Old TITL tpa_2 in C2/c REM SHELXT solution in C2/c: R1 0.150, Rweak 0.179, Alpha 0.027 REM 0.734 for 122 systematic absences, Orientation as input REM Formula found by SHELXT: C48 N2 O2 Cl CELL 0.71073 14.6095 17.9909 14.0147 90 104.842 90 ZERR 4 0.0011 0.0012 0.001 0 0.007 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O S UNIT 192 136 8 8 4 L.S. 10 PLAN 5 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta OMIT -3 50 REM REM REM WGHT 0.060900 1.184000 FVAR 0.25573 S1 5 0.500000 1.013004 0.750000 10.50000 0.03444 0.01787 = 0.01931 0.00000 0.00748 0.00000 O1 4 0.578108 1.054892 0.733558 11.00000 0.05078 0.02653 = 0.02764 0.00020 0.01071 -0.01393 N1 3 0.318673 0.588302 0.249676 11.00000 0.03745 0.02251 = 0.02054 -0.00326 -0.00262 0.00082 C1 1 0.273094 0.607295 0.149968 11.00000 0.02932 0.02387 = 0.01834 -0.00357 0.00247 -0.00366 C2 1 0.202905 0.661878 0.129882 11.00000 0.03120 0.03458 = 0.02401 -0.00473 0.00440 0.00134 AFIX 43 H2 2 0.184872 0.685041 0.181539 11.00000 -1.20000 AFIX 0 C3 1 0.159975 0.681686 0.033190 11.00000 0.03139 0.03254 = 0.03284 0.00289 -0.00039 0.00218 AFIX 43 H3 2 0.113812 0.718551 0.020542 11.00000 -1.20000 AFIX 0 C4 1 0.184910 0.647372 -0.044466 11.00000 0.04716 0.03382 = 0.01916 0.00278 0.00078 -0.01162 AFIX 43 H4 2 0.155975 0.660995 -0.109180 11.00000 -1.20000 AFIX 0 C5 1 0.253164 0.592687 -0.025092 11.00000 0.04680 0.03652 = 0.02368 -0.00699 0.01445 -0.01118 AFIX 43 H5 2 0.269040 0.568660 -0.077388 11.00000 -1.20000 AFIX 0 C6 1 0.298473 0.572871 0.070580 11.00000 0.03023 0.02754 = 0.02964 -0.00225 0.00811 -0.00121 AFIX 43 H6 2 0.345662 0.536820 0.082357 11.00000 -1.20000 AFIX 0 C7 1 0.350372 0.514771 0.276058 11.00000 0.02841 0.02539 = 0.01975 -0.00316 0.00647 0.00006 C8 1 0.434272 0.501416 0.347742 11.00000 0.02831 0.03138 = 0.03361 -0.00612 0.00350 0.00076 AFIX 43 H8 2 0.471064 0.541233 0.377975 11.00000 -1.20000 AFIX 0 C9 1 0.463252 0.429987 0.374259 11.00000 0.03372 0.04254 = 0.04196 0.00373 0.00658 0.01074 AFIX 43 H9 2 0.519107 0.421749 0.422698 11.00000 -1.20000 AFIX 0 C10 1 0.409272 0.369919 0.328850 11.00000 0.06217 0.02800 = 0.05314 0.00718 0.03049 0.01587 AFIX 43 H10 2 0.428691 0.321660 0.347551 11.00000 -1.20000 AFIX 0 C11 1 0.327584 0.381850 0.256649 11.00000 0.04985 0.03229 = 0.03550 -0.00510 0.01861 -0.00813 AFIX 43 H11 2 0.292572 0.341727 0.224809 11.00000 -1.20000 AFIX 0 C12 1 0.297138 0.453959 0.231079 11.00000 0.03499 0.02958 = 0.02570 -0.00376 0.00668 -0.00404 AFIX 43 H12 2 0.240633 0.461830 0.183440 11.00000 -1.20000 AFIX 0 C13 1 0.324160 0.639569 0.413242 11.00000 0.03242 0.02225 = 0.02359 0.00159 0.00215 -0.00277 AFIX 43 H13 2 0.295806 0.596586 0.428964 11.00000 -1.20000 AFIX 0 C14 1 0.347937 0.696273 0.481788 11.00000 0.03349 0.02685 = 0.01539 -0.00174 0.00388 0.00089 AFIX 43 H14 2 0.336292 0.690506 0.543570 11.00000 -1.20000 AFIX 0 C15 1 0.389032 0.761894 0.459923 11.00000 0.02694 0.02247 = 0.01904 0.00154 0.00145 0.00347 C16 1 0.406867 0.768326 0.366917 11.00000 0.03572 0.02449 = 0.01952 0.00097 0.00274 -0.00368 AFIX 43 H16 2 0.434089 0.811666 0.350611 11.00000 -1.20000 AFIX 0 C17 1 0.384654 0.711222 0.298723 11.00000 0.03632 0.03027 = 0.01768 -0.00051 0.00519 -0.00129 AFIX 43 H17 2 0.398097 0.716242 0.237672 11.00000 -1.20000 AFIX 0 C18 1 0.342414 0.646416 0.320722 11.00000 0.02930 0.02306 = 0.01920 -0.00404 -0.00117 0.00148 C19 1 0.412927 0.824547 0.531209 11.00000 0.02456 0.02358 = 0.01902 -0.00129 0.00433 0.00154 C20 1 0.401347 0.897794 0.495906 11.00000 0.03140 0.02516 = 0.01697 0.00317 0.00210 0.00364 AFIX 43 H20 2 0.377216 0.905669 0.428552 11.00000 -1.20000 AFIX 0 C21 1 0.424454 0.958704 0.557463 11.00000 0.03385 0.01928 = 0.02028 0.00340 0.00695 0.00396 AFIX 43 H21 2 0.415136 1.006897 0.532888 11.00000 -1.20000 AFIX 0 C22 1 0.462128 0.945220 0.657440 11.00000 0.02781 0.01935 = 0.02083 -0.00080 0.00831 0.00139 C23 1 0.476716 0.873206 0.695961 11.00000 0.02280 0.01968 = 0.01785 0.00001 0.00585 0.00086 C24 1 0.449453 0.812888 0.633121 11.00000 0.02693 0.01665 = 0.02047 0.00194 0.00583 0.00199 AFIX 43 H24 2 0.455362 0.764843 0.658453 11.00000 -1.20000 AFIX 0 HKLF 4 REM tpa_2_a.res in C2/c REM wR2 = 0.1338, GooF = S = 1.062, Restrained GooF = 1.062 for all data REM R1 = 0.0508 for 2524 Fo > 4sig(Fo) and 0.0642 for all 3145 data REM 240 parameters refined using 0 restraints END WGHT 0.0609 1.1443 REM Highest difference peak 0.247, deepest hole -0.383, 1-sigma level 0.056 Q1 1 0.5000 1.0814 0.7500 10.50000 0.05 0.25 Q2 1 0.6461 1.0259 0.7568 11.00000 0.05 0.23 Q3 1 0.6555 1.0399 0.7456 11.00000 0.05 0.22 Q4 1 0.3541 0.3337 0.2588 11.00000 0.05 0.20 Q5 1 0.5129 1.0490 0.6795 11.00000 0.05 0.20 ; _shelx_res_checksum 45126 _shelx_hkl_file ; 0 0 -2 608.53 20.36 0 0 -2 719.83 18.93 0 0 -3 -0.21 0.28 0 0 -3 0.73 0.45 0 0 -4 1667.75 46.00 0 0 4 1775.63 49.90 0 0 -4 1699.25 49.80 0 0 5 0.38 0.61 0 0 -5 0.98 1.01 0 0 -5 0.99 0.59 0 0 -6 0.84 0.99 0 0 -6 2.01 0.91 0 0 6 0.03 0.66 0 0 -7 1.04 1.34 0 0 -7 3.97 1.24 0 0 7 0.49 0.73 0 0 -8 550.61 25.62 0 0 8 483.15 24.96 0 0 -9 0.13 1.17 0 0 9 -0.51 1.08 0 0 -9 0.13 0.48 0 0 -10 1008.92 39.83 0 0 10 1143.88 43.30 0 0 -11 2.23 1.58 0 0 11 0.10 1.68 0 0 -11 1.76 1.09 0 0 -12 7.19 1.87 0 0 12 3.11 2.14 0 0 13 0.66 1.81 0 0 -13 3.17 1.43 0 0 -13 3.74 2.35 0 0 -14 40.10 7.22 0 0 14 33.75 7.75 0 0 15 6.63 4.22 0 0 -15 2.63 2.42 0 0 -16 27.93 6.66 0 0 16 9.55 5.55 0 -2 0 913.21 25.12 0 2 -1 735.70 21.54 0 -2 -1 756.91 21.92 0 2 2 3241.49 81.85 0 -2 -2 3179.80 83.53 0 2 -2 3107.44 83.38 0 2 -3 786.23 24.32 0 2 3 802.00 23.35 0 -2 -3 759.98 23.95 0 -2 -3 738.84 25.09 0 -2 -3 751.47 22.69 0 2 -4 415.98 17.15 0 -2 -4 536.35 17.53 0 -2 -4 441.08 15.97 0 -2 -4 497.94 18.93 0 2 5 262.75 13.53 0 -2 -5 224.88 10.51 0 2 -5 233.62 12.12 0 -2 -5 260.13 11.33 0 2 -5 215.43 7.23 0 -2 -5 271.62 13.44 0 -2 -6 1227.48 38.29 0 -2 -6 1140.59 41.49 0 -2 6 1217.77 42.21 0 -2 -6 1185.01 38.71 0 2 6 1237.83 42.82 0 2 -6 1225.82 41.35 0 -2 -7 151.71 11.64 0 2 -7 160.95 11.50 0 -2 -7 173.58 10.46 0 2 7 194.03 13.20 0 -2 -7 176.82 9.70 0 2 -7 197.67 7.07 0 -2 7 135.56 11.19 0 2 -8 148.11 11.60 0 2 -8 144.75 6.42 0 -2 -8 159.19 12.54 0 -2 -8 166.26 9.52 0 -2 8 140.19 11.65 0 -2 -8 149.06 10.29 0 2 8 170.18 13.05 0 2 9 69.88 8.86 0 2 -9 70.78 4.32 0 2 -9 65.30 7.94 0 -2 9 60.69 7.95 0 -2 -9 69.07 8.46 0 -2 -9 77.79 7.62 0 -2 -9 70.74 6.05 0 -2 10 212.28 16.39 0 -2 -10 233.64 17.05 0 2 -10 240.39 9.38 0 -2 -10 206.83 11.54 0 -2 -11 0.29 0.53 0 2 -11 1.18 0.80 0 2 12 472.05 28.55 0 -2 -12 461.65 23.86 0 -2 12 420.43 26.85 0 -2 -12 403.02 18.50 0 2 -12 460.17 16.31 0 -2 -13 7.50 2.06 0 -2 13 4.40 2.30 0 2 -13 6.19 1.53 0 -2 -13 8.62 3.24 0 2 -14 -0.92 1.25 0 -2 14 -0.64 1.56 0 -2 -14 2.31 1.60 0 -2 15 15.72 6.10 0 2 -15 31.58 7.60 0 -2 -15 15.29 4.68 0 -2 16 9.43 4.18 0 2 -16 5.57 2.83 0 -2 -16 12.48 4.21 0 -2 17 39.63 9.84 0 2 -17 57.70 10.67 0 -4 0 928.55 27.70 0 -4 -1 885.37 27.40 0 -4 1 946.06 27.58 0 -4 1 852.11 25.55 0 4 -2 247.46 11.09 0 -4 2 260.54 8.60 0 -4 -2 244.55 11.27 0 -4 -3 138.73 8.33 0 4 -3 161.04 8.96 0 -4 -4 35.75 4.09 0 4 4 33.79 3.42 0 4 -4 33.63 4.06 0 -4 -5 129.28 8.57 0 -4 -5 130.23 9.45 0 -4 -6 144.92 11.04 0 4 -6 174.32 11.22 0 -4 -6 158.60 9.91 0 4 6 172.25 10.40 0 4 -7 3.36 1.44 0 -4 -7 2.35 1.41 0 -4 -7 3.45 1.85 0 -4 -8 77.96 7.01 0 4 -8 62.96 7.46 0 -4 -8 80.74 8.69 0 -4 8 55.90 7.41 0 -4 -9 172.26 11.08 0 -4 9 174.37 14.40 0 -4 -9 178.16 14.22 0 4 -9 175.23 13.55 0 -4 -9 185.30 11.25 0 -4 -10 95.95 8.11 0 -4 10 86.57 10.54 0 -4 11 347.60 23.03 0 -4 -11 333.69 16.81 0 -4 -12 21.94 3.91 0 -4 -12 30.42 5.09 0 -4 12 26.74 6.35 0 -4 13 42.30 8.86 0 -4 14 4.19 2.95 0 -4 15 4.39 3.36 0 4 -16 13.77 5.51 0 -4 16 4.09 2.42 0 4 -17 75.16 13.46 0 -6 0 45.94 4.35 0 -6 -1 78.95 6.12 0 -6 1 81.92 5.38 0 -6 1 68.84 5.67 0 -6 2 28.12 3.78 0 -6 2 31.98 2.90 0 -6 -2 27.35 3.67 0 -6 3 412.68 17.67 0 -6 3 430.74 13.24 0 -6 -3 394.26 17.55 0 -6 -4 16.91 3.16 0 -6 4 14.74 1.30 0 6 -4 12.86 2.77 0 6 5 49.13 4.91 0 6 -5 54.06 6.10 0 -6 -5 52.66 5.85 0 -6 -6 48.92 6.33 0 6 -6 42.84 5.96 0 6 6 42.76 4.90 0 -6 -6 50.00 5.82 0 -6 -7 475.07 20.20 0 6 7 477.48 19.94 0 6 -7 508.08 22.70 0 6 -8 9.98 3.01 0 -6 8 7.15 2.69 0 -6 -8 12.62 3.18 0 -6 -8 10.45 3.46 0 6 8 12.34 2.88 0 -6 9 6.95 2.85 0 -6 -9 13.43 3.46 0 -6 -9 14.42 4.53 0 -6 -10 5.77 3.19 0 -6 10 0.90 1.54 0 -6 11 27.09 6.27 0 -6 12 13.34 4.84 0 -6 13 4.90 2.60 0 -6 14 34.42 8.21 0 -6 15 14.35 5.73 0 -6 16 -5.13 3.87 0 -8 0 24.12 3.47 0 -8 -1 68.21 6.31 0 -8 1 78.19 6.09 0 -8 1 59.21 5.93 0 -8 2 385.35 19.48 0 -8 -2 469.01 20.43 0 -8 3 1249.67 36.11 0 -8 -3 1248.47 42.09 0 8 -4 2.07 1.69 0 -8 -4 0.51 1.18 0 -8 4 0.58 0.50 0 -8 5 137.24 5.56 0 -8 -5 183.21 11.95 0 -8 5 109.98 9.66 0 8 -5 197.27 12.75 0 8 6 9.59 2.42 0 -8 -6 9.13 2.72 0 -8 6 5.52 2.04 0 8 -6 8.27 2.78 0 8 -7 143.98 12.05 0 8 7 134.35 10.04 0 -8 -7 149.31 11.21 0 -8 -7 126.11 11.59 0 -8 7 131.25 11.54 0 -8 -8 26.56 5.53 0 -8 8 21.07 4.95 0 -8 -8 31.97 5.21 0 8 8 25.27 4.34 0 -8 9 -0.59 1.71 0 8 9 0.23 0.85 0 -8 10 0.34 1.58 0 -8 11 98.67 12.41 0 -8 12 49.34 9.23 0 -8 13 13.45 5.43 0 -8 14 10.10 4.43 0 -8 15 7.92 4.45 0 -10 0 2.90 1.63 0 -10 -1 96.98 8.12 0 -10 1 85.09 7.02 0 -10 2 1.75 0.94 0 -10 -2 0.46 0.92 0 -10 -3 5.31 1.99 0 -10 3 4.13 1.39 0 -10 3 5.27 2.01 0 -10 4 299.12 17.38 0 -10 4 283.77 11.60 0 -10 -4 284.97 16.47 0 -10 5 136.17 6.49 0 10 -5 134.48 11.19 0 -10 -5 142.61 11.20 0 -10 5 117.86 10.87 0 -10 6 57.28 3.50 0 -10 6 49.81 6.99 0 10 -6 55.34 7.42 0 -10 -6 54.86 6.92 0 -10 7 4.83 2.28 0 10 7 7.47 2.56 0 10 8 279.68 16.77 0 -10 8 320.08 20.61 0 -10 9 542.45 28.64 0 10 9 400.65 22.12 0 -10 10 0.14 1.15 0 10 10 2.74 2.15 0 -10 11 52.88 9.33 0 -10 12 31.05 7.35 0 -10 13 46.64 9.63 0 -10 14 6.03 3.97 0 -10 15 26.79 7.92 0 -12 0 11.22 2.98 0 -12 1 42.60 6.10 0 -12 1 34.14 4.72 0 -12 -1 45.70 5.95 0 -12 2 121.62 11.05 0 -12 -2 125.90 10.45 0 -12 2 145.07 9.48 0 -12 3 35.93 4.30 0 -12 3 46.02 6.70 0 -12 -3 39.97 5.85 0 -12 4 -0.06 1.62 0 -12 4 -0.60 0.69 0 -12 5 0.70 1.31 0 -12 5 1.85 0.81 0 -12 6 1.88 1.20 0 -12 6 5.79 1.31 0 -12 7 9.31 3.09 0 -12 7 8.80 1.38 0 12 8 117.08 10.64 0 -12 8 117.94 12.63 0 -12 9 182.85 16.48 0 12 9 141.55 12.35 0 12 10 81.09 9.61 0 -12 10 91.98 12.00 0 -12 11 72.82 11.37 0 -12 12 2.21 2.67 0 -12 13 112.89 15.59 0 -12 14 23.51 7.45 0 -14 0 9.10 2.79 0 -14 -1 6.61 2.58 0 -14 1 2.98 2.66 0 -14 1 7.56 2.51 0 -14 2 133.94 12.59 0 -14 2 131.27 9.68 0 -14 3 275.75 13.95 0 -14 3 200.75 16.21 0 -14 4 42.00 4.67 0 -14 4 51.30 7.97 0 -14 5 -0.71 0.44 0 -14 5 1.75 1.51 0 -14 6 29.91 6.15 0 -14 6 24.83 2.98 0 -14 7 116.70 12.69 0 -14 7 108.71 6.43 0 -14 8 33.64 7.15 0 -14 9 21.42 5.81 0 -14 10 20.17 5.95 0 -14 11 27.20 7.22 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24.37 2.53 -8 0 8 23.67 3.47 -8 0 7 1.25 0.90 8 0 -7 0.98 0.71 -8 0 7 0.78 1.16 8 0 -6 479.02 17.36 -8 0 6 425.34 16.06 -8 0 6 480.42 22.03 8 0 -5 1.48 1.19 -8 0 5 0.49 0.41 -8 0 4 985.34 27.86 8 0 -4 792.42 30.66 8 0 -3 0.90 1.79 -8 0 2 -0.29 0.83 -8 0 1 0.85 1.10 -8 0 0 394.51 17.88 -8 0 0 418.99 19.97 -8 0 -1 2.75 1.81 -8 0 -1 -0.65 0.67 -8 0 -2 12.49 3.28 -8 0 -2 10.73 2.98 -8 0 -3 2.01 1.93 -8 0 -3 0.58 1.31 -8 0 -4 1.09 1.61 -8 0 -4 0.89 0.91 -8 0 -5 0.66 1.57 -8 0 -5 -0.52 1.14 -8 0 -6 4.15 2.33 -8 0 -7 -1.31 1.95 -8 0 -8 1.49 1.82 -8 0 -9 1.85 1.89 -8 0 -10 33.85 7.66 -8 0 -11 4.18 3.61 -8 0 -12 2.38 1.63 -8 0 -13 2.77 2.72 -8 0 -14 118.61 16.40 -8 -2 18 13.79 5.44 -8 -2 17 27.26 7.07 -8 -2 16 8.27 3.64 -8 2 16 16.54 4.70 -8 2 16 21.18 5.78 -8 -2 15 14.41 4.40 -8 -2 15 16.46 3.85 -8 2 15 13.96 4.34 -8 2 15 14.44 4.36 -8 -2 14 183.77 12.80 -8 2 14 186.59 14.87 -8 -2 14 173.87 15.68 -8 2 14 184.10 15.80 -8 -2 13 50.57 5.96 -8 2 13 51.97 7.17 -8 -2 13 48.89 7.68 8 -2 -13 42.13 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4.56 -17 -1 3 -2.53 3.68 -17 1 3 0.16 1.59 -17 -1 2 -2.04 1.95 -17 1 2 1.42 1.63 -17 -1 1 47.59 12.61 -17 1 1 54.74 11.65 -17 -1 0 5.56 4.35 -17 1 0 -2.85 3.98 -17 -1 -1 -2.15 3.74 -17 1 -1 3.40 4.47 -17 -1 -2 3.90 4.11 -17 1 -2 3.88 3.74 -17 -1 -3 3.01 3.73 -17 1 -3 -2.75 3.69 -17 1 -3 5.80 4.13 -17 1 -4 39.16 10.76 -17 -3 13 0.93 1.71 -17 -3 12 4.60 2.78 -17 3 11 5.77 2.95 -17 -3 11 6.07 3.65 -17 3 10 1.96 2.16 -17 -3 10 3.86 2.93 -17 3 9 7.00 3.63 -17 -3 9 5.24 3.59 -17 3 8 18.87 5.78 -17 -3 8 10.74 4.97 -17 -3 7 0.33 2.47 -17 3 7 1.00 1.53 -17 -3 6 11.99 5.75 -17 3 6 21.23 6.17 -17 -3 5 0.44 4.21 -17 3 5 14.07 5.17 -17 -3 4 30.93 9.22 -17 3 4 42.24 8.79 -17 -3 3 -0.31 3.52 -17 3 3 8.35 4.71 -17 -3 2 31.40 9.77 -17 3 2 40.51 9.16 -17 3 1 9.63 4.17 -17 -3 1 12.34 6.89 -17 3 1 11.94 4.67 -17 3 0 31.58 7.28 -17 3 0 56.81 11.00 -17 3 -1 12.55 4.61 -17 3 -1 24.01 7.63 -17 3 -2 3.70 1.69 -17 3 -2 4.58 2.86 -17 3 -3 44.89 10.74 -17 3 -3 6.35 3.68 -17 3 -4 10.76 4.70 -17 3 -5 16.17 6.51 -17 -5 13 1.91 2.16 -17 -5 12 25.03 6.11 -17 -5 11 3.83 2.21 -17 -5 10 -0.50 2.51 -17 5 9 1.87 1.65 -17 -5 9 4.78 3.32 -17 5 8 64.07 9.95 -17 -5 8 47.14 9.94 -17 5 7 6.25 3.59 -17 -5 7 0.79 2.82 -17 5 6 14.73 4.93 -17 -5 6 5.09 2.59 -17 5 5 2.98 2.31 -17 -5 5 -7.56 6.94 -17 -5 4 34.69 10.50 -17 5 4 28.74 7.22 -17 5 3 16.19 5.30 -17 5 3 16.80 5.55 -17 5 2 19.61 5.70 -17 5 2 20.83 6.10 -17 5 1 0.93 1.53 -17 5 1 0.48 1.31 -17 5 0 21.05 6.06 -17 5 0 36.38 8.55 -17 5 -1 0.69 2.61 -17 5 -1 2.91 2.58 -17 5 -2 9.02 4.14 -17 5 -2 19.68 6.28 -17 5 -3 11.91 4.80 -17 5 -4 59.89 11.22 -17 5 -5 0.48 1.78 -17 -7 12 15.84 5.16 -17 -7 11 4.08 2.70 -17 -7 10 3.39 2.65 -17 -7 9 5.69 4.07 -17 -7 8 3.17 3.88 -17 7 7 -0.92 1.42 -17 -7 7 2.85 2.97 -17 7 6 2.02 2.04 -17 -7 6 -3.10 4.42 -17 7 5 -1.77 2.34 -17 -7 5 -8.62 5.39 -17 7 4 45.95 8.91 -17 7 4 30.65 6.63 -17 7 3 47.82 8.81 -17 7 3 38.45 7.71 -17 7 2 78.92 11.48 -17 7 2 65.08 10.38 -17 7 1 -0.56 1.14 -17 7 1 1.50 2.47 -17 7 0 0.87 2.08 -17 7 0 6.12 4.19 -17 7 -1 9.27 4.13 -17 7 -1 11.54 4.60 -17 7 -2 10.24 4.54 -17 7 -2 17.18 6.00 -17 7 -3 52.24 9.50 -17 7 -4 18.94 6.17 -17 -9 11 3.20 2.07 -17 -9 10 5.91 3.43 -17 -9 9 4.68 3.59 -17 -9 8 5.11 4.19 -17 -9 7 7.96 4.67 -17 -9 6 0.43 1.78 -17 9 4 53.69 9.03 -17 9 3 2.14 1.25 -17 9 3 4.87 3.52 -17 9 2 19.80 5.78 -17 9 2 13.91 4.80 -17 9 1 3.23 2.88 -17 9 1 1.68 1.81 -17 9 0 0.31 2.03 -17 9 0 0.76 1.78 -17 9 -1 9.81 4.17 -17 9 -1 1.59 3.11 -17 9 -2 44.52 8.28 -17 9 -3 14.07 5.06 -17 -11 7 2.46 2.22 -17 -11 6 15.77 5.68 -17 -11 5 -0.70 2.64 -17 11 1 -2.71 1.52 -17 11 0 -0.64 1.48 -17 -13 6 0.66 2.31 -17 -13 5 23.07 7.02 -18 0 8 -0.82 1.47 -18 0 7 -4.10 2.92 -18 0 6 5.56 4.19 -18 0 5 4.24 3.58 -18 0 4 -0.87 1.96 -18 0 3 -4.80 4.34 -18 0 2 20.09 7.64 -18 0 1 -3.73 3.30 -18 -2 9 5.21 3.33 -18 -2 8 63.01 11.25 -18 -2 7 -0.93 1.83 -18 2 7 2.49 2.71 -18 -2 6 15.21 6.74 -18 2 6 6.58 4.30 -18 -2 5 -3.24 1.79 -18 2 5 7.63 4.82 -18 -2 4 -5.42 5.14 -18 2 4 8.41 4.74 -18 -2 3 -7.19 4.86 -18 2 3 -4.70 3.14 -18 -2 2 5.94 4.66 -18 2 2 0.72 2.07 -18 2 1 3.20 3.52 -18 2 0 7.22 4.86 -18 -4 9 10.79 5.37 -18 -4 8 13.71 6.01 -18 -4 7 13.89 6.07 -18 -4 6 -1.50 3.26 -18 -4 5 -5.02 4.69 -18 4 5 4.41 3.45 -18 -4 4 -1.35 2.45 -18 4 4 1.07 2.29 -18 4 3 1.85 2.79 -18 4 2 5.23 3.78 -18 4 1 10.61 4.48 -18 4 1 18.72 6.56 -18 4 0 15.22 5.49 -18 4 -1 3.17 3.25 -18 6 3 11.62 4.66 -18 6 2 5.35 3.53 -18 6 1 2.44 2.47 -18 6 0 7.85 4.48 -18 6 -1 -4.29 3.42 -18 8 2 5.59 3.43 -18 8 1 1.67 2.13 -18 8 0 18.54 6.59 0 0 0 0.00 0.00 TITL tpa_2 in C2/c REM C2/c (#15 in standard setting) CELL 0.71073 14.609543 17.990881 14.014657 90.0000 104.8425 90.0000 ZERR 8.00 0.001090 0.001240 0.000952 0.0000 0.0072 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O UNIT 88.00 80.00 8.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 97184 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.646 _oxdiff_exptl_absorpt_empirical_full_min 0.651 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_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 0.500000 1.01300(4) 0.750000 0.0238(2) Uani 1 2 d S T P . . O1 O 0.57811(12) 1.05489(9) 0.73356(10) 0.0349(4) Uani 1 1 d . . . . . N1 N 0.31867(13) 0.58830(10) 0.24968(12) 0.0287(5) Uani 1 1 d . . . . . C1 C 0.27309(15) 0.60730(12) 0.14997(14) 0.0245(5) Uani 1 1 d . . . . . C2 C 0.20291(15) 0.66188(13) 0.12988(16) 0.0304(5) Uani 1 1 d . . . . . H2 H 0.184872 0.685041 0.181539 0.037 Uiso 1 1 calc R U . . . C3 C 0.15997(16) 0.68169(13) 0.03319(16) 0.0338(6) Uani 1 1 d . . . . . H3 H 0.113812 0.718551 0.020542 0.041 Uiso 1 1 calc R U . . . C4 C 0.18491(17) 0.64737(13) -0.04447(16) 0.0348(6) Uani 1 1 d . . . . . H4 H 0.155975 0.660995 -0.109180 0.042 Uiso 1 1 calc R U . . . C5 C 0.25316(17) 0.59269(14) -0.02509(16) 0.0347(6) Uani 1 1 d . . . . . H5 H 0.269040 0.568660 -0.077388 0.042 Uiso 1 1 calc R U . . . C6 C 0.29847(16) 0.57287(12) 0.07058(16) 0.0291(5) Uani 1 1 d . . . . . H6 H 0.345662 0.536820 0.082357 0.035 Uiso 1 1 calc R U . . . C7 C 0.35037(15) 0.51477(12) 0.27606(15) 0.0245(5) Uani 1 1 d . . . . . C8 C 0.43427(16) 0.50142(13) 0.34774(16) 0.0319(5) Uani 1 1 d . . . . . H8 H 0.471064 0.541233 0.377975 0.038 Uiso 1 1 calc R U . . . C9 C 0.46325(18) 0.42999(14) 0.37426(18) 0.0400(6) Uani 1 1 d . . . . . H9 H 0.519107 0.421749 0.422698 0.048 Uiso 1 1 calc R U . . . C10 C 0.4093(2) 0.36992(14) 0.3288(2) 0.0449(7) Uani 1 1 d . . . . . H10 H 0.428691 0.321660 0.347551 0.054 Uiso 1 1 calc R U . . . C11 C 0.32758(18) 0.38185(14) 0.25665(17) 0.0378(6) Uani 1 1 d . . . . . H11 H 0.292572 0.341727 0.224809 0.045 Uiso 1 1 calc R U . . . C12 C 0.29714(16) 0.45396(12) 0.23108(16) 0.0303(5) Uani 1 1 d . . . . . H12 H 0.240633 0.461830 0.183440 0.036 Uiso 1 1 calc R U . . . C13 C 0.32416(15) 0.63957(12) 0.41324(15) 0.0270(5) Uani 1 1 d . . . . . H13 H 0.295806 0.596586 0.428964 0.032 Uiso 1 1 calc R U . . . C14 C 0.34794(15) 0.69627(12) 0.48179(14) 0.0257(5) Uani 1 1 d . . . . . H14 H 0.336292 0.690506 0.543570 0.031 Uiso 1 1 calc R U . . . C15 C 0.38903(14) 0.76189(12) 0.45992(14) 0.0236(5) Uani 1 1 d . . . . . C16 C 0.40687(15) 0.76833(12) 0.36692(14) 0.0274(5) Uani 1 1 d . . . . . H16 H 0.434089 0.811666 0.350611 0.033 Uiso 1 1 calc R U . . . C17 C 0.38465(15) 0.71122(12) 0.29872(15) 0.0284(5) Uani 1 1 d . . . . . H17 H 0.398097 0.716242 0.237672 0.034 Uiso 1 1 calc R U . . . C18 C 0.34241(15) 0.64642(12) 0.32072(14) 0.0252(5) Uani 1 1 d . . . . . C19 C 0.41293(14) 0.82455(12) 0.53121(14) 0.0226(5) Uani 1 1 d . . . . . C20 C 0.40135(15) 0.89779(12) 0.49591(15) 0.0253(5) Uani 1 1 d . . . . . H20 H 0.377216 0.905669 0.428552 0.030 Uiso 1 1 calc R U . . . C21 C 0.42445(15) 0.95870(12) 0.55746(15) 0.0245(5) Uani 1 1 d . . . . . H21 H 0.415136 1.006897 0.532888 0.029 Uiso 1 1 calc R U . . . C22 C 0.46213(14) 0.94522(11) 0.65744(14) 0.0223(5) Uani 1 1 d . . . . . C23 C 0.47672(14) 0.87321(11) 0.69596(14) 0.0200(5) Uani 1 1 d . . . . . C24 C 0.44945(14) 0.81289(11) 0.63312(14) 0.0214(5) Uani 1 1 d . . . . . H24 H 0.455362 0.764843 0.658453 0.026 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 0.0344(5) 0.0179(4) 0.0193(4) 0.000 0.0075(3) 0.000 O1 0.0508(10) 0.0265(9) 0.0276(9) 0.0002(7) 0.0107(7) -0.0139(7) N1 0.0374(11) 0.0225(11) 0.0205(10) -0.0033(8) -0.0026(8) 0.0008(8) C1 0.0293(12) 0.0239(12) 0.0183(11) -0.0036(9) 0.0025(9) -0.0037(9) C2 0.0312(13) 0.0346(14) 0.0240(12) -0.0047(10) 0.0044(10) 0.0013(10) C3 0.0314(13) 0.0325(14) 0.0328(13) 0.0029(11) -0.0004(10) 0.0022(10) C4 0.0472(15) 0.0338(14) 0.0192(12) 0.0028(10) 0.0008(10) -0.0116(11) C5 0.0468(15) 0.0365(15) 0.0237(12) -0.0070(11) 0.0144(11) -0.0112(12) C6 0.0302(12) 0.0275(13) 0.0296(12) -0.0022(10) 0.0081(10) -0.0012(10) C7 0.0284(12) 0.0254(12) 0.0197(11) -0.0032(9) 0.0065(9) 0.0001(9) C8 0.0283(12) 0.0314(13) 0.0336(13) -0.0061(11) 0.0035(10) 0.0008(10) C9 0.0337(14) 0.0425(16) 0.0420(15) 0.0037(13) 0.0066(11) 0.0107(12) C10 0.0622(19) 0.0280(14) 0.0531(17) 0.0072(13) 0.0305(15) 0.0159(13) C11 0.0499(16) 0.0323(15) 0.0355(14) -0.0051(12) 0.0186(12) -0.0081(12) C12 0.0350(13) 0.0296(14) 0.0257(12) -0.0038(10) 0.0067(10) -0.0040(10) C13 0.0324(12) 0.0222(12) 0.0236(11) 0.0016(10) 0.0022(9) -0.0028(9) C14 0.0335(12) 0.0269(13) 0.0154(11) -0.0017(9) 0.0039(9) 0.0009(10) C15 0.0269(11) 0.0225(12) 0.0190(11) 0.0015(9) 0.0015(9) 0.0035(9) C16 0.0357(13) 0.0245(12) 0.0195(11) 0.0010(10) 0.0027(9) -0.0037(10) C17 0.0363(13) 0.0303(13) 0.0177(11) -0.0005(10) 0.0052(9) -0.0013(10) C18 0.0293(12) 0.0231(12) 0.0192(11) -0.0040(9) -0.0012(9) 0.0015(9) C19 0.0246(11) 0.0236(12) 0.0190(11) -0.0013(9) 0.0043(9) 0.0015(9) C20 0.0314(12) 0.0252(12) 0.0170(11) 0.0032(9) 0.0021(9) 0.0036(9) C21 0.0339(12) 0.0193(12) 0.0203(11) 0.0034(9) 0.0069(9) 0.0040(9) C22 0.0278(12) 0.0194(11) 0.0208(11) -0.0008(9) 0.0083(9) 0.0014(9) C23 0.0228(11) 0.0197(11) 0.0179(10) 0.0000(9) 0.0058(8) 0.0009(8) C24 0.0269(11) 0.0166(11) 0.0205(11) 0.0019(9) 0.0058(9) 0.0020(9) 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 O1 S1 O1 116.62(14) . 2_656 ? O1 S1 C22 110.97(9) . . ? O1 S1 C22 111.65(9) . 2_656 ? O1 S1 C22 110.96(9) 2_656 2_656 ? O1 S1 C22 111.65(9) 2_656 . ? C22 S1 C22 92.47(14) 2_656 . ? C7 N1 C1 121.18(16) . . ? C7 N1 C18 119.84(17) . . ? C18 N1 C1 118.55(17) . . ? C2 C1 N1 120.04(18) . . ? C2 C1 C6 118.7(2) . . ? C6 C1 N1 121.25(19) . . ? C1 C2 H2 119.9 . . ? C3 C2 C1 120.2(2) . . ? C3 C2 H2 119.9 . . ? C2 C3 H3 119.6 . . ? C4 C3 C2 120.8(2) . . ? C4 C3 H3 119.6 . . ? C3 C4 H4 120.4 . . ? C5 C4 C3 119.2(2) . . ? C5 C4 H4 120.4 . . ? C4 C5 H5 119.4 . . ? C4 C5 C6 121.2(2) . . ? C6 C5 H5 119.4 . . ? C1 C6 H6 120.1 . . ? C5 C6 C1 119.8(2) . . ? C5 C6 H6 120.1 . . ? C8 C7 N1 121.14(19) . . ? C8 C7 C12 118.4(2) . . ? C12 C7 N1 120.4(2) . . ? C7 C8 H8 119.7 . . ? C9 C8 C7 120.7(2) . . ? C9 C8 H8 119.7 . . ? C8 C9 H9 119.9 . . ? C8 C9 C10 120.2(2) . . ? C10 C9 H9 119.9 . . ? C9 C10 H10 120.0 . . ? C11 C10 C9 120.0(2) . . ? C11 C10 H10 120.0 . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.9(2) . . ? C12 C11 H11 120.1 . . ? C7 C12 H12 119.6 . . ? C11 C12 C7 120.7(2) . . ? C11 C12 H12 119.6 . . ? C14 C13 H13 119.8 . . ? C14 C13 C18 120.5(2) . . ? C18 C13 H13 119.8 . . ? C13 C14 H14 119.4 . . ? C13 C14 C15 121.18(18) . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 117.96(19) . . ? C14 C15 C19 122.31(17) . . ? C16 C15 C19 119.73(19) . . ? C15 C16 H16 119.5 . . ? C17 C16 C15 121.0(2) . . ? C17 C16 H16 119.5 . . ? C16 C17 H17 119.7 . . ? C16 C17 C18 120.55(18) . . ? C18 C17 H17 119.7 . . ? C13 C18 N1 120.99(19) . . ? C17 C18 N1 120.21(18) . . ? C17 C18 C13 118.80(19) . . ? C20 C19 C15 119.26(18) . . ? C20 C19 C24 118.58(19) . . ? C24 C19 C15 122.13(19) . . ? C19 C20 H20 118.8 . . ? C21 C20 C19 122.46(19) . . ? C21 C20 H20 118.8 . . ? C20 C21 H21 121.3 . . ? C20 C21 C22 117.5(2) . . ? C22 C21 H21 121.3 . . ? C21 C22 S1 126.15(16) . . ? C21 C22 C23 122.20(18) . . ? C23 C22 S1 111.63(14) . . ? C22 C23 C23 112.11(11) . 2_656 ? C24 C23 C22 119.21(18) . . ? C24 C23 C23 128.67(12) . 2_656 ? C19 C24 H24 120.0 . . ? C23 C24 C19 119.97(19) . . ? C23 C24 H24 120.0 . . ? 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 O1 1.4345(15) . ? S1 O1 1.4345(15) 2_656 ? S1 C22 1.763(2) 2_656 ? S1 C22 1.763(2) . ? N1 C1 1.427(3) . ? N1 C7 1.419(3) . ? N1 C18 1.424(3) . ? C1 C2 1.395(3) . ? C1 C6 1.404(3) . ? C2 H2 0.9300 . ? C2 C3 1.386(3) . ? C3 H3 0.9300 . ? C3 C4 1.379(3) . ? C4 H4 0.9300 . ? C4 C5 1.377(4) . ? C5 H5 0.9300 . ? C5 C6 1.381(3) . ? C6 H6 0.9300 . ? C7 C8 1.392(3) . ? C7 C12 1.396(3) . ? C8 H8 0.9300 . ? C8 C9 1.374(3) . ? C9 H9 0.9300 . ? C9 C10 1.392(4) . ? C10 H10 0.9300 . ? C10 C11 1.370(4) . ? C11 H11 0.9300 . ? C11 C12 1.388(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C13 C14 1.383(3) . ? C13 C18 1.395(3) . ? C14 H14 0.9300 . ? C14 C15 1.394(3) . ? C15 C16 1.398(3) . ? C15 C19 1.487(3) . ? C16 H16 0.9300 . ? C16 C17 1.384(3) . ? C17 H17 0.9300 . ? C17 C18 1.390(3) . ? C19 C20 1.403(3) . ? C19 C24 1.407(3) . ? C20 H20 0.9300 . ? C20 C21 1.382(3) . ? C21 H21 0.9300 . ? C21 C22 1.389(3) . ? C22 C23 1.399(3) . ? C23 C23 1.493(4) 2_656 ? C23 C24 1.390(3) . ? C24 H24 0.9300 . ? 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 C22 C23 C23 -2.0(3) . . . 2_656 ? S1 C22 C23 C24 179.06(14) . . . . ? O1 S1 C22 C21 -63.3(2) . . . . ? O1 S1 C22 C21 68.6(2) 2_656 . . . ? O1 S1 C22 C23 -112.99(15) 2_656 . . . ? O1 S1 C22 C23 115.07(15) . . . . ? N1 C1 C2 C3 178.5(2) . . . . ? N1 C1 C6 C5 -179.8(2) . . . . ? N1 C7 C8 C9 178.6(2) . . . . ? N1 C7 C12 C11 -179.86(18) . . . . ? C1 N1 C7 C8 142.9(2) . . . . ? C1 N1 C7 C12 -37.8(3) . . . . ? C1 N1 C18 C13 135.1(2) . . . . ? C1 N1 C18 C17 -45.1(3) . . . . ? C1 C2 C3 C4 0.8(3) . . . . ? C2 C1 C6 C5 -0.8(3) . . . . ? C2 C3 C4 C5 0.2(3) . . . . ? C3 C4 C5 C6 -1.5(3) . . . . ? C4 C5 C6 C1 1.8(3) . . . . ? C6 C1 C2 C3 -0.4(3) . . . . ? C7 N1 C1 C2 147.3(2) . . . . ? C7 N1 C1 C6 -33.7(3) . . . . ? C7 N1 C18 C13 -52.4(3) . . . . ? C7 N1 C18 C17 127.4(2) . . . . ? C7 C8 C9 C10 0.6(3) . . . . ? C8 C7 C12 C11 -0.5(3) . . . . ? C8 C9 C10 C11 0.8(4) . . . . ? C9 C10 C11 C12 -2.1(3) . . . . ? C10 C11 C12 C7 2.0(3) . . . . ? C12 C7 C8 C9 -0.7(3) . . . . ? C13 C14 C15 C16 -0.9(3) . . . . ? C13 C14 C15 C19 178.3(2) . . . . ? C14 C13 C18 N1 179.7(2) . . . . ? C14 C13 C18 C17 -0.1(3) . . . . ? C14 C15 C16 C17 -0.2(3) . . . . ? C14 C15 C19 C20 -143.5(2) . . . . ? C14 C15 C19 C24 38.4(3) . . . . ? C15 C16 C17 C18 1.1(3) . . . . ? C15 C19 C20 C21 -178.24(18) . . . . ? C15 C19 C24 C23 175.64(18) . . . . ? C16 C15 C19 C20 35.8(3) . . . . ? C16 C15 C19 C24 -142.4(2) . . . . ? C16 C17 C18 N1 179.2(2) . . . . ? C16 C17 C18 C13 -1.0(3) . . . . ? C18 N1 C1 C2 -40.3(3) . . . . ? C18 N1 C1 C6 138.7(2) . . . . ? C18 N1 C7 C8 -29.4(3) . . . . ? C18 N1 C7 C12 149.90(19) . . . . ? C18 C13 C14 C15 1.1(3) . . . . ? C19 C15 C16 C17 -179.4(2) . . . . ? C19 C20 C21 C22 1.3(3) . . . . ? C20 C19 C24 C23 -2.5(3) . . . . ? C20 C21 C22 S1 178.20(15) . . . . ? C20 C21 C22 C23 0.0(3) . . . . ? C21 C22 C23 C23 176.5(2) . . . 2_656 ? C21 C22 C23 C24 -2.5(3) . . . . ? C22 S1 C22 C21 -177.6(2) 2_656 . . . ? C22 S1 C22 C23 0.74(10) 2_656 . . . ? C22 C23 C24 C19 3.8(3) . . . . ? C23 C23 C24 C19 -175.0(2) 2_656 . . . ? C24 C19 C20 C21 0.0(3) . . . . ?