#------------------------------------------------------------------------------ #$Date: 2024-06-07 04:52:58 +0300 (Fri, 07 Jun 2024) $ #$Revision: 292253 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571797.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_1571797 loop_ _publ_author_name 'Liu, Yang' 'Gong, Xiao-Ting' 'Wang, Kang-Nan' 'He, Simeng' 'Wang, Yumeng' 'Lin, Qiaowen' 'Liu, Zhiqiang' 'Yu, Xiaoqiang' 'Liu, Bin' _publ_section_title ; Dual-targeted fluorescent probe for tracking polarity and phase transition processes during lipophagy. ; _journal_name_full 'Materials horizons' _journal_paper_doi 10.1039/d4mh00190g _journal_year 2024 _chemical_formula_moiety 'C30 H24 N O2 S, C2 H6 O, I' _chemical_formula_sum 'C32 H30 I N O3 S' _chemical_formula_weight 635.53 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-05-13 _audit_creation_method ; Olex2 1.5-beta (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-05-14 deposited with the CCDC. 2024-05-17 downloaded from the CCDC. ; _cell_angle_alpha 87.189(9) _cell_angle_beta 78.325(9) _cell_angle_gamma 74.102(10) _cell_formula_units_Z 2 _cell_length_a 9.431(3) _cell_length_b 11.607(3) _cell_length_c 13.247(4) _cell_measurement_reflns_used 9829 _cell_measurement_temperature 173.0 _cell_measurement_theta_max 66.523 _cell_measurement_theta_min 3.407 _cell_volume 1365.7(7) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 173.0 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON III' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_unetI/netI 0.0343 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 16753 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 66.627 _diffrn_reflns_theta_max 66.627 _diffrn_reflns_theta_min 3.407 _diffrn_source_current 1.1 _diffrn_source_power 0.05500000000000001 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 10.200 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.5248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1295 before and 0.0583 after correction. The Ratio of minimum to maximum transmission is 0.6971. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light black' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.545 _exptl_crystal_description block _exptl_crystal_F_000 644 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.843 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.071 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 355 _refine_ls_number_reflns 4780 _refine_ls_number_restraints 36 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0317 _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^)+(0.0553P)^2^+0.4166P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.0871 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4606 _reflns_number_total 4780 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4mh00190g10.cif _cod_data_source_block cu_230301e_0m _cod_original_cell_volume 1365.7(6) _cod_database_code 1571797 _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. ; _shelx_estimated_absorpt_t_max 0.905 _shelx_estimated_absorpt_t_min 0.496 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Uiso/Uaniso restraints and constraints C29 \\sim C7 \\sim O1 \\sim C23 \\sim O3: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A I1 \\sim I1A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A 3. Others Sof(I1A)=1-FVAR(1) Sof(I1)=FVAR(1) 4.a Ternary CH refined with riding coordinates: C23(H23) 4.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C21(H21A,H21B), C7(H7A,H7B), C29(H29A,H29B), C15(H15A,H15B) 4.c Aromatic/amide H refined with riding coordinates: C8(H8), C10(H10), C12(H12), C16(H16), C20(H20), C26(H26), C32(H32), C17(H17), C9(H9), C19(H19), C5(H5), C11(H11), C3(H3), C25(H25), C13(H13) 4.d Idealised Me refined as rotating group: C31(H31A,H31B,H31C) 4.e Idealised tetrahedral OH refined as rotating group: O2(H2) ; _shelx_res_file ; TITL cu_230301e_0m_a.res in P-1 cu_230301e_0m.res created by SHELXL-2018/3 at 22:25:25 on 13-May-2024 REM Old TITL cu_230301E_0m in P1 REM SHELXT solution in P-1: R1 0.113, Rweak 0.014, Alpha 0.038 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C32 I N4 S CELL 1.54178 9.4307 11.607 13.2474 87.189 78.325 74.102 ZERR 2 0.0026 0.0031 0.0035 0.009 0.009 0.01 LATT 1 SFAC C H I N O S UNIT 64 60 2 2 6 2 SIMU 0.004 0.008 2 C29 C7 O1 C23 O3 SIMU 0.01 0.01 2 I1 I1A L.S. 24 0 0 PLAN 2 SIZE 0.06 0.08 0.01 TEMP -100.15 CONF list 4 MORE -1 BOND $H fmap 2 53 ACTA OMIT -4 1 0 REM REM REM WGHT 0.055300 0.416600 FVAR 0.52744 0.98470 PART 1 I1 3 0.745714 0.293059 0.120031 21.00000 0.07020 0.05840 = 0.04778 -0.00342 -0.01870 -0.01466 PART 0 S1 6 0.665464 0.199499 0.591891 11.00000 0.05542 0.05373 = 0.04284 -0.00253 -0.01265 -0.01538 O1 5 0.409878 0.158462 0.905762 11.00000 0.06780 0.05415 = 0.06056 -0.00671 -0.00976 -0.02319 N1 4 0.624586 0.291947 0.769561 11.00000 0.04312 0.04685 = 0.04255 -0.00020 -0.00904 -0.01450 O3 5 0.286941 0.260265 1.053113 11.00000 0.07783 0.06410 = 0.06256 -0.00427 0.01081 -0.03160 O2 5 0.604480 0.188553 0.363094 11.00000 0.08706 0.07813 = 0.05967 0.00136 -0.01434 -0.00944 AFIX 147 H2 2 0.622978 0.225725 0.308139 11.00000 -1.50000 AFIX 0 C1 1 0.224712 0.512170 0.454932 11.00000 0.04060 0.04065 = 0.04583 0.00239 -0.00758 -0.01420 C4 1 0.093199 0.600945 0.436486 11.00000 0.04286 0.04029 = 0.04632 0.00255 -0.00841 -0.01586 C6 1 0.004785 0.684293 0.515775 11.00000 0.04528 0.04008 = 0.05286 -0.00137 -0.00653 -0.01434 C8 1 0.443775 0.406458 0.665969 11.00000 0.04744 0.05196 = 0.04504 0.00160 -0.00922 -0.01669 AFIX 43 H8 2 0.394869 0.464316 0.718988 11.00000 -1.20000 AFIX 0 C10 1 0.307396 0.429096 0.372463 11.00000 0.04126 0.04581 = 0.04676 0.00074 -0.00857 -0.01014 AFIX 43 H10 2 0.395505 0.369918 0.382430 11.00000 -1.20000 AFIX 0 C12 1 0.394511 0.417996 0.576356 11.00000 0.04546 0.04758 = 0.04569 0.00297 -0.01023 -0.01644 AFIX 43 H12 2 0.449044 0.360926 0.523752 11.00000 -1.20000 AFIX 0 C14 1 0.265771 0.509508 0.552441 11.00000 0.04681 0.04521 = 0.04502 0.00248 -0.01072 -0.01776 C16 1 0.176855 0.594441 0.628368 11.00000 0.05458 0.05048 = 0.04362 -0.00146 -0.01046 -0.01809 AFIX 43 H16 2 0.204990 0.593361 0.693405 11.00000 -1.20000 AFIX 0 C18 1 -0.084245 0.692283 0.322421 11.00000 0.04199 0.04704 = 0.05678 0.00808 -0.01233 -0.01382 C20 1 0.262698 0.433283 0.281270 11.00000 0.04745 0.04799 = 0.04386 -0.00115 -0.00676 -0.01355 AFIX 43 H20 2 0.319284 0.375957 0.229344 11.00000 -1.20000 AFIX 0 C22 1 0.568502 0.308886 0.683685 11.00000 0.04696 0.04893 = 0.04304 0.00291 -0.00935 -0.01881 C24 1 0.047818 0.605372 0.339735 11.00000 0.04282 0.04478 = 0.04937 0.00301 -0.01003 -0.01704 C26 1 0.050544 0.678640 0.610366 11.00000 0.05676 0.04584 = 0.05010 -0.00789 -0.00554 -0.01585 AFIX 43 H26 2 -0.007038 0.734287 0.663333 11.00000 -1.20000 AFIX 0 C28 1 0.132524 0.521632 0.260694 11.00000 0.04204 0.04927 = 0.04658 0.00337 -0.00906 -0.01717 C30 1 0.747907 0.191098 0.767462 11.00000 0.04236 0.04483 = 0.04764 0.00063 -0.00812 -0.01566 C32 1 -0.128621 0.769646 0.495938 11.00000 0.04959 0.04156 = 0.06101 -0.00407 -0.00624 -0.01053 AFIX 43 H32 2 -0.188238 0.825050 0.548537 11.00000 -1.20000 AFIX 0 C2 1 0.564750 0.374587 0.860476 11.00000 0.04778 0.04596 = 0.04198 -0.00198 -0.00996 -0.01278 AFIX 23 H2A 2 0.549676 0.458100 0.835653 11.00000 -1.20000 H2B 2 0.641261 0.359840 0.904352 11.00000 -1.20000 AFIX 0 C17 1 0.830715 0.151042 0.844391 11.00000 0.05035 0.04952 = 0.04874 0.00136 -0.01306 -0.01619 AFIX 43 H17 2 0.805923 0.192299 0.908457 11.00000 -1.20000 AFIX 0 C9 1 0.987957 -0.012537 0.730913 11.00000 0.04954 0.04829 = 0.06709 -0.00039 -0.00866 -0.01274 AFIX 43 H9 2 1.070676 -0.082118 0.719813 11.00000 -1.20000 AFIX 0 C19 1 0.085863 0.528286 0.166528 11.00000 0.04999 0.06645 = 0.04697 -0.00082 -0.01104 -0.01880 AFIX 43 H19 2 0.142558 0.473082 0.113012 11.00000 -1.20000 AFIX 0 C5 1 -0.171393 0.773105 0.404449 11.00000 0.04599 0.04290 = 0.06943 0.00404 -0.01129 -0.00928 AFIX 43 H5 2 -0.260988 0.830199 0.394181 11.00000 -1.20000 AFIX 0 C21 1 0.418006 0.362296 0.926152 11.00000 0.04955 0.04549 = 0.04876 -0.00261 -0.00717 -0.01130 AFIX 23 H21A 2 0.385338 0.424215 0.981076 11.00000 -1.20000 H21B 2 0.341175 0.380526 0.882377 11.00000 -1.20000 AFIX 0 C11 1 0.949770 0.049655 0.824645 11.00000 0.05084 0.05252 = 0.06155 0.00466 -0.01767 -0.01692 AFIX 43 H11 2 1.007557 0.021203 0.876204 11.00000 -1.20000 AFIX 0 C23 1 0.418630 0.242866 0.976514 11.00000 0.05552 0.05391 = 0.04707 -0.00122 -0.00901 -0.01875 AFIX 13 H23 2 0.509975 0.211706 1.007549 11.00000 -1.20000 AFIX 0 C3 1 -0.126504 0.695013 0.227151 11.00000 0.04708 0.05856 = 0.06278 0.01206 -0.01728 -0.01527 AFIX 43 H3 2 -0.214384 0.753039 0.215186 11.00000 -1.20000 AFIX 0 C25 1 -0.042216 0.614397 0.149866 11.00000 0.05470 0.07130 = 0.05195 0.00725 -0.01923 -0.01968 AFIX 43 H25 2 -0.071966 0.617895 0.085172 11.00000 -1.20000 AFIX 0 C13 1 0.906150 0.026583 0.654397 11.00000 0.05509 0.04937 = 0.05376 -0.00608 -0.00570 -0.01490 AFIX 43 H13 2 0.931019 -0.015100 0.590534 11.00000 -1.20000 AFIX 0 C27 1 0.785776 0.129336 0.673968 11.00000 0.04853 0.04848 = 0.04548 0.00108 -0.01150 -0.01738 C7 1 0.244705 0.151071 1.061260 11.00000 0.08150 0.06907 = 0.07920 0.00309 0.00044 -0.03599 AFIX 23 H7A 2 0.133904 0.166736 1.075289 11.00000 -1.20000 H7B 2 0.284596 0.100907 1.117195 11.00000 -1.20000 AFIX 0 C29 1 0.312584 0.091224 0.959164 11.00000 0.08676 0.06424 = 0.08095 0.00268 -0.01204 -0.03515 AFIX 23 H29A 2 0.369952 0.007379 0.968123 11.00000 -1.20000 H29B 2 0.233301 0.090985 0.920362 11.00000 -1.20000 AFIX 0 C15 1 0.575784 0.078591 0.340160 11.00000 0.09918 0.07570 = 0.09531 0.02838 -0.01071 -0.00086 AFIX 23 H15A 2 0.536790 0.042927 0.405737 11.00000 -1.20000 H15B 2 0.672346 0.022204 0.308395 11.00000 -1.20000 AFIX 0 C31 1 0.468528 0.089833 0.270913 11.00000 0.10661 0.08574 = 0.09759 -0.01817 0.01315 -0.04013 AFIX 137 H31A 2 0.506287 0.124043 0.205200 11.00000 -1.50000 H31B 2 0.370780 0.142393 0.302862 11.00000 -1.50000 H31C 2 0.457216 0.010537 0.258644 11.00000 -1.50000 AFIX 0 PART 2 I1A 3 0.821039 0.328836 0.094786 -21.00000 0.06260 0.07185 = 0.08833 -0.01160 -0.01210 -0.03968 HKLF 4 REM cu_230301e_0m_a.res in P-1 REM wR2 = 0.0871, GooF = S = 1.043, Restrained GooF = 1.066 for all data REM R1 = 0.0317 for 4606 Fo > 4sig(Fo) and 0.0325 for all 4780 data REM 355 parameters refined using 36 restraints END WGHT 0.0553 0.4166 REM Highest difference peak 0.843, deepest hole -0.273, 1-sigma level 0.071 Q1 1 0.8032 0.2212 0.1099 11.00000 0.05 0.84 Q2 1 0.7066 0.2636 0.1757 11.00000 0.05 0.76 ; _shelx_res_checksum 82480 _shelx_hkl_file ; -1 0 0 40.0273 2.50171 0 1 0 0 36.4672 2.50171 0 2 0 0 2064.07 110.92 0 -3 0 0 325.165 19.2189 0 -3 0 0 383.73 19.4477 0 -3 0 0 326.691 19.4477 0 -3 0 0 312.277 18.8376 0 -3 0 0 352.918 19.524 0 -4 0 0 456.454 26.3453 0 -4 0 0 434.031 25.5608 0 -4 0 0 499.07 26.3453 0 -4 0 0 495.606 26.5414 0 -4 0 0 459.395 26.0838 0 -4 0 0 450.701 26.4107 0 -5 0 0 10.4369 2.22062 0 -5 0 0 9.6042 1.49892 0 -5 0 0 12.3245 2.33166 0 -5 0 0 9.77075 2.27614 0 -5 0 0 14.101 2.16511 0 -6 0 0 815.261 44.1712 0 -6 0 0 744.49 44.502 0 -6 0 0 813.938 44.7382 0 -6 0 0 820.175 43.6043 0 -6 0 0 813.938 44.6909 0 -7 0 0 51.5725 4.68144 0 -7 0 0 52.0164 4.60072 0 -7 0 0 49.1914 3.67251 0 -7 0 0 51.6129 4.11644 0 -7 0 0 50.8461 4.56037 0 -8 0 0 47.7067 4.2586 0 -8 0 0 49.3686 4.39709 0 -8 0 0 44.0367 4.15473 0 -8 0 0 46.1486 3.39303 0 -8 0 0 47.6374 3.8085 0 -9 0 0-0.29749 0.95196 0 -9 0 0 0.29749 0.83297 0 -9 0 0-0.20824 1.2197 0 -9 1 0 31.4434 3.07003 0 -8 1 0 0.4999 1.19975 0 -8 1 0 1.36638 1.33305 0 -8 1 0 0.16663 0.93314 0 -8 1 0 0.46657 0.93314 0 -8 1 0 0.83316 0.96647 0 -7 1 0 16.7974 2.79309 0 -7 1 0 25.6771 3.41378 0 -7 1 0 24.009 3.3362 0 -7 1 0 24.0866 2.28879 0 -7 1 0 22.4185 2.44396 0 -6 1 0 23.6936 2.58277 0 -6 1 0 30.2185 3.39839 0 -6 1 0 25.9138 3.12652 0 -6 1 0 27.4544 3.03589 0 -6 1 0 30.1731 2.58277 0 -5 1 0 227.239 13.6494 0 -5 1 0 217.945 13.1714 0 -5 1 0 227.186 12.9059 0 -5 1 0 211.731 13.5963 0 -5 1 0 236.48 13.9681 0 -4 1 0 84.6237 5.92909 0 -4 1 0 84.8734 6.30356 0 -3 1 0 1348.69 76.8897 0 -3 1 0 1432.42 76.9625 0 -3 1 0 1488.79 77.181 0 -3 1 0 1298.16 76.38 0 -3 1 0 1445.17 76.6712 0 -3 1 0 1510.63 77.4722 0 -2 1 0 816.528 44.671 0 1 -1 0 4287.07 229.315 0 0 1 0 1469.55 76.1666 0 0 1 0 1381.05 76.1666 0 -1 -1 0 1902.31 103.487 0 1 1 0 1969.10 103.487 0 -2 -1 0 21.0353 1.58425 0 -2 -1 0 20.0671 1.40822 0 -2 -1 0 25.26 1.9363 0 2 1 0 23.2356 1.9363 0 -3 -1 0 1289.76 63.948 0 -3 -1 0 1168.61 64.5682 0 -3 -1 0 1164.03 64.4907 0 -3 -1 0 1110.47 63.2503 0 -4 -1 0 13.8308 2.33854 0 -4 -1 0 13.6972 1.67039 0 -4 -1 0 16.4366 2.60581 0 -4 -1 0 12.0936 0.8686 0 -4 -1 0 19.5101 2.53899 0 -4 -1 0 12.0936 2.1381 0 -4 -1 0 15.0335 1.93765 0 -5 -1 0 497.736 29.7716 0 -5 -1 0 561.726 29.6008 0 -5 -1 0 550.624 29.9993 0 -5 -1 0 500.526 29.373 0 -6 -1 0 533.745 27.8906 0 -6 -1 0 472.72 27.9392 0 -6 -1 0 477.911 26.7263 0 -6 -1 0 466.849 27.8906 0 -6 -1 0 486.303 27.5025 0 -7 -1 0 146.98 9.94903 0 -7 -1 0 141.056 8.62249 0 -7 -1 0 155.686 9.74176 0 -7 -1 0 150.877 9.41012 0 -7 -1 0 140.062 9.78321 0 -8 -1 0 27.2765 3.30776 0 -8 -1 0 28.8059 3.45003 0 -8 -1 0 27.241 2.80981 0 -8 -1 0 24.0399 3.02322 0 -9 -1 0 90.7577 6.72347 0 -9 -1 0 100.996 6.96796 0 -9 -1 0 101.882 6.47898 0 -10 -1 0 0.68655 1.18825 0 -10 -1 0 0.87139 1.13544 0 -9 2 0 16.3228 1.72858 0 -9 2 0 16.4051 2.30478 0 -8 2 0 28.0891 2.41245 0 -8 2 0 22.7881 3.07904 0 -8 2 0 24.1213 2.8251 0 -7 2 0 72.6294 5.64134 0 -7 2 0 81.7367 5.97318 0 -7 2 0 76.9803 5.08826 0 -7 2 0 72.0395 6.01005 0 -7 2 0 70.4171 5.12513 0 -6 2 0 60.1822 4.46144 0 -6 2 0 64.086 5.01912 0 -6 2 0 62.9706 5.4052 0 -6 2 0 61.6837 4.33274 0 -6 2 0 56.879 4.89042 0 -5 2 0 132.82 8.00515 0 -5 2 0 141.626 8.7056 0 -5 2 0 131.219 9.10586 0 -5 2 0 119.767 8.50547 0 -5 2 0 127.317 8.10522 0 -4 2 0 192.064 11.8006 0 -4 2 0 183.71 11.3333 0 -4 2 0 200.593 11.3333 0 -4 2 0 200.535 12.4432 0 -3 2 0 575.874 31.6451 0 -3 2 0 592.368 31.9847 0 -3 2 0 549.865 31.6451 0 -3 2 0 598.548 32.7996 0 -3 2 0 570.577 30.8981 0 -2 2 0 3328.54 167.563 0 -2 2 0 2924.51 165.776 0 -2 2 0 3078.56 166.32 0 0 -2 0 3882.32 207.724 0 -1 -2 0 91.7884 5.46414 0 1 2 0 92.7902 5.64628 0 -2 -2 0 1427.86 81.5526 0 2 2 0 1610.67 81.6379 0 -3 -2 0 100.767 5.80219 0 -3 -2 0 111.379 6.10757 0 -3 -2 0 102.829 6.03122 0 -3 -2 0 99.3167 7.0237 0 -3 -2 0 88.3231 7.0237 0 -3 -2 0 97.0264 5.80219 0 3 2 0 112.753 6.48929 0 -4 -2 0 122.275 7.18951 0 -4 -2 0 111.224 7.98835 0 -4 -2 0 117.149 6.59039 0 -5 -2 0 387.528 21.6681 0 -5 -2 0 380.667 20.0101 0 -5 -2 0 369.982 21.6109 0 -5 -2 0 342.882 20.6962 0 -6 -2 0 183.53 11.4106 0 -6 -2 0 175.449 10.9699 0 -6 -2 0 166.933 11.2637 0 -7 -2 0 15.0317 2.64524 0 -7 -2 0 15.1157 2.4353 0 -7 -2 0 15.0737 2.47729 0 -7 -2 0 17.1311 3.10711 0 -8 -2 0 104.265 7.69074 0 -8 -2 0 96.6831 7.4741 0 -8 -2 0 117.625 7.40189 0 -9 -2 0 12.8379 2.45567 0 -9 -2 0 14.0191 2.23808 0 -10 -2 0 52.5372 3.81835 0 -10 -2 0 57.7807 4.35614 0 -9 3 0 11.6259 1.37846 0 -8 3 0 21.1075 2.54885 0 -8 3 0 20.2079 2.72877 0 -8 3 0 24.6459 2.18901 0 -7 3 0 5.51846 1.59654 0 -7 3 0 7.94797 2.11715 0 -7 3 0 9.82217 1.59654 0 -6 3 0 154.061 9.11529 0 -6 3 0 127.08 10.7215 0 -6 3 0 145.708 10.2396 0 -6 3 0 163.015 9.95856 0 -5 3 0 111.28 7.16493 0 -5 3 0 100.067 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36.8222 2.68335 0 1 5 0 40.7802 3.2871 0 -2 -5 0 1348.53 74.3877 0 -2 -5 0 1490.77 74.1239 0 -2 -5 0 1413.16 75.1132 0 2 5 0 1315.22 74.7834 0 2 5 0 1344.18 74.6515 0 -3 -5 0 121.985 8.41576 0 -3 -5 0 128.281 7.66769 0 -3 -5 0 124.852 7.16898 0 -3 -5 0 137.944 7.54301 0 3 5 0 121.798 7.97938 0 3 5 0 124.167 7.41833 0 -4 -5 0 931.209 48.6251 0 -4 -5 0 947.547 48.5108 0 -4 -5 0 883.041 49.6537 0 4 5 0 905.836 48.5108 0 4 5 0 817.843 49.0823 0 -5 -5 0 188.967 10.7187 0 -5 -5 0 191.172 10.6161 0 -5 -5 0 186.556 11.9495 0 5 5 0 184.915 10.7187 0 -6 -5 0 605.091 33.1326 0 -6 -5 0 619.087 34.7235 0 6 5 0 613.859 33.3598 0 -7 -5 0 127.054 8.43905 0 -7 -5 0 113.935 8.47905 0 -7 -5 0 128.654 8.27907 0 -7 -5 0 118.055 6.87923 0 7 5 0 122.134 7.23919 0 -8 -5 0 286.145 17.4979 0 -8 -5 0 328.361 17.4628 0 8 5 0 259.744 16.0602 0 -9 -5 0 20.8537 2.84828 0 -9 -5 0 18.3117 2.8789 0 9 5 0 15.3409 1.59259 0 -10 -5 0 11.3645 1.87621 0 -10 -5 0 11.0428 1.66179 0 -8 6 0 33.9073 2.41523 0 -7 6 0 75.1021 4.82437 0 -7 6 0 75.8507 5.40662 0 -6 6 0 0.97612 0.91314 0 -6 6 0 0.37785 1.00761 0 5 -6 0 221.277 12.3956 0 -5 6 0 256.388 14.1102 0 -5 6 0 202.809 13.0386 0 4 -6 0 28.7573 2.0141 0 -4 6 0 23.8832 3.86706 0 -4 6 0 29.1601 2.77945 0 -4 6 0 35.2427 3.3434 0 -4 6 0 31.295 1.93353 0 3 -6 0 286.351 15.9199 0 -3 6 0 287.479 16.5964 0 -3 6 0 310.204 16.0101 0 -3 6 0 272.641 18.1749 0 2 -6 0 14.7245 1.24783 0 -2 6 0 14.0756 1.39758 0 -2 6 0 16.8707 2.04645 0 -2 6 0 13.5265 1.39758 0 1 -6 0 692.975 36.7219 0 1 -6 0 611.014 37.4814 0 -1 6 0 655.711 37.1017 0 -1 6 0 679.901 37.2102 0 -1 6 0 763.007 37.0474 0 0 -6 0 34.4678 2.30207 0 0 -6 0 35.849 2.93514 0 0 6 0 35.1008 2.64738 0 0 6 0 32.5686 2.82004 0 0 6 0 33.8347 2.87759 0 -1 -6 0 211.688 11.2392 0 -1 -6 0 186.08 10.7069 0 -1 -6 0 190.34 11.2984 0 1 6 0 187.264 11.4167 0 1 6 0 188.565 11.1209 0 -2 -6 0 37.1624 2.46614 0 -2 -6 0 35.166 2.75973 0 -2 -6 0 32.5825 2.87717 0 2 6 0 37.3973 3.22947 0 2 6 0 35.4009 2.9946 0 2 6 0 39.335 2.70102 0 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80.1985 5.2261 0 -5 -7 0 80.4642 5.40325 0 5 7 0 91.8465 5.35897 0 -6 -7 0 364.242 20.4892 0 -6 -7 0 355.327 20.5295 0 -6 -7 0 377.515 21.8608 0 6 7 0 396.067 20.6909 0 -7 -7 0 7.30304 0.98101 0 -7 -7 0 4.10569 1.48968 0 -7 -7 0 7.01237 1.88934 0 7 7 0 7.41204 1.16267 0 -8 -7 0 147.765 9.40665 0 -8 -7 0 144.817 8.07674 0 -8 -7 0 144.525 9.5364 0 8 7 0 144.33 8.46598 0 -9 -7 0 0.31686 0.86416 0 -9 -7 0 0.11522 1.0946 0 9 7 0 0.02881 0.40327 0 -10 -7 0 0.56024 0.68757 0 10 7 0 0.8149 0.38198 0 -6 8 0 7.07956 1.44213 0 -6 8 0 6.3716 1.15371 0 5 -8 0 9.70246 0.87938 0 -5 8 0 7.76783 1.28975 0 -5 8 0 11.3147 1.99326 0 4 -8 0 7.04713 0.84827 0 -4 8 0 7.145 1.30502 0 -4 8 0 11.0927 2.08804 0 -4 8 0 8.2869 0.71776 0 3 -8 0 10.19 1.0442 0 -3 8 0 7.95755 1.44028 0 -3 8 0 9.36182 1.0442 0 2 -8 0 8.16827 0.98176 0 -2 8 0 8.63952 1.13885 0 -2 8 0 10.4067 1.64936 0 -2 8 0 7.30432 0.98176 0 1 -8 0 82.4785 4.85466 0 -1 8 0 82.2252 5.2768 0 -1 8 0 78.2571 5.31902 0 -1 8 0 82.3941 5.15016 0 0 -8 0 213.825 13.4016 0 0 -8 0 235.107 12.7338 0 0 8 0 227.85 13.0454 0 0 8 0 256.652 13.4016 0 0 8 0 210.397 13.0454 0 -1 -8 0 324.043 18.1827 0 -1 -8 0 336.395 18.9174 0 1 8 0 305.539 18.5501 0 1 8 0 361.69 19.0551 0 -2 -8 0 314.81 17.7786 0 -2 -8 0 333.558 17.4092 0 -2 -8 0 309.731 18.0095 0 2 8 0 302.527 17.4553 0 2 8 0 296.297 18.148 0 2 8 0 343.302 17.9633 0 -3 -8 0 533.076 29.5987 0 -3 -8 0 564.716 28.965 0 -3 -8 0 572.18 29.3724 0 3 8 0 499.268 29.8251 0 3 8 0 553.807 29.1914 0 3 8 0 477.812 29.4629 0 -4 -8 0 35.4823 2.64309 0 -4 -8 0 33.7925 2.90306 0 4 8 0 31.2794 2.55643 0 4 8 0 33.6192 3.29302 0 -5 -8 0 156.171 9.22093 0 -5 -8 0 174.978 9.5459 0 5 8 0 143.822 9.18031 0 -6 -8 0 8.16865 1.12413 0 -6 -8 0 7.79394 2.02343 0 -6 -8 0 9.55507 1.31148 0 6 8 0 10.0797 1.34895 0 -7 -8 0 19.9605 1.56981 0 -7 -8 0 17.9811 2.69598 0 7 8 0 15.4251 1.67219 0 -8 -8 0 8.32976 0.8299 0 -8 -8 0 5.93227 1.50612 0 -8 -8 0 9.65146 1.99791 0 8 8 0 7.22323 1.01433 0 -9 -8 0 15.2152 1.81953 0 9 8 0 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27.9649 1.76255 0 -5 2 -14 10.4361 1.01154 0 5 -2 14 10.9295 0.78949 0 3 1 -14 8.96946 0.74941 0 -3 -1 14 7.98586 0.65573 0 2 1 -14 44.6165 2.54837 0 -2 -1 14 38.5953 2.52339 0 1 1 -14 39.2034 2.83797 0 -1 -1 14 41.119 2.60147 0 -1 -1 14 40.9614 2.73286 0 0 1 -14 67.9406 4.96987 0 0 -1 14 80.0529 4.3724 0 0 -1 14 65.7435 4.42671 0 -1 1 -14 65.1025 4.6723 0 -1 1 -14 69.1638 4.39583 0 1 -1 14 62.7802 4.14701 0 1 -1 14 70.9885 4.39583 0 -2 1 -14 16.6013 1.5523 0 -2 1 -14 15.9361 1.85722 0 2 -1 14 14.4115 1.74634 0 -3 1 -14 37.3053 2.51823 0 -3 1 -14 33.2817 2.7372 0 3 -1 14 33.6922 2.10765 0 -4 1 -14 38.9745 2.98186 0 -4 1 -14 44.3765 2.82212 0 4 -1 14 41.7141 2.47601 0 5 -1 14 18.9578 1.24873 0 -6 1 -14 94.3235 5.24472 0 -6 1 -14 86.0134 5.02918 0 6 -1 14 87.4982 4.93339 0 2 0 -14 21.376 1.44516 0 -2 0 14 18.7099 1.39533 0 -2 0 14 21.4507 1.84383 0 1 0 -14 22.3241 1.55156 0 -1 0 14 21.9296 1.60416 0 -1 0 14 22.403 1.97233 0 -1 0 14 21.8244 1.76194 0 0 0 -14 12.5703 1.93599 0 0 0 14 15.4579 1.30884 0 0 0 14 15.158 1.52698 0 0 0 14 19.2481 1.99052 0 -1 0 -14 48.4828 3.36995 0 -1 0 -14 47.1738 3.64846 0 1 0 14 42.9126 3.20285 0 1 0 14 49.5689 3.09144 0 -2 0 -14 14.4825 1.79315 0 -2 0 -14 15.9674 1.56901 0 2 0 14 14.3704 1.62504 0 -3 0 -14 95.1356 5.55099 0 -3 0 -14 93.6646 5.80078 0 3 0 14 85.1161 5.0514 0 -4 0 -14 15.3797 1.67907 0 -4 0 -14 16.9234 1.4895 0 4 0 14 16.4089 1.13744 0 -5 0 -14 78.2596 4.63305 0 5 0 14 77.1664 4.3988 0 -6 0 -14 18.3629 1.37495 0 6 0 14 18.3874 1.20308 0 2 -1 -14 18.3931 1.27884 0 -2 1 14 17.4094 1.25424 0 -2 1 14 18.2947 1.62314 0 1 -1 -14 9.12261 0.86013 0 -1 1 14 10.7386 1.40749 0 -1 1 14 8.3146 0.99045 0 -1 1 14 7.40234 0.83407 0 0 1 14 72.9042 4.04014 0 0 1 14 59.729 4.09437 0 -1 -1 -14 0.30564 0.83355 0 1 1 14 2.11167 0.63906 0 1 1 14 0.94469 0.52792 0 -2 -1 -14 149.771 8.02069 0 -2 -1 -14 134.29 8.27308 0 2 1 14 127.84 7.9646 0 2 1 14 130.476 7.82438 0 -3 -1 -14 3.14961 0.72469 0 -3 -1 -14 4.09728 0.94767 0 3 1 14 3.81855 0.47384 0 3 1 14 3.53982 1.05916 0 -4 -1 -14 110.027 6.9575 0 -4 -1 -14 120.804 6.82108 0 4 1 14 116.821 6.4391 0 -5 -1 -14 6.52487 0.89454 0 5 1 14 7.84036 0.65775 0 -6 -1 -14 141.858 7.92617 0 6 1 14 141.534 7.77662 0 2 -2 -14 0.09613 0.28839 0 -2 2 14 0.12016 0.24033 0 -2 2 14-0.16823 0.52872 0 1 -2 -14 66.6361 3.96385 0 -1 2 14 65.383 3.98942 0 -1 2 14 72.9271 4.39859 0 0 -2 -14 0.02671 0.40058 0 0 2 14 0.02671 0.29376 0 0 2 14 0.42729 0.50741 0 -1 -2 -14 58.0288 4.44728 0 1 2 14 64.6448 4.0904 0 1 2 14 67.1155 3.92569 0 -2 -2 -14 12.4532 1.47326 0 -2 -2 -14 14.9522 1.86242 0 2 2 14 15.2857 1.36207 0 2 2 14 12.064 1.44546 0 -3 -2 -14 168.907 8.92575 0 -3 -2 -14 160.924 9.20295 0 3 2 14 133.346 8.95347 0 -4 -2 -14 0.68062 0.49005 0 -4 -2 -14 1.36124 0.70784 0 4 2 14 0.16335 0.24502 0 -5 -2 -14 154.117 8.79705 0 -5 -2 -14 154.354 8.77071 0 5 2 14 154.538 8.48098 0 -6 -2 -14 3.43082 0.57598 0 6 2 14 3.1804 0.40068 0 7 2 14 69.2523 3.87121 0 1 -3 -14 25.4742 1.63726 0 -1 3 14 23.192 1.61245 0 0 -3 -14 65.9476 3.98546 0 0 3 14 78.0602 4.1157 0 0 3 14 63.8663 4.1678 0 1 3 14 29.6569 1.96119 0 1 3 14 24.7136 2.04178 0 -2 -3 -14 223.453 11.6527 0 2 3 14 191.936 11.4071 0 2 3 14 198.868 11.5708 0 -3 -3 -14 11.5765 1.33785 0 3 3 14 13.2966 1.50167 0 -4 -3 -14 150.95 8.52898 0 -4 -3 -14 150.331 8.25993 0 4 3 14 132.468 7.85635 0 -5 -3 -14 4.41318 0.70506 0 -5 -3 -14 6.21501 1.01843 0 5 3 14 4.88322 0.52227 0 -6 -3 -14 69.0642 4.00885 0 6 3 14 65.7276 3.78475 0 -7 -3 -14 0.44495 0.2576 0 7 3 14 0.11709 0.16393 0 1 -4 -14 8.10423 0.76275 0 -1 4 14 7.74669 0.69124 0 0 -4 -14 40.7113 2.81322 0 0 4 14 46.3629 2.71275 0 1 4 14 54.7539 3.33293 0 1 4 14 54.4935 3.48917 0 -2 -4 -14 55.75 3.90101 0 2 4 14 51.5571 3.50295 0 2 4 14 53.4943 3.34373 0 -3 -4 -14 105.979 5.86021 0 3 4 14 90.0527 5.91348 0 -4 -4 -14 45.0537 2.97584 0 -5 -4 -14 139.561 7.35676 0 -5 -4 -14 124.591 7.51056 0 5 4 14 122.002 7.02353 0 -6 -4 -14 3.9695 0.58807 0 6 4 14 3.74897 0.41655 0 0 5 14 62.2723 3.61839 0 1 5 14 60.3377 3.59064 0 2 5 14 55.0359 3.39696 0 2 5 14 55.9554 3.57575 0 -3 -5 -14 25.9627 2.2903 0 -3 -5 -14 25.551 1.95576 0 3 5 14 25.6025 2.1359 0 -4 -5 -14 78.5879 4.6938 0 -5 -5 -14 24.8216 1.76604 0 -6 -5 -14 37.3416 2.19684 0 6 5 14 31.231 1.93418 0 1 6 14 22.5426 1.51404 0 2 6 14 47.6459 2.91294 0 -3 -6 -14 18.8457 2.42964 0 3 6 14 21.1035 1.59522 0 -4 -6 -14 27.927 1.95311 0 -5 -6 -14 23.7352 1.67334 0 0 -3 15 45.9104 2.7977 0 -1 3 -15 11.2108 1.21391 0 -2 3 -15 48.3955 3.04135 0 0 -2 15 3.48674 0.52902 0 -1 2 -15 48.9133 3.20574 0 -2 2 -15-0.19606 0.44114 0 -3 2 -15 93.5327 5.4826 0 -4 2 -15 19.8361 1.33821 0 4 -2 15 14.178 1.33821 0 -1 -1 15 6.59384 0.63583 0 0 -1 15 105.494 6.0009 0 1 -1 15 0.47347 0.44855 0 -4 1 -15 72.3722 4.14423 0 4 -1 15 66.6137 3.87919 0 -1 0 15 43.2838 2.59212 0 0 0 15 8.15767 0.80842 0 1 0 15 91.0332 5.29935 0 -2 0 -15 4.00243 0.75996 0 -2 0 -15 4.91438 1.08927 0 -3 0 -15 116.382 7.64067 0 -3 0 -15 120.956 6.86152 0 -4 0 -15 0.34346 0.31893 0 5 0 15 39.6582 2.29006 0 -1 1 15 16.7097 1.16868 0 0 1 15 105.84 5.99014 0 1 1 15 14.8523 1.22747 0 -2 -1 -15 113.532 6.64318 0 -2 -1 -15 113.482 7.45456 0 -3 -1 -15 8.17985 1.00986 0 -3 -1 -15 6.18538 1.23708 0 -4 -1 -15 50.0211 3.14054 0 -5 -1 -15 8.8953 0.81083 0 5 1 15 7.48827 0.5962 0 0 2 15 30.933 2.0368 0 0 2 15 33.5449 2.32435 0 1 2 15 46.7783 2.89304 0 -2 -2 -15 25.9676 1.95906 0 2 2 15 24.5862 1.78325 0 -3 -2 -15 61.4312 3.81467 0 -4 -2 -15 26.0728 1.85019 0 -5 -2 -15 19.0245 1.31302 0 5 2 15 14.6079 1.14591 0 0 3 15 11.6775 0.98287 0 0 3 15 16.5427 1.3339 0 1 3 15 30.4906 1.98132 0 2 3 15 30.012 2.01902 0 -3 -3 -15 25.329 1.8764 0 -4 -3 -15 10.1816 0.99867 0 -5 -3 -15 34.5886 2.22557 0 1 4 15 0.37497 0.28123 0 2 4 15 36.1148 2.29483 0 -3 -4 -15 0.31263 0.45693 0 -4 -4 -15 21.9331 1.59574 0 0 0 0 0. 0. ; _shelx_hkl_checksum 23105 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 I1 I 0.74571(3) 0.29306(2) 0.12003(2) 0.05817(12) Uani 0.9847(10) 1 d . U P A 1 S1 S 0.66546(8) 0.19950(6) 0.59189(5) 0.05000(17) Uani 1 1 d . . . . . O1 O 0.4099(2) 0.15846(18) 0.90576(16) 0.0597(5) Uani 1 1 d . U . . . N1 N 0.6246(2) 0.29195(19) 0.76956(16) 0.0436(4) Uani 1 1 d . . . . . O3 O 0.2869(3) 0.2603(2) 1.05311(17) 0.0691(6) Uani 1 1 d . U . . . O2 O 0.6045(3) 0.1886(2) 0.36309(19) 0.0776(7) Uani 1 1 d . . . . . H2 H 0.622978 0.225725 0.308139 0.116 Uiso 1 1 calc R U . . . C1 C 0.2247(3) 0.5122(2) 0.45493(19) 0.0419(5) Uani 1 1 d . . . . . C4 C 0.0932(3) 0.6009(2) 0.43649(19) 0.0424(5) Uani 1 1 d . . . . . C6 C 0.0048(3) 0.6843(2) 0.5158(2) 0.0459(6) Uani 1 1 d . . . . . C8 C 0.4438(3) 0.4065(2) 0.6660(2) 0.0475(6) Uani 1 1 d . . . . . H8 H 0.394869 0.464316 0.718988 0.057 Uiso 1 1 calc R U . . . C10 C 0.3074(3) 0.4291(2) 0.3725(2) 0.0450(5) Uani 1 1 d . . . . . H10 H 0.395505 0.369918 0.382430 0.054 Uiso 1 1 calc R U . . . C12 C 0.3945(3) 0.4180(2) 0.5764(2) 0.0454(5) Uani 1 1 d . . . . . H12 H 0.449044 0.360926 0.523752 0.054 Uiso 1 1 calc R U . . . C14 C 0.2658(3) 0.5095(2) 0.5524(2) 0.0444(5) Uani 1 1 d . . . . . C16 C 0.1769(3) 0.5944(2) 0.6284(2) 0.0486(6) Uani 1 1 d . . . . . H16 H 0.204990 0.593361 0.693405 0.058 Uiso 1 1 calc R U . . . C18 C -0.0842(3) 0.6923(2) 0.3224(2) 0.0481(6) Uani 1 1 d . . . . . C20 C 0.2627(3) 0.4333(2) 0.2813(2) 0.0466(5) Uani 1 1 d . . . . . H20 H 0.319284 0.375957 0.229344 0.056 Uiso 1 1 calc R U . . . C22 C 0.5685(3) 0.3089(2) 0.68368(19) 0.0451(5) Uani 1 1 d . . . . . C24 C 0.0478(3) 0.6054(2) 0.3397(2) 0.0446(5) Uani 1 1 d . . . . . C26 C 0.0505(3) 0.6786(2) 0.6104(2) 0.0509(6) Uani 1 1 d . . . . . H26 H -0.007038 0.734287 0.663333 0.061 Uiso 1 1 calc R U . . . C28 C 0.1325(3) 0.5216(2) 0.2607(2) 0.0450(5) Uani 1 1 d . . . . . C30 C 0.7479(3) 0.1911(2) 0.7675(2) 0.0443(5) Uani 1 1 d . . . . . C32 C -0.1286(3) 0.7696(2) 0.4959(2) 0.0516(6) Uani 1 1 d . . . . . H32 H -0.188238 0.825050 0.548537 0.062 Uiso 1 1 calc R U . . . C2 C 0.5648(3) 0.3746(2) 0.86048(19) 0.0450(5) Uani 1 1 d . . . . . H2A H 0.549676 0.458100 0.835653 0.054 Uiso 1 1 calc R U . . . H2B H 0.641261 0.359840 0.904352 0.054 Uiso 1 1 calc R U . . . C17 C 0.8307(3) 0.1510(2) 0.8444(2) 0.0485(6) Uani 1 1 d . . . . . H17 H 0.805923 0.192299 0.908457 0.058 Uiso 1 1 calc R U . . . C9 C 0.9880(3) -0.0125(3) 0.7309(2) 0.0554(6) Uani 1 1 d . . . . . H9 H 1.070676 -0.082118 0.719813 0.067 Uiso 1 1 calc R U . . . C19 C 0.0859(3) 0.5283(3) 0.1665(2) 0.0536(6) Uani 1 1 d . . . . . H19 H 0.142558 0.473082 0.113012 0.064 Uiso 1 1 calc R U . . . C5 C -0.1714(3) 0.7731(2) 0.4044(2) 0.0535(6) Uani 1 1 d . . . . . H5 H -0.260988 0.830199 0.394181 0.064 Uiso 1 1 calc R U . . . C21 C 0.4180(3) 0.3623(2) 0.9262(2) 0.0485(6) Uani 1 1 d . . . . . H21A H 0.385338 0.424215 0.981076 0.058 Uiso 1 1 calc R U . . . H21B H 0.341175 0.380526 0.882377 0.058 Uiso 1 1 calc R U . . . C11 C 0.9498(3) 0.0497(3) 0.8246(2) 0.0536(6) Uani 1 1 d . . . . . H11 H 1.007557 0.021203 0.876204 0.064 Uiso 1 1 calc R U . . . C23 C 0.4186(3) 0.2429(2) 0.9765(2) 0.0515(6) Uani 1 1 d . U . . . H23 H 0.509975 0.211706 1.007549 0.062 Uiso 1 1 calc R U . . . C3 C -0.1265(3) 0.6950(3) 0.2272(2) 0.0554(6) Uani 1 1 d . . . . . H3 H -0.214384 0.753039 0.215186 0.066 Uiso 1 1 calc R U . . . C25 C -0.0422(3) 0.6144(3) 0.1499(2) 0.0577(7) Uani 1 1 d . . . . . H25 H -0.071966 0.617895 0.085172 0.069 Uiso 1 1 calc R U . . . C13 C 0.9061(3) 0.0266(2) 0.6544(2) 0.0531(6) Uani 1 1 d . . . . . H13 H 0.931019 -0.015100 0.590534 0.064 Uiso 1 1 calc R U . . . C27 C 0.7858(3) 0.1293(2) 0.6740(2) 0.0463(5) Uani 1 1 d . . . . . C7 C 0.2447(5) 0.1511(3) 1.0613(3) 0.0759(8) Uani 1 1 d . U . . . H7A H 0.133904 0.166736 1.075289 0.091 Uiso 1 1 calc R U . . . H7B H 0.284596 0.100907 1.117195 0.091 Uiso 1 1 calc R U . . . C29 C 0.3126(5) 0.0912(3) 0.9592(3) 0.0751(8) Uani 1 1 d . U . . . H29A H 0.369952 0.007379 0.968123 0.090 Uiso 1 1 calc R U . . . H29B H 0.233301 0.090985 0.920362 0.090 Uiso 1 1 calc R U . . . C15 C 0.5758(6) 0.0786(4) 0.3402(4) 0.0968(14) Uani 1 1 d . . . . . H15A H 0.536790 0.042927 0.405737 0.116 Uiso 1 1 calc R U . . . H15B H 0.672346 0.022204 0.308395 0.116 Uiso 1 1 calc R U . . . C31 C 0.4685(6) 0.0898(4) 0.2709(4) 0.0980(14) Uani 1 1 d . . . . . H31A H 0.506287 0.124043 0.205200 0.147 Uiso 1 1 calc R U . . . H31B H 0.370780 0.142393 0.302862 0.147 Uiso 1 1 calc R U . . . H31C H 0.457216 0.010537 0.258644 0.147 Uiso 1 1 calc R U . . . I1A I 0.8210(19) 0.3288(14) 0.0948(13) 0.070(4) Uani 0.0153(10) 1 d . U P A 2 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 I1 0.07020(19) 0.05840(14) 0.04778(13) -0.00342(9) -0.01870(10) -0.01466(11) S1 0.0554(4) 0.0537(3) 0.0428(3) -0.0025(3) -0.0127(3) -0.0154(3) O1 0.0678(12) 0.0542(10) 0.0606(11) -0.0067(8) -0.0098(9) -0.0232(9) N1 0.0431(11) 0.0468(11) 0.0426(11) -0.0002(8) -0.0090(8) -0.0145(9) O3 0.0778(13) 0.0641(11) 0.0626(12) -0.0043(9) 0.0108(10) -0.0316(10) O2 0.0871(17) 0.0781(15) 0.0597(13) 0.0014(11) -0.0143(12) -0.0094(13) C1 0.0406(13) 0.0407(12) 0.0458(13) 0.0024(10) -0.0076(10) -0.0142(10) C4 0.0429(13) 0.0403(12) 0.0463(13) 0.0025(10) -0.0084(10) -0.0159(10) C6 0.0453(14) 0.0401(12) 0.0529(14) -0.0014(10) -0.0065(11) -0.0143(10) C8 0.0474(14) 0.0520(14) 0.0450(13) 0.0016(11) -0.0092(10) -0.0167(11) C10 0.0413(13) 0.0458(13) 0.0468(13) 0.0007(10) -0.0086(10) -0.0101(10) C12 0.0455(14) 0.0476(13) 0.0457(13) 0.0030(10) -0.0102(10) -0.0164(11) C14 0.0468(14) 0.0452(12) 0.0450(13) 0.0025(10) -0.0107(10) -0.0178(10) C16 0.0546(15) 0.0505(14) 0.0436(13) -0.0015(10) -0.0105(11) -0.0181(12) C18 0.0420(13) 0.0470(13) 0.0568(15) 0.0081(11) -0.0123(11) -0.0138(10) C20 0.0475(14) 0.0480(13) 0.0439(13) -0.0011(10) -0.0068(10) -0.0136(11) C22 0.0470(14) 0.0489(13) 0.0430(13) 0.0029(10) -0.0093(10) -0.0188(11) C24 0.0428(13) 0.0448(12) 0.0494(13) 0.0030(10) -0.0100(10) -0.0170(10) C26 0.0568(16) 0.0458(13) 0.0501(14) -0.0079(11) -0.0055(12) -0.0159(12) C28 0.0420(13) 0.0493(13) 0.0466(13) 0.0034(10) -0.0091(10) -0.0172(11) C30 0.0424(13) 0.0448(12) 0.0476(13) 0.0006(10) -0.0081(10) -0.0157(10) C32 0.0496(15) 0.0416(13) 0.0610(16) -0.0041(11) -0.0062(12) -0.0105(11) C2 0.0478(14) 0.0460(13) 0.0420(13) -0.0020(10) -0.0100(10) -0.0128(10) C17 0.0504(15) 0.0495(13) 0.0487(14) 0.0014(11) -0.0131(11) -0.0162(11) C9 0.0495(15) 0.0483(14) 0.0671(18) -0.0004(12) -0.0087(13) -0.0127(12) C19 0.0500(15) 0.0664(17) 0.0470(14) -0.0008(12) -0.0110(11) -0.0188(13) C5 0.0460(14) 0.0429(13) 0.0694(18) 0.0040(12) -0.0113(12) -0.0093(11) C21 0.0496(15) 0.0455(13) 0.0488(14) -0.0026(10) -0.0072(11) -0.0113(11) C11 0.0508(15) 0.0525(15) 0.0616(16) 0.0047(12) -0.0177(12) -0.0169(12) C23 0.0555(14) 0.0539(13) 0.0471(12) -0.0012(10) -0.0090(10) -0.0187(11) C3 0.0471(15) 0.0586(16) 0.0628(17) 0.0121(13) -0.0173(12) -0.0153(12) C25 0.0547(16) 0.0713(18) 0.0520(15) 0.0073(13) -0.0192(12) -0.0197(14) C13 0.0551(16) 0.0494(14) 0.0538(15) -0.0061(11) -0.0057(12) -0.0149(12) C27 0.0485(14) 0.0485(13) 0.0455(13) 0.0011(10) -0.0115(11) -0.0174(11) C7 0.0815(19) 0.0691(16) 0.0792(18) 0.0031(14) 0.0004(15) -0.0360(14) C29 0.0868(19) 0.0642(16) 0.0810(18) 0.0027(14) -0.0120(16) -0.0352(15) C15 0.099(3) 0.076(3) 0.095(3) 0.028(2) -0.011(2) -0.001(2) C31 0.107(3) 0.086(3) 0.098(3) -0.018(2) 0.013(3) -0.040(2) I1A 0.063(7) 0.072(7) 0.088(7) -0.012(6) -0.012(6) -0.040(6) 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' I I -0.3257 6.8362 '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_ _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 C22 S1 C27 91.02(13) . . ? C23 O1 C29 107.4(2) . . ? C22 N1 C30 114.7(2) . . ? C22 N1 C2 123.3(2) . . ? C30 N1 C2 122.0(2) . . ? C23 O3 C7 107.0(2) . . ? C15 O2 H2 109.5 . . ? C4 C1 C10 117.5(2) . . ? C14 C1 C4 119.0(2) . . ? C14 C1 C10 123.5(2) . . ? C6 C4 C1 120.2(2) . . ? C24 C4 C1 120.4(2) . . ? C24 C4 C6 119.4(2) . . ? C4 C6 C32 118.8(3) . . ? C26 C6 C4 118.7(2) . . ? C26 C6 C32 122.5(3) . . ? C12 C8 H8 119.0 . . ? C12 C8 C22 121.9(2) . . ? C22 C8 H8 119.0 . . ? C1 C10 H10 119.2 . . ? C20 C10 C1 121.7(2) . . ? C20 C10 H10 119.2 . . ? C8 C12 H12 116.9 . . ? C8 C12 C14 126.3(3) . . ? C14 C12 H12 116.9 . . ? C1 C14 C12 121.0(2) . . ? C16 C14 C1 119.2(2) . . ? C16 C14 C12 119.7(2) . . ? C14 C16 H16 119.3 . . ? C26 C16 C14 121.5(3) . . ? C26 C16 H16 119.3 . . ? C24 C18 C5 118.8(3) . . ? C3 C18 C24 119.3(3) . . ? C3 C18 C5 122.0(3) . . ? C10 C20 H20 119.0 . . ? C10 C20 C28 121.9(2) . . ? C28 C20 H20 119.0 . . ? N1 C22 S1 111.95(19) . . ? N1 C22 C8 125.5(2) . . ? C8 C22 S1 122.6(2) . . ? C18 C24 C4 120.2(2) . . ? C28 C24 C4 120.2(2) . . ? C28 C24 C18 119.6(2) . . ? C6 C26 H26 119.3 . . ? C16 C26 C6 121.5(2) . . ? C16 C26 H26 119.3 . . ? C24 C28 C20 118.3(2) . . ? C19 C28 C20 122.7(3) . . ? C19 C28 C24 119.0(2) . . ? C17 C30 N1 128.0(2) . . ? C17 C30 C27 120.3(2) . . ? C27 C30 N1 111.7(2) . . ? C6 C32 H32 119.2 . . ? C5 C32 C6 121.6(3) . . ? C5 C32 H32 119.2 . . ? N1 C2 H2A 108.6 . . ? N1 C2 H2B 108.6 . . ? N1 C2 C21 114.7(2) . . ? H2A C2 H2B 107.6 . . ? C21 C2 H2A 108.6 . . ? C21 C2 H2B 108.6 . . ? C30 C17 H17 121.0 . . ? C11 C17 C30 117.9(3) . . ? C11 C17 H17 121.0 . . ? C11 C9 H9 119.8 . . ? C13 C9 H9 119.8 . . ? C13 C9 C11 120.4(3) . . ? C28 C19 H19 119.5 . . ? C25 C19 C28 121.0(3) . . ? C25 C19 H19 119.5 . . ? C18 C5 H5 119.4 . . ? C32 C5 C18 121.2(3) . . ? C32 C5 H5 119.4 . . ? C2 C21 H21A 108.0 . . ? C2 C21 H21B 108.0 . . ? H21A C21 H21B 107.2 . . ? C23 C21 C2 117.2(2) . . ? C23 C21 H21A 108.0 . . ? C23 C21 H21B 108.0 . . ? C17 C11 C9 121.9(3) . . ? C17 C11 H11 119.0 . . ? C9 C11 H11 119.0 . . ? O1 C23 C21 111.4(2) . . ? O1 C23 H23 110.6 . . ? O3 C23 O1 106.2(2) . . ? O3 C23 C21 107.3(2) . . ? O3 C23 H23 110.6 . . ? C21 C23 H23 110.6 . . ? C18 C3 H3 119.5 . . ? C25 C3 C18 120.9(3) . . ? C25 C3 H3 119.5 . . ? C19 C25 H25 119.9 . . ? C3 C25 C19 120.2(3) . . ? C3 C25 H25 119.9 . . ? C9 C13 H13 121.1 . . ? C9 C13 C27 117.8(3) . . ? C27 C13 H13 121.1 . . ? C30 C27 S1 110.6(2) . . ? C30 C27 C13 121.6(3) . . ? C13 C27 S1 127.8(2) . . ? O3 C7 H7A 110.8 . . ? O3 C7 H7B 110.8 . . ? O3 C7 C29 104.7(3) . . ? H7A C7 H7B 108.9 . . ? C29 C7 H7A 110.8 . . ? C29 C7 H7B 110.8 . . ? O1 C29 C7 106.3(3) . . ? O1 C29 H29A 110.5 . . ? O1 C29 H29B 110.5 . . ? C7 C29 H29A 110.5 . . ? C7 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? O2 C15 H15A 108.5 . . ? O2 C15 H15B 108.5 . . ? O2 C15 C31 115.1(3) . . ? H15A C15 H15B 107.5 . . ? C31 C15 H15A 108.5 . . ? C31 C15 H15B 108.5 . . ? C15 C31 H31A 109.5 . . ? C15 C31 H31B 109.5 . . ? C15 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 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 C22 1.730(3) . ? S1 C27 1.743(3) . ? O1 C23 1.418(3) . ? O1 C29 1.424(4) . ? N1 C22 1.333(3) . ? N1 C30 1.403(3) . ? N1 C2 1.494(3) . ? O3 C23 1.409(4) . ? O3 C7 1.422(4) . ? O2 H2 0.8400 . ? O2 C15 1.434(6) . ? C1 C4 1.434(4) . ? C1 C10 1.442(4) . ? C1 C14 1.418(4) . ? C4 C6 1.427(4) . ? C4 C24 1.425(4) . ? C6 C26 1.399(4) . ? C6 C32 1.435(4) . ? C8 H8 0.9500 . ? C8 C12 1.348(4) . ? C8 C22 1.441(4) . ? C10 H10 0.9500 . ? C10 C20 1.352(4) . ? C12 H12 0.9500 . ? C12 C14 1.456(4) . ? C14 C16 1.411(4) . ? C16 H16 0.9500 . ? C16 C26 1.373(4) . ? C18 C24 1.423(4) . ? C18 C5 1.433(4) . ? C18 C3 1.395(4) . ? C20 H20 0.9500 . ? C20 C28 1.432(4) . ? C24 C28 1.420(4) . ? C26 H26 0.9500 . ? C28 C19 1.396(4) . ? C30 C17 1.393(4) . ? C30 C27 1.394(4) . ? C32 H32 0.9500 . ? C32 C5 1.348(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C21 1.517(4) . ? C17 H17 0.9500 . ? C17 C11 1.379(4) . ? C9 H9 0.9500 . ? C9 C11 1.399(4) . ? C9 C13 1.381(4) . ? C19 H19 0.9500 . ? C19 C25 1.390(4) . ? C5 H5 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C23 1.508(4) . ? C11 H11 0.9500 . ? C23 H23 1.0000 . ? C3 H3 0.9500 . ? C3 C25 1.383(5) . ? C25 H25 0.9500 . ? C13 H13 0.9500 . ? C13 C27 1.396(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C29 1.490(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C31 1.474(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 N1 C30 C17 C11 -179.1(2) . . . . ? N1 C30 C27 S1 -0.1(3) . . . . ? N1 C30 C27 C13 179.4(2) . . . . ? N1 C2 C21 C23 61.5(3) . . . . ? O3 C7 C29 O1 9.8(4) . . . . ? C1 C4 C6 C26 1.1(4) . . . . ? C1 C4 C6 C32 -178.1(2) . . . . ? C1 C4 C24 C18 178.9(2) . . . . ? C1 C4 C24 C28 0.1(3) . . . . ? C1 C10 C20 C28 1.2(4) . . . . ? C1 C14 C16 C26 0.8(4) . . . . ? C4 C1 C10 C20 -0.6(4) . . . . ? C4 C1 C14 C12 177.4(2) . . . . ? C4 C1 C14 C16 -0.3(3) . . . . ? C4 C6 C26 C16 -0.6(4) . . . . ? C4 C6 C32 C5 -0.4(4) . . . . ? C4 C24 C28 C20 0.4(4) . . . . ? C4 C24 C28 C19 -179.8(2) . . . . ? C6 C4 C24 C18 0.1(3) . . . . ? C6 C4 C24 C28 -178.7(2) . . . . ? C6 C32 C5 C18 -0.7(4) . . . . ? C8 C12 C14 C1 -179.9(2) . . . . ? C8 C12 C14 C16 -2.2(4) . . . . ? C10 C1 C4 C6 178.8(2) . . . . ? C10 C1 C4 C24 0.0(3) . . . . ? C10 C1 C14 C12 -1.9(4) . . . . ? C10 C1 C14 C16 -179.6(2) . . . . ? C10 C20 C28 C24 -1.0(4) . . . . ? C10 C20 C28 C19 179.1(2) . . . . ? C12 C8 C22 S1 0.3(4) . . . . ? C12 C8 C22 N1 179.3(2) . . . . ? C12 C14 C16 C26 -176.9(2) . . . . ? C14 C1 C4 C6 -0.6(3) . . . . ? C14 C1 C4 C24 -179.3(2) . . . . ? C14 C1 C10 C20 178.7(2) . . . . ? C14 C16 C26 C6 -0.3(4) . . . . ? C18 C24 C28 C20 -178.4(2) . . . . ? C18 C24 C28 C19 1.4(4) . . . . ? C18 C3 C25 C19 0.6(4) . . . . ? C20 C28 C19 C25 179.2(3) . . . . ? C22 S1 C27 C30 0.1(2) . . . . ? C22 S1 C27 C13 -179.3(3) . . . . ? C22 N1 C30 C17 179.3(2) . . . . ? C22 N1 C30 C27 0.1(3) . . . . ? C22 N1 C2 C21 76.2(3) . . . . ? C22 C8 C12 C14 176.9(2) . . . . ? C24 C4 C6 C26 179.8(2) . . . . ? C24 C4 C6 C32 0.6(3) . . . . ? C24 C18 C5 C32 1.5(4) . . . . ? C24 C18 C3 C25 0.2(4) . . . . ? C24 C28 C19 C25 -0.6(4) . . . . ? C26 C6 C32 C5 -179.5(3) . . . . ? C28 C19 C25 C3 -0.4(4) . . . . ? C30 N1 C22 S1 0.0(3) . . . . ? C30 N1 C22 C8 -179.1(2) . . . . ? C30 N1 C2 C21 -105.4(3) . . . . ? C30 C17 C11 C9 -0.1(4) . . . . ? C32 C6 C26 C16 178.5(3) . . . . ? C2 N1 C22 S1 178.53(17) . . . . ? C2 N1 C22 C8 -0.6(4) . . . . ? C2 N1 C30 C17 0.8(4) . . . . ? C2 N1 C30 C27 -178.5(2) . . . . ? C2 C21 C23 O1 -79.2(3) . . . . ? C2 C21 C23 O3 164.9(2) . . . . ? C17 C30 C27 S1 -179.4(2) . . . . ? C17 C30 C27 C13 0.1(4) . . . . ? C9 C13 C27 S1 179.2(2) . . . . ? C9 C13 C27 C30 -0.2(4) . . . . ? C5 C18 C24 C4 -1.2(4) . . . . ? C5 C18 C24 C28 177.7(2) . . . . ? C5 C18 C3 C25 -178.6(3) . . . . ? C11 C9 C13 C27 0.1(4) . . . . ? C23 O1 C29 C7 8.3(4) . . . . ? C23 O3 C7 C29 -24.4(4) . . . . ? C3 C18 C24 C4 180.0(2) . . . . ? C3 C18 C24 C28 -1.2(4) . . . . ? C3 C18 C5 C32 -179.7(3) . . . . ? C13 C9 C11 C17 0.0(4) . . . . ? C27 S1 C22 N1 -0.1(2) . . . . ? C27 S1 C22 C8 179.1(2) . . . . ? C27 C30 C17 C11 0.1(4) . . . . ? C7 O3 C23 O1 30.2(3) . . . . ? C7 O3 C23 C21 149.5(3) . . . . ? C29 O1 C23 O3 -23.6(3) . . . . ? C29 O1 C23 C21 -140.2(3) . . . . ?