#------------------------------------------------------------------------------ #$Date: 2020-05-30 06:33:03 +0300 (Sat, 30 May 2020) $ #$Revision: 252475 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/75/7157526.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_7157526 loop_ _publ_author_name 'you, yong' 'Quan, Bao-Xue' 'Wang, Zhen-Hua' 'Zhao, Jian-Qiang' 'Yuan, Weicheng' _publ_section_title ; Divergent synthesis of oxindole derivatives via controllable reaction of isatin-derived para-quinone methides with sulfur ylides ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D0OB00979B _journal_year 2020 _chemical_formula_moiety 'C31 H33 N O3' _chemical_formula_sum 'C31 H33 N O3' _chemical_formula_weight 467.58 _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 _audit_update_record ; 2020-04-29 deposited with the CCDC. 2020-05-28 downloaded from the CCDC. ; _cell_angle_alpha 83.6440(10) _cell_angle_beta 83.3400(10) _cell_angle_gamma 62.8550(10) _cell_formula_units_Z 2 _cell_length_a 9.4791(2) _cell_length_b 9.7988(2) _cell_length_c 15.5180(4) _cell_measurement_reflns_used 9927 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 72.2312 _cell_measurement_theta_min 2.8731 _cell_volume 1271.23(5) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_collection 'Bruker Instrument Service vV6.2.9' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 882)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON II' _diffrn_radiation_monochromator 'Helixos MX multilayer Optic' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_unetI/netI 0.0234 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 22434 _diffrn_reflns_theta_full 72.33 _diffrn_reflns_theta_max 72.33 _diffrn_reflns_theta_min 2.87 _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _exptl_absorpt_coefficient_mu 0.613 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 500 _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.260 _refine_diff_density_max 0.284 _refine_diff_density_min -0.211 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 325 _refine_ls_number_reflns 4956 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0389 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.5568P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0931 _refine_ls_wR_factor_ref 0.0940 _reflns_number_gt 4772 _reflns_number_total 4956 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob00979b2.cif _cod_data_source_block yy1 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 7157526 _shelx_res_file ; TITL yy1_0m_a.res in P-1 yy1_0m.res created by SHELXL-2017/1 at 16:18:36 on 15-Apr-2020 CELL 1.54178 9.4791 9.7988 15.5180 83.644 83.340 62.855 ZERR 2.00 0.0002 0.0002 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H N O UNIT 62 66 2 6 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.190 SIZE 0.260 0.290 0.360 ACTA EQIV $1 x-1, y+1, z HTAB O3 O1_$1 L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.038400 0.556800 FVAR 1.46612 O1 4 0.788800 0.261423 0.322820 11.00000 0.01794 0.01781 = 0.02609 -0.00322 -0.00038 -0.00356 O2 4 0.474903 0.313592 0.232952 11.00000 0.02607 0.02142 = 0.02555 -0.00373 0.00098 -0.01552 O3 4 -0.078458 1.057670 0.194562 11.00000 0.01339 0.01479 = 0.02851 -0.00301 -0.00328 -0.00272 AFIX 148 H3A 2 -0.107255 1.123514 0.234089 11.00000 -1.50000 AFIX 0 N1 3 0.772194 0.404116 0.435152 11.00000 0.01889 0.02101 = 0.02020 0.00318 -0.00564 -0.00990 C1 1 -0.218701 0.895125 0.328897 11.00000 0.01745 0.02460 = 0.02881 -0.00765 0.00713 -0.00903 AFIX 137 H4 2 -0.247506 1.001591 0.307136 11.00000 -1.50000 H1 2 -0.164966 0.872926 0.382671 11.00000 -1.50000 H3 2 -0.315037 0.880709 0.340600 11.00000 -1.50000 AFIX 0 C2 1 -0.106426 0.785298 0.260162 11.00000 0.01205 0.01725 = 0.02206 -0.00357 0.00138 -0.00682 C3 1 0.052606 0.794296 0.246428 11.00000 0.01256 0.01720 = 0.01385 -0.00399 0.00063 -0.00672 C4 1 0.195162 0.664970 0.263110 11.00000 0.01548 0.01479 = 0.01401 -0.00138 -0.00005 -0.00757 AFIX 43 H19 2 0.193626 0.569918 0.281641 11.00000 -1.20000 AFIX 0 C5 1 0.339606 0.671883 0.253249 11.00000 0.01313 0.01547 = 0.01485 -0.00299 -0.00077 -0.00530 C6 1 0.487920 0.532188 0.275120 11.00000 0.01218 0.01497 = 0.01671 -0.00094 0.00191 -0.00722 C7 1 0.572097 0.520022 0.341790 11.00000 0.01296 0.01502 = 0.01712 -0.00109 0.00167 -0.00704 C8 1 0.544523 0.625749 0.409010 11.00000 0.01799 0.02068 = 0.01472 -0.00102 0.00205 -0.01262 C9 1 0.668988 0.550557 0.464087 11.00000 0.02210 0.02232 = 0.01678 0.00143 -0.00003 -0.01451 C10 1 0.680743 0.617438 0.535168 11.00000 0.03805 0.03429 = 0.01735 0.00313 -0.00666 -0.02465 AFIX 43 H8 2 0.766394 0.564916 0.571497 11.00000 -1.20000 AFIX 0 C11 1 0.562579 0.764430 0.551534 11.00000 0.04889 0.03392 = 0.01625 -0.00570 0.00256 -0.02881 AFIX 43 H2 2 0.567300 0.813140 0.600010 11.00000 -1.20000 AFIX 0 C12 1 -0.184981 0.824147 0.173733 11.00000 0.01658 0.02624 = 0.02864 -0.00291 -0.00457 -0.01097 AFIX 137 H7 2 -0.111690 0.754776 0.130324 11.00000 -1.50000 H6 2 -0.210666 0.930619 0.153409 11.00000 -1.50000 H5 2 -0.282718 0.811837 0.182311 11.00000 -1.50000 AFIX 0 C13 1 0.060588 0.931596 0.214994 11.00000 0.01253 0.01443 = 0.01654 -0.00334 -0.00138 -0.00374 C14 1 0.206733 0.938917 0.197786 11.00000 0.01555 0.01410 = 0.01818 -0.00360 -0.00020 -0.00677 C15 1 0.343949 0.807931 0.220373 11.00000 0.01263 0.01707 = 0.01975 -0.00368 -0.00059 -0.00729 AFIX 43 H20 2 0.443017 0.811745 0.213107 11.00000 -1.20000 AFIX 0 C16 1 0.721670 0.378769 0.362403 11.00000 0.01398 0.01846 = 0.01765 0.00162 0.00000 -0.00864 C17 1 0.438204 0.840794 0.498239 11.00000 0.03540 0.02531 = 0.02251 -0.00866 0.00860 -0.01700 AFIX 43 H9 2 0.358903 0.941078 0.510713 11.00000 -1.20000 AFIX 0 C18 1 0.427601 0.772536 0.426375 11.00000 0.02170 0.02175 = 0.02053 -0.00449 0.00432 -0.01129 AFIX 43 H10 2 0.342008 0.825525 0.390050 11.00000 -1.20000 AFIX 0 C19 1 0.912776 0.293877 0.477074 11.00000 0.02518 0.03153 = 0.03033 0.00732 -0.01276 -0.01148 AFIX 137 H13 2 0.961310 0.198498 0.446810 11.00000 -1.50000 H11 2 0.883112 0.272349 0.537806 11.00000 -1.50000 H12 2 0.989024 0.336194 0.474971 11.00000 -1.50000 AFIX 0 C20 1 0.531473 0.403236 0.215799 11.00000 0.01266 0.01448 = 0.01924 -0.00008 -0.00475 -0.00450 C21 1 0.625843 0.407120 0.132386 11.00000 0.01261 0.01377 = 0.01801 -0.00063 -0.00302 -0.00293 C22 1 0.697853 0.504331 0.117975 11.00000 0.01948 0.01803 = 0.02037 -0.00408 -0.00036 -0.00798 AFIX 43 H14 2 0.693573 0.564473 0.163111 11.00000 -1.20000 AFIX 0 C23 1 0.776092 0.513752 0.037700 11.00000 0.02378 0.02162 = 0.02642 -0.00092 0.00273 -0.01117 AFIX 43 H18 2 0.825965 0.579586 0.028109 11.00000 -1.20000 AFIX 0 C24 1 0.781128 0.426875 -0.028269 11.00000 0.02242 0.02412 = 0.01839 -0.00079 0.00252 -0.00497 AFIX 43 H15 2 0.832003 0.435448 -0.083629 11.00000 -1.20000 AFIX 0 C25 1 0.712256 0.327451 -0.013880 11.00000 0.02331 0.02181 = 0.01971 -0.00634 -0.00264 -0.00455 AFIX 43 H16 2 0.717842 0.266653 -0.058982 11.00000 -1.20000 AFIX 0 C26 1 0.635228 0.316760 0.066338 11.00000 0.01761 0.01671 = 0.02313 -0.00384 -0.00370 -0.00574 AFIX 43 H17 2 0.588869 0.247991 0.076349 11.00000 -1.20000 AFIX 0 C27 1 0.217673 1.081204 0.150729 11.00000 0.01677 0.01443 = 0.03319 0.00026 0.00013 -0.00744 C28 1 0.146289 1.113555 0.062105 11.00000 0.03475 0.02827 = 0.03534 0.01289 -0.00763 -0.01712 AFIX 137 H22 2 0.152592 1.203893 0.031580 11.00000 -1.50000 H23 2 0.034823 1.132976 0.071191 11.00000 -1.50000 H21 2 0.206043 1.024374 0.027168 11.00000 -1.50000 AFIX 0 C29 1 0.132259 1.222524 0.204584 11.00000 0.02697 0.01791 = 0.05449 -0.00881 0.00724 -0.01216 AFIX 137 H24 2 0.172642 1.197346 0.262526 11.00000 -1.50000 H25 2 0.017790 1.253531 0.210063 11.00000 -1.50000 H26 2 0.151715 1.307081 0.175609 11.00000 -1.50000 AFIX 0 C30 1 0.390632 1.054243 0.132493 11.00000 0.02005 0.01936 = 0.04559 0.00249 0.00309 -0.01076 AFIX 137 H27 2 0.393330 1.144755 0.099984 11.00000 -1.50000 H29 2 0.449927 0.964169 0.098181 11.00000 -1.50000 H28 2 0.439171 1.036575 0.187659 11.00000 -1.50000 AFIX 0 C31 1 -0.082603 0.622975 0.292646 11.00000 0.01589 0.02104 = 0.03226 -0.00091 0.00146 -0.01054 AFIX 137 H30 2 -0.185450 0.620397 0.299002 11.00000 -1.50000 H31 2 -0.036214 0.595487 0.349027 11.00000 -1.50000 H32 2 -0.010936 0.549405 0.250647 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM yy1_0m_a.res in P-1 REM R1 = 0.0389 for 4772 Fo > 4sig(Fo) and 0.0403 for all 4956 data REM 325 parameters refined using 0 restraints END WGHT 0.0384 0.5568 REM Instructions for potential hydrogen bonds HTAB O3 O1_$1 REM Highest difference peak 0.284, deepest hole -0.211, 1-sigma level 0.038 Q1 1 0.6410 0.4571 0.3475 11.00000 0.05 0.28 Q2 1 -0.0324 0.7970 0.2551 11.00000 0.05 0.27 Q3 1 0.5860 0.5808 0.4498 11.00000 0.05 0.26 Q4 1 -0.0959 0.7159 0.2738 11.00000 0.05 0.26 Q5 1 -0.1549 0.8426 0.2948 11.00000 0.05 0.26 ; _shelx_res_checksum 2615 _shelx_hkl_file ; -4 0 0 108.89 5.80 -5 0 0 33.10 3.40 5 0 0 33.30 3.10 -6 0 0 261.17 11.50 -6 0 0 235.28 11.60 -6 0 0 233.98 11.80 -6 0 0 239.28 11.00 -6 0 0 226.38 13.00 -6 0 0 234.78 11.80 -6 0 0 241.98 12.20 -6 0 0 247.38 11.40 -6 0 0 238.68 12.20 -6 0 0 241.68 11.90 -6 0 0 244.38 12.70 -6 0 0 235.78 11.60 6 0 0 210.78 11.00 -7 0 0 1946.71 64.29 -7 0 0 2035.80 66.49 -7 0 0 2023.20 63.59 -7 0 0 2017.60 63.89 -7 0 0 2028.00 67.49 -7 0 0 2000.80 64.49 -7 0 0 1754.42 65.79 -7 0 0 1938.01 65.29 -7 0 0 2033.40 65.69 -7 0 0 2006.90 64.39 -7 0 0 1984.50 64.49 -7 0 0 2058.39 63.99 -8 0 0 739.93 27.00 -8 0 0 718.83 28.40 -8 0 0 737.43 27.70 -8 0 0 760.92 27.40 -8 0 0 731.53 30.00 -8 0 0 738.73 27.60 -8 0 0 729.83 28.50 -8 0 0 742.53 27.20 -8 0 0 735.03 29.30 -8 0 0 751.52 27.80 -8 0 0 731.63 27.70 -9 0 0 440.46 17.50 -9 0 0 446.26 17.30 -9 0 0 426.46 17.20 -9 0 0 435.46 17.00 -9 0 0 450.25 18.20 -9 0 0 441.36 18.40 -9 0 0 445.86 17.60 -9 0 0 420.06 17.50 -9 0 0 432.06 18.70 -9 0 0 401.66 17.20 -10 0 0 34.30 4.00 -9 1 0 6.20 1.60 -9 1 0 8.80 2.60 -9 1 0 7.10 1.90 -9 1 0 8.70 2.20 -9 1 0 10.20 2.20 -8 1 0 -0.70 1.40 -8 1 0 1.00 1.20 -8 1 0 5.90 1.80 -8 1 0 3.00 1.90 -8 1 0 1.60 1.60 -8 1 0 2.90 1.60 -8 1 0 1.40 1.80 -8 1 0 3.10 1.60 -8 1 0 1.50 1.30 -7 1 0 27.20 3.60 -7 1 0 25.30 3.50 -7 1 0 22.40 3.50 -7 1 0 35.80 5.90 -7 1 0 27.90 3.90 -7 1 0 29.30 4.00 -7 1 0 22.50 4.10 -7 1 0 22.50 3.90 -7 1 0 27.30 4.00 -7 1 0 23.80 3.90 -7 1 0 22.60 4.20 -6 1 0 2272.27 73.69 -6 1 0 2266.47 74.49 -6 1 0 2252.87 72.39 -6 1 0 2240.08 71.59 -6 1 0 2255.07 72.69 -6 1 0 2283.87 73.49 -6 1 0 2297.27 71.89 -6 1 0 2283.67 72.69 -6 1 0 2304.17 71.59 -6 1 0 2294.17 72.79 -6 1 0 2245.28 75.29 -6 1 0 2312.27 72.59 5 -1 0 24.70 2.30 -5 1 0 30.60 4.10 -5 1 0 28.10 3.40 -5 1 0 25.50 3.30 -5 1 0 22.10 3.70 -5 1 0 20.00 3.10 -5 1 0 22.60 2.90 -5 1 0 23.70 3.70 -5 1 0 23.10 3.80 -5 1 0 23.00 3.50 -5 1 0 27.90 3.20 -5 1 0 23.10 3.10 4 -1 0 2994.80 92.99 -4 1 0 3224.48 94.49 -3 1 0 6.30 0.50 -3 1 0 5.40 1.20 -3 1 0 5.00 0.50 1 -1 0 1720.83 50.89 -2 -1 0 644.74 20.30 -3 -1 0 1229.28 38.10 -4 -1 0 93.29 5.20 -5 -1 0 1968.80 61.89 -6 -1 0 315.67 16.50 -6 -1 0 310.97 13.90 -6 -1 0 298.17 14.40 -6 -1 0 318.47 15.30 -6 -1 0 274.67 16.40 -6 -1 0 296.77 17.40 -6 -1 0 267.37 17.10 6 1 0 296.87 12.20 -7 -1 0 14.40 3.10 -7 -1 0 16.60 3.70 -7 -1 0 12.40 2.60 -7 -1 0 9.10 2.60 -7 -1 0 13.90 3.10 -7 -1 0 14.20 3.10 -7 -1 0 8.80 2.10 -7 -1 0 12.80 2.70 -7 -1 0 9.40 2.60 -7 -1 0 10.40 3.00 -7 -1 0 12.10 3.00 7 1 0 11.20 2.30 -8 -1 0 148.49 9.20 -8 -1 0 143.69 8.50 -8 -1 0 146.59 9.20 -8 -1 0 139.99 9.90 -8 -1 0 144.89 9.10 -8 -1 0 144.59 8.90 -8 -1 0 154.98 9.10 -8 -1 0 153.18 8.90 -8 -1 0 142.39 10.30 -8 -1 0 150.88 9.60 -8 -1 0 137.99 9.40 -9 -1 0 174.68 9.70 -9 -1 0 162.68 9.90 -9 -1 0 173.48 11.00 -9 -1 0 180.68 9.90 -9 -1 0 177.08 9.20 -9 -1 0 172.28 9.50 -9 -1 0 177.38 10.60 -9 -1 0 169.48 9.40 -9 -1 0 168.58 9.40 -9 -1 0 174.68 10.10 -9 -1 0 175.58 9.80 -10 -1 0 43.60 3.80 -10 -1 0 41.80 3.70 -10 -1 0 41.70 3.80 -10 -1 0 47.10 3.80 -9 2 0 13.30 1.90 -9 2 0 12.80 2.00 -9 2 0 13.20 1.90 -8 2 0 1.20 1.10 -8 2 0 -0.40 1.10 -8 2 0 0.00 1.30 -8 2 0 4.60 1.60 -8 2 0 0.00 1.90 -7 2 0 634.94 25.30 -7 2 0 595.84 23.00 -7 2 0 602.04 24.80 -7 2 0 605.04 23.10 -7 2 0 613.24 23.80 -7 2 0 620.14 24.00 -6 2 0 83.99 7.90 -6 2 0 78.29 6.30 -6 2 0 70.39 5.90 -6 2 0 74.89 5.70 -6 2 0 78.89 6.10 -6 2 0 80.49 6.10 -6 2 0 78.89 5.80 -6 2 0 65.09 6.10 -6 2 0 67.99 6.60 -6 2 0 71.89 6.30 -6 2 0 74.89 7.10 -6 2 0 73.19 6.70 -5 2 0 200.08 10.50 -5 2 0 192.98 10.10 -5 2 0 208.08 10.10 -5 2 0 194.58 10.20 -5 2 0 200.58 10.00 -5 2 0 186.78 10.80 -5 2 0 202.38 11.60 -5 2 0 206.98 12.20 -5 2 0 193.78 10.20 -5 2 0 198.08 9.80 -5 2 0 195.38 10.40 -5 2 0 201.28 10.90 4 -2 0 81.39 3.90 -4 2 0 91.69 5.50 3 -2 0 2107.19 66.09 -3 2 0 2250.77 67.49 -3 2 0 2244.18 67.49 -3 2 0 2222.58 67.39 2 -2 0 178.08 6.90 -2 2 0 182.28 8.90 -2 2 0 184.68 8.70 -2 2 0 199.88 7.80 -1 2 0 3810.02 115.59 0 -2 0 445.26 14.20 0 2 0 441.06 14.30 -5 -2 0 1334.37 43.20 5 2 0 1308.87 41.70 -6 -2 0 966.50 34.00 -6 -2 0 957.40 34.00 -6 -2 0 965.50 35.20 -6 -2 0 936.31 33.80 -6 -2 0 983.90 33.00 -6 -2 0 1014.30 34.20 -6 -2 0 997.30 33.40 -6 -2 0 997.60 40.10 -6 -2 0 1021.00 34.70 -6 -2 0 999.60 33.40 6 2 0 982.60 32.60 -7 -2 0 44.10 4.90 -7 -2 0 51.39 5.70 -7 -2 0 44.00 4.90 -7 -2 0 54.29 4.90 -7 -2 0 45.30 4.50 -7 -2 0 46.50 5.00 -7 -2 0 47.80 4.60 -7 -2 0 47.60 4.70 -7 -2 0 49.90 5.40 -7 -2 0 55.99 5.30 -7 -2 0 45.10 5.00 -7 -2 0 46.60 4.40 7 2 0 42.10 4.10 -8 -2 0 9.70 2.60 -8 -2 0 13.90 3.50 -8 -2 0 8.90 2.50 -8 -2 0 5.30 1.90 -8 -2 0 16.70 3.10 -8 -2 0 17.60 3.50 -8 -2 0 10.50 2.70 -8 -2 0 9.80 2.70 -8 -2 0 6.50 2.30 -8 -2 0 10.30 3.20 -8 -2 0 9.90 2.60 -9 -2 0 275.97 12.50 -9 -2 0 248.78 14.10 -9 -2 0 261.87 12.80 -9 -2 0 267.57 13.20 -9 -2 0 268.17 12.90 -9 -2 0 272.77 13.00 -9 -2 0 280.37 13.20 -9 -2 0 250.37 13.50 -9 -2 0 250.67 12.30 -9 -2 0 258.47 13.00 -9 -2 0 264.87 13.70 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105.79 4.30 0 4 0 113.09 5.70 -1 -4 0 1148.99 36.40 1 4 0 1123.59 36.20 1 4 0 1155.68 41.60 3 4 0 12.00 3.30 3 4 0 9.70 1.60 4 4 0 1958.20 60.59 5 4 0 665.43 23.30 -6 -4 0 204.58 10.20 -6 -4 0 197.48 9.80 -6 -4 0 197.98 10.30 -6 -4 0 203.18 10.20 -6 -4 0 199.08 9.90 -6 -4 0 228.58 14.50 6 4 0 208.48 10.00 -7 -4 0 101.09 7.40 -7 -4 0 92.29 6.90 -7 -4 0 100.29 6.90 -7 -4 0 106.49 7.70 -7 -4 0 108.79 7.20 -7 -4 0 95.39 6.70 -7 -4 0 85.29 8.10 -7 -4 0 91.19 6.50 -7 -4 0 83.69 6.40 7 4 0 95.29 6.60 -8 -4 0 2.70 1.80 -8 -4 0 5.60 2.20 -8 -4 0 3.20 1.80 -8 -4 0 6.30 2.40 -8 -4 0 7.30 2.20 -8 -4 0 6.10 2.70 -8 -4 0 2.40 1.50 -8 -4 0 2.50 1.40 8 4 0 4.40 2.20 -9 -4 0 501.85 20.70 -9 -4 0 521.05 21.60 -9 -4 0 507.65 21.00 -9 -4 0 518.95 21.90 -9 -4 0 506.95 22.50 -9 -4 0 529.95 21.00 -10 -4 0 25.20 4.00 -10 -4 0 30.60 4.00 -10 -4 0 25.10 3.50 -10 -4 0 25.30 3.60 -10 -4 0 30.10 3.70 -11 -4 0 490.25 17.70 -11 -4 0 474.15 17.90 -11 -4 0 488.55 21.30 -7 5 0 2.20 0.90 -7 5 0 3.80 1.30 -7 5 0 2.10 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295.67 12.60 6 7 0 311.47 13.70 6 7 0 269.27 18.20 -7 -7 0 79.69 6.20 -7 -7 0 89.19 6.30 -7 -7 0 76.59 6.00 -7 -7 0 88.49 5.50 -7 -7 0 92.69 6.80 7 7 0 81.19 7.10 7 7 0 85.29 6.50 -8 -7 0 80.09 6.50 -8 -7 0 74.39 5.90 -8 -7 0 69.19 4.10 -8 -7 0 75.99 5.80 8 7 0 69.89 6.90 8 7 0 64.09 5.70 -9 -7 0 12.30 2.70 -9 -7 0 10.60 2.60 -9 -7 0 13.80 3.00 9 7 0 6.50 2.60 -10 -7 0 3.50 1.60 -10 -7 0 2.40 1.30 -10 -7 0 1.00 1.60 -11 -7 0 49.40 3.70 -11 -7 0 49.90 3.80 -11 -7 0 36.10 3.50 -4 8 0 435.96 15.10 -4 8 0 433.86 14.50 3 -8 0 76.29 4.50 -3 8 0 67.49 6.80 -3 8 0 89.69 5.30 2 -8 0 112.59 6.30 -2 8 0 112.29 7.10 -2 8 0 112.09 7.10 -2 8 0 106.49 5.70 1 -8 0 519.25 19.50 -1 8 0 505.65 21.10 -1 8 0 509.35 20.00 -1 8 0 520.95 21.80 0 -8 0 346.57 14.80 0 8 0 372.06 15.80 0 8 0 357.96 16.50 0 8 0 345.07 23.30 -1 -8 0 289.37 12.60 -1 -8 0 267.77 13.40 1 8 0 259.57 12.00 1 8 0 288.57 15.00 1 8 0 284.57 13.60 -2 -8 0 11.80 2.30 -2 -8 0 14.90 3.10 2 8 0 10.80 2.20 2 8 0 20.40 11.50 2 8 0 13.10 3.00 2 8 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196.58 9.60 1 9 0 206.28 24.30 1 9 0 203.58 10.60 -2 -9 0 118.49 6.90 -2 -9 0 110.29 7.90 2 9 0 108.29 15.70 2 9 0 107.49 6.80 2 9 0 113.59 7.80 -3 -9 0 483.65 18.00 -3 -9 0 463.15 19.50 3 9 0 475.65 19.90 3 9 0 448.56 21.60 3 9 0 481.15 19.10 -4 -9 0 618.64 23.40 -4 -9 0 610.74 21.30 4 9 0 511.55 26.70 4 9 0 615.94 23.20 4 9 0 616.24 24.00 -5 -9 0 13.50 2.30 -5 -9 0 20.20 3.20 5 9 0 19.90 3.20 5 9 0 12.60 3.20 5 9 0 11.30 2.60 5 9 0 12.50 2.90 -6 -9 0 105.49 7.40 -6 -9 0 124.79 7.50 6 9 0 125.79 8.00 -7 -9 0 125.39 8.10 -7 -9 0 129.79 7.30 -7 -9 0 118.39 7.20 7 9 0 127.19 7.90 -8 -9 0 395.06 17.00 -8 -9 0 388.36 14.70 -8 -9 0 395.36 16.10 8 9 0 408.46 16.40 -9 -9 0 67.09 4.90 -9 -9 0 62.89 5.10 9 9 0 59.79 4.50 -10 -9 0 160.18 7.90 -10 -9 0 176.18 8.90 10 9 0 179.18 8.80 1 -10 0 130.69 5.80 -1 10 0 134.79 5.70 -1 10 0 137.19 6.90 0 -10 0 134.39 6.40 0 10 0 135.09 7.00 0 10 0 127.99 6.30 0 10 0 132.99 7.00 -1 -10 0 94.39 5.40 -1 -10 0 89.29 6.90 1 10 0 93.69 9.30 1 10 0 89.09 6.00 1 10 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6 17 12.60 1.70 -5 -6 -17 0.90 0.90 -5 -6 -17 1.80 0.70 5 6 17 3.10 1.20 2 2 -18 20.90 1.80 -2 -2 18 19.00 2.60 1 2 -18 1.00 1.00 1 2 -18 1.80 1.10 -1 -2 18 2.00 1.10 -1 -2 18 1.60 0.90 0 2 -18 23.10 3.00 0 2 -18 21.40 2.30 0 -2 18 18.70 2.40 -1 2 -18 77.99 4.60 -1 2 -18 80.39 4.70 1 -2 18 78.89 3.90 -2 2 -18 410.46 14.50 -2 2 -18 378.36 14.00 2 -2 18 419.16 13.80 2 1 -18 216.98 8.70 -2 -1 18 204.18 8.70 -2 -1 18 195.68 8.10 1 1 -18 106.49 5.00 1 1 -18 101.49 5.50 -1 -1 18 82.89 5.60 -1 -1 18 106.49 5.20 0 1 -18 50.79 4.00 0 1 -18 53.59 3.00 0 -1 18 58.89 4.20 0 -1 18 51.39 2.90 0 -1 18 56.59 3.70 0 -1 18 53.39 3.40 -1 1 -18 4.60 1.40 -1 1 -18 4.60 1.50 1 -1 18 5.00 1.60 1 -1 18 4.70 1.10 1 -1 18 5.70 2.50 -2 1 -18 67.89 6.30 -2 1 -18 58.89 4.90 2 -1 18 57.09 3.80 -3 1 -18 2.40 1.10 -3 1 -18 1.90 1.40 3 -1 18 1.30 1.00 2 0 -18 267.07 10.10 -2 0 18 290.57 11.60 -2 0 18 269.47 10.70 1 0 -18 214.38 11.90 -1 0 18 198.28 9.10 -1 0 18 200.88 9.00 0 0 -18 20.70 2.10 0 0 -18 24.10 2.90 0 0 18 18.30 2.50 -1 0 -18 77.29 5.00 1 0 18 77.39 5.20 1 0 18 78.59 5.10 -2 0 -18 -0.50 0.70 -2 0 -18 -0.20 0.60 2 0 18 -0.60 0.70 2 0 18 1.80 1.50 -3 0 -18 5.50 1.80 3 0 18 9.00 2.60 -4 0 -18 12.00 1.40 -4 0 -18 16.30 1.90 4 0 18 14.30 2.20 2 -1 -18 318.27 11.90 -2 1 18 347.47 14.80 -2 1 18 320.57 12.00 1 -1 -18 175.98 8.20 1 -1 -18 176.18 8.10 -1 1 18 174.48 10.00 -1 1 18 187.18 8.30 0 -1 -18 -0.40 1.00 0 -1 -18 1.40 1.00 0 -1 -18 1.50 0.90 0 1 18 0.80 0.70 0 1 18 -0.90 1.10 -1 -1 -18 13.80 2.10 -1 -1 -18 14.60 2.30 -1 -1 -18 15.10 2.30 1 1 18 17.20 2.50 1 1 18 19.60 2.70 -2 -1 -18 129.89 7.00 -2 -1 -18 141.79 6.90 -2 -1 -18 107.89 6.30 2 1 18 132.79 6.30 2 1 18 121.09 7.80 -3 -1 -18 36.20 3.00 -3 -1 -18 46.20 4.30 -3 -1 -18 34.60 3.10 3 1 18 38.80 3.10 -4 -1 -18 4.00 1.10 4 1 18 5.10 1.20 1 -2 -18 12.80 1.60 -1 2 18 13.10 2.10 -1 2 18 14.10 2.50 0 -2 -18 51.19 3.90 0 -2 -18 64.89 4.90 0 2 18 56.99 4.60 0 2 18 52.49 3.90 -1 -2 -18 25.70 2.30 -1 -2 -18 28.70 3.00 -1 -2 -18 24.40 2.80 1 2 18 18.00 2.60 1 2 18 30.20 3.10 -2 -2 -18 3.20 1.10 -2 -2 -18 6.10 2.20 -2 -2 -18 6.70 1.50 2 2 18 5.00 1.50 2 2 18 3.50 1.20 -3 -2 -18 51.29 3.70 -3 -2 -18 52.19 3.80 3 2 18 54.79 3.70 3 2 18 47.70 4.20 -4 -2 -18 127.39 6.80 -4 -2 -18 128.79 6.50 -4 -2 -18 99.69 6.50 4 2 18 121.79 6.90 -5 -2 -18 1.00 1.10 -5 -2 -18 2.10 1.30 -5 -2 -18 0.90 0.60 5 2 18 1.40 0.80 1 -3 -18 75.19 3.80 -1 3 18 77.89 5.70 0 -3 -18 178.38 7.70 0 -3 -18 173.28 6.90 -1 -3 -18 50.29 3.70 -1 -3 -18 48.20 3.60 1 3 18 43.40 4.00 -2 -3 -18 103.79 6.10 -2 -3 -18 94.79 6.30 -2 -3 -18 99.19 5.50 2 3 18 107.39 5.80 2 3 18 99.09 5.10 -3 -3 -18 72.99 4.50 -3 -3 -18 65.39 5.60 -3 -3 -18 72.89 4.10 3 3 18 69.29 4.60 3 3 18 74.39 4.20 -4 -3 -18 8.30 1.80 -4 -3 -18 6.60 2.40 -4 -3 -18 7.80 1.70 -5 -3 -18 43.80 3.20 -5 -3 -18 42.50 2.50 5 3 18 55.09 4.80 0 -4 -18 18.80 1.60 0 4 18 16.90 2.40 0 4 18 18.20 2.10 -1 -4 -18 229.08 9.10 -1 -4 -18 209.58 7.70 1 4 18 213.28 9.70 1 4 18 225.68 9.10 -2 -4 -18 165.78 8.20 -2 -4 -18 135.49 6.60 2 4 18 133.09 7.10 2 4 18 129.99 5.70 -3 -4 -18 33.60 3.20 -3 -4 -18 38.00 3.80 3 4 18 30.90 2.50 -4 -4 -18 6.60 1.40 -4 -4 -18 9.80 1.60 4 4 18 9.10 1.60 -5 -4 -18 56.49 3.10 -5 -4 -18 56.59 3.70 5 4 18 64.09 3.80 -2 -5 -18 10.10 1.80 -2 -5 -18 10.60 1.70 2 5 18 11.30 1.90 -3 -5 -18 63.49 4.20 3 5 18 68.09 3.80 3 5 18 56.99 3.60 -4 -5 -18 1.80 1.10 -4 -5 -18 1.40 0.80 4 5 18 1.70 0.70 0 0 -19 2.90 1.00 0 0 19 4.40 1.20 0 0 19 0.60 1.70 -1 0 -19 267.67 10.50 -1 0 -19 269.17 10.40 1 0 19 266.27 10.90 0 -1 -19 -1.00 1.20 0 1 19 -0.50 0.70 0 1 19 3.10 1.40 -1 -1 -19 64.39 3.80 -1 -1 -19 64.69 3.80 1 1 19 60.19 3.90 1 1 19 62.89 3.90 -2 -1 -19 33.90 2.60 -2 -1 -19 36.30 2.60 2 1 19 32.60 2.60 2 1 19 32.10 2.10 -1 -2 -19 117.39 5.70 -1 -2 -19 125.19 5.50 1 2 19 118.79 6.10 1 2 19 127.29 5.90 -2 -2 -19 11.60 1.50 -2 -2 -19 9.10 1.60 2 2 19 7.30 1.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 99614 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.78880(9) 0.26142(9) 0.32282(5) 0.02230(19) Uani d . . . 1 . . O O2 0.47490(10) 0.31359(9) 0.23295(5) 0.02254(19) Uani d . . . 1 . . O O3 -0.07846(9) 1.05767(9) 0.19456(6) 0.02001(18) Uani d . . . 1 . . H H3A -0.1073(12) 1.1235(15) 0.2341(10) 0.03 Uiso calc U . R 1 . . N N1 0.77219(11) 0.40412(11) 0.43515(6) 0.0197(2) Uani d . . . 1 . . C C1 -0.21870(14) 0.89513(14) 0.32890(8) 0.0241(3) Uani d . . . 1 . . H H4 -0.247506 1.001591 0.307136 0.036 Uiso calc U . R 1 . . H H1 -0.164966 0.872926 0.382671 0.036 Uiso calc U . R 1 . . H H3 -0.315037 0.880709 0.3406 0.036 Uiso calc U . R 1 . . C C2 -0.10643(12) 0.78530(12) 0.26016(7) 0.0171(2) Uani d . . . 1 . . C C3 0.05261(12) 0.79430(12) 0.24643(7) 0.0144(2) Uani d . . . 1 . . C C4 0.19516(12) 0.66497(12) 0.26311(7) 0.0145(2) Uani d . . . 1 . . H H19 0.193626 0.569918 0.281641 0.017 Uiso calc U . R 1 . . C C5 0.33961(12) 0.67188(12) 0.25325(7) 0.0148(2) Uani d . . . 1 . . C C6 0.48792(12) 0.53219(12) 0.27512(7) 0.0145(2) Uani d . . . 1 . . C C7 0.57210(12) 0.52002(12) 0.34179(7) 0.0150(2) Uani d . . . 1 . . C C8 0.54452(13) 0.62575(13) 0.40901(7) 0.0166(2) Uani d . . . 1 . . C C9 0.66899(14) 0.55056(13) 0.46409(7) 0.0190(2) Uani d . . . 1 . . C C10 0.68074(16) 0.61744(15) 0.53517(8) 0.0266(3) Uani d . . . 1 . . H H8 0.766394 0.564916 0.571497 0.032 Uiso calc U . R 1 . . C C11 0.56258(18) 0.76443(15) 0.55153(8) 0.0292(3) Uani d . . . 1 . . H H2 0.5673 0.81314 0.60001 0.035 Uiso calc U . R 1 . . C C12 -0.18498(14) 0.82415(14) 0.17373(8) 0.0229(2) Uani d . . . 1 . . H H7 -0.11169 0.754776 0.130324 0.034 Uiso calc U . R 1 . . H H6 -0.210666 0.930619 0.153409 0.034 Uiso calc U . R 1 . . H H5 -0.282718 0.811837 0.182311 0.034 Uiso calc U . R 1 . . C C13 0.06059(12) 0.93160(12) 0.21499(7) 0.0152(2) Uani d . . . 1 . . C C14 0.20673(13) 0.93892(12) 0.19779(7) 0.0158(2) Uani d . . . 1 . . C C15 0.34395(12) 0.80793(12) 0.22037(7) 0.0161(2) Uani d . . . 1 . . H H20 0.443017 0.811745 0.213107 0.019 Uiso calc U . R 1 . . C C16 0.72167(12) 0.37877(12) 0.36240(7) 0.0165(2) Uani d . . . 1 . . C C17 0.43820(16) 0.84079(15) 0.49824(8) 0.0268(3) Uani d . . . 1 . . H H9 0.358903 0.941078 0.510713 0.032 Uiso calc U . R 1 . . C C18 0.42760(14) 0.77254(13) 0.42638(7) 0.0210(2) Uani d . . . 1 . . H H10 0.342008 0.825525 0.39005 0.025 Uiso calc U . R 1 . . C C19 0.91278(15) 0.29388(15) 0.47707(9) 0.0293(3) Uani d . . . 1 . . H H13 0.96131 0.198498 0.44681 0.044 Uiso calc U . R 1 . . H H11 0.883112 0.272349 0.537806 0.044 Uiso calc U . R 1 . . H H12 0.989024 0.336194 0.474971 0.044 Uiso calc U . R 1 . . C C20 0.53147(12) 0.40324(12) 0.21580(7) 0.0159(2) Uani d . . . 1 . . C C21 0.62584(12) 0.40712(12) 0.13239(7) 0.0158(2) Uani d . . . 1 . . C C22 0.69785(13) 0.50433(13) 0.11798(7) 0.0193(2) Uani d . . . 1 . . H H14 0.693573 0.564473 0.163111 0.023 Uiso calc U . R 1 . . C C23 0.77609(14) 0.51375(14) 0.03770(8) 0.0240(3) Uani d . . . 1 . . H H18 0.825965 0.579586 0.028109 0.029 Uiso calc U . R 1 . . C C24 0.78113(14) 0.42688(14) -0.02827(8) 0.0242(3) Uani d . . . 1 . . H H15 0.832003 0.435448 -0.083629 0.029 Uiso calc U . R 1 . . C C25 0.71226(14) 0.32745(14) -0.01388(8) 0.0233(3) Uani d . . . 1 . . H H16 0.717842 0.266653 -0.058982 0.028 Uiso calc U . R 1 . . C C26 0.63523(13) 0.31676(13) 0.06634(7) 0.0195(2) Uani d . . . 1 . . H H17 0.588869 0.247991 0.076349 0.023 Uiso calc U . R 1 . . C C27 0.21767(13) 1.08120(13) 0.15073(8) 0.0216(2) Uani d . . . 1 . . C C28 0.14629(17) 1.11355(16) 0.06211(9) 0.0325(3) Uani d . . . 1 . . H H22 0.152592 1.203893 0.03158 0.049 Uiso calc U . R 1 . . H H23 0.034823 1.132976 0.071191 0.049 Uiso calc U . R 1 . . H H21 0.206043 1.024374 0.027168 0.049 Uiso calc U . R 1 . . C C29 0.13226(16) 1.22252(14) 0.20458(10) 0.0327(3) Uani d . . . 1 . . H H24 0.172642 1.197346 0.262526 0.049 Uiso calc U . R 1 . . H H25 0.01779 1.253531 0.210063 0.049 Uiso calc U . R 1 . . H H26 0.151715 1.307081 0.175609 0.049 Uiso calc U . R 1 . . C C30 0.39063(15) 1.05424(14) 0.13249(9) 0.0285(3) Uani d . . . 1 . . H H27 0.39333 1.144755 0.099984 0.043 Uiso calc U . R 1 . . H H29 0.449927 0.964169 0.098181 0.043 Uiso calc U . R 1 . . H H28 0.439171 1.036575 0.187659 0.043 Uiso calc U . R 1 . . C C31 -0.08260(14) 0.62297(13) 0.29265(8) 0.0226(2) Uani d . . . 1 . . H H30 -0.18545 0.620397 0.299002 0.034 Uiso calc U . R 1 . . H H31 -0.036214 0.595487 0.349027 0.034 Uiso calc U . R 1 . . H H32 -0.010936 0.549405 0.250647 0.034 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0179(4) 0.0178(4) 0.0261(4) -0.0036(3) -0.0004(3) -0.0032(3) O2 0.0261(4) 0.0214(4) 0.0256(4) -0.0155(4) 0.0010(3) -0.0037(3) O3 0.0134(4) 0.0148(4) 0.0285(4) -0.0027(3) -0.0033(3) -0.0030(3) N1 0.0189(5) 0.0210(5) 0.0202(5) -0.0099(4) -0.0056(4) 0.0032(4) C1 0.0174(5) 0.0246(6) 0.0288(6) -0.0090(5) 0.0071(5) -0.0077(5) C2 0.0121(5) 0.0172(5) 0.0221(5) -0.0068(4) 0.0014(4) -0.0036(4) C3 0.0126(5) 0.0172(5) 0.0139(5) -0.0067(4) 0.0006(4) -0.0040(4) C4 0.0155(5) 0.0148(5) 0.0140(5) -0.0076(4) 0.0000(4) -0.0014(4) C5 0.0131(5) 0.0155(5) 0.0149(5) -0.0053(4) -0.0008(4) -0.0030(4) C6 0.0122(5) 0.0150(5) 0.0167(5) -0.0072(4) 0.0019(4) -0.0009(4) C7 0.0130(5) 0.0150(5) 0.0171(5) -0.0070(4) 0.0017(4) -0.0011(4) C8 0.0180(5) 0.0207(5) 0.0147(5) -0.0126(4) 0.0021(4) -0.0010(4) C9 0.0221(6) 0.0223(6) 0.0168(5) -0.0145(5) 0.0000(4) 0.0014(4) C10 0.0380(7) 0.0343(7) 0.0173(6) -0.0247(6) -0.0067(5) 0.0031(5) C11 0.0489(8) 0.0339(7) 0.0163(6) -0.0288(6) 0.0026(5) -0.0057(5) C12 0.0166(5) 0.0262(6) 0.0286(6) -0.0110(5) -0.0046(5) -0.0029(5) C13 0.0125(5) 0.0144(5) 0.0165(5) -0.0037(4) -0.0014(4) -0.0033(4) C14 0.0156(5) 0.0141(5) 0.0182(5) -0.0068(4) -0.0002(4) -0.0036(4) C15 0.0126(5) 0.0171(5) 0.0197(5) -0.0073(4) -0.0006(4) -0.0037(4) C16 0.0140(5) 0.0185(5) 0.0176(5) -0.0086(4) 0.0000(4) 0.0016(4) C17 0.0354(7) 0.0253(6) 0.0225(6) -0.0170(5) 0.0086(5) -0.0087(5) C18 0.0217(6) 0.0218(6) 0.0205(6) -0.0113(5) 0.0043(4) -0.0045(4) C19 0.0252(6) 0.0315(7) 0.0303(7) -0.0115(5) -0.0128(5) 0.0073(5) C20 0.0127(5) 0.0145(5) 0.0192(5) -0.0045(4) -0.0048(4) -0.0001(4) C21 0.0126(5) 0.0138(5) 0.0180(5) -0.0029(4) -0.0030(4) -0.0006(4) C22 0.0195(5) 0.0180(5) 0.0204(5) -0.0080(4) -0.0004(4) -0.0041(4) C23 0.0238(6) 0.0216(6) 0.0264(6) -0.0112(5) 0.0027(5) -0.0009(5) C24 0.0224(6) 0.0241(6) 0.0184(5) -0.0050(5) 0.0025(4) -0.0008(4) C25 0.0233(6) 0.0218(6) 0.0197(6) -0.0045(5) -0.0026(4) -0.0063(4) C26 0.0176(5) 0.0167(5) 0.0231(6) -0.0057(4) -0.0037(4) -0.0038(4) C27 0.0168(5) 0.0144(5) 0.0332(6) -0.0074(4) 0.0001(5) 0.0003(5) C28 0.0348(7) 0.0283(7) 0.0353(7) -0.0171(6) -0.0076(6) 0.0129(5) C29 0.0270(6) 0.0179(6) 0.0545(9) -0.0122(5) 0.0072(6) -0.0088(6) C30 0.0200(6) 0.0194(6) 0.0456(8) -0.0108(5) 0.0031(5) 0.0025(5) C31 0.0159(5) 0.0210(6) 0.0323(6) -0.0105(5) 0.0015(5) -0.0009(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C13 O3 H3A . . 109.5 ? C16 N1 C9 . . 110.95(9) ? C16 N1 C19 . . 124.27(10) ? C9 N1 C19 . . 124.78(10) ? C2 C1 H4 . . 109.5 ? C2 C1 H1 . . 109.5 ? H4 C1 H1 . . 109.5 ? C2 C1 H3 . . 109.5 ? H4 C1 H3 . . 109.5 ? H1 C1 H3 . . 109.5 ? C31 C2 C12 . . 107.06(9) ? C31 C2 C3 . . 111.54(9) ? C12 C2 C3 . . 110.03(9) ? C31 C2 C1 . . 107.04(9) ? C12 C2 C1 . . 110.28(9) ? C3 C2 C1 . . 110.79(9) ? C4 C3 C13 . . 117.55(9) ? C4 C3 C2 . . 120.75(9) ? C13 C3 C2 . . 121.69(9) ? C5 C4 C3 . . 121.55(10) ? C5 C4 H19 . . 119.2 ? C3 C4 H19 . . 119.2 ? C15 C5 C4 . . 119.42(10) ? C15 C5 C6 . . 120.95(9) ? C4 C5 C6 . . 119.59(9) ? C7 C6 C5 . . 123.43(10) ? C7 C6 C20 . . 123.45(9) ? C5 C6 C20 . . 113.10(9) ? C6 C7 C8 . . 131.61(10) ? C6 C7 C16 . . 122.62(10) ? C8 C7 C16 . . 105.73(9) ? C18 C8 C9 . . 119.14(10) ? C18 C8 C7 . . 134.07(10) ? C9 C8 C7 . . 106.79(10) ? C10 C9 C8 . . 122.44(11) ? C10 C9 N1 . . 127.92(11) ? C8 C9 N1 . . 109.64(10) ? C9 C10 C11 . . 117.60(12) ? C9 C10 H8 . . 121.2 ? C11 C10 H8 . . 121.2 ? C17 C11 C10 . . 121.01(11) ? C17 C11 H2 . . 119.5 ? C10 C11 H2 . . 119.5 ? C2 C12 H7 . . 109.5 ? C2 C12 H6 . . 109.5 ? H7 C12 H6 . . 109.5 ? C2 C12 H5 . . 109.5 ? H7 C12 H5 . . 109.5 ? H6 C12 H5 . . 109.5 ? O3 C13 C3 . . 117.92(9) ? O3 C13 C14 . . 119.77(9) ? C3 C13 C14 . . 122.11(10) ? C15 C14 C13 . . 117.32(10) ? C15 C14 C27 . . 120.52(9) ? C13 C14 C27 . . 122.05(10) ? C5 C15 C14 . . 121.75(10) ? C5 C15 H20 . . 119.1 ? C14 C15 H20 . . 119.1 ? O1 C16 N1 . . 125.23(10) ? O1 C16 C7 . . 127.88(10) ? N1 C16 C7 . . 106.89(9) ? C11 C17 C18 . . 120.99(12) ? C11 C17 H9 . . 119.5 ? C18 C17 H9 . . 119.5 ? C8 C18 C17 . . 118.81(11) ? C8 C18 H10 . . 120.6 ? C17 C18 H10 . . 120.6 ? N1 C19 H13 . . 109.5 ? N1 C19 H11 . . 109.5 ? H13 C19 H11 . . 109.5 ? N1 C19 H12 . . 109.5 ? H13 C19 H12 . . 109.5 ? H11 C19 H12 . . 109.5 ? O2 C20 C21 . . 123.11(10) ? O2 C20 C6 . . 119.54(10) ? C21 C20 C6 . . 116.84(9) ? C22 C21 C26 . . 119.63(10) ? C22 C21 C20 . . 121.15(10) ? C26 C21 C20 . . 119.15(10) ? C23 C22 C21 . . 120.19(10) ? C23 C22 H14 . . 119.9 ? C21 C22 H14 . . 119.9 ? C24 C23 C22 . . 119.82(11) ? C24 C23 H18 . . 120.1 ? C22 C23 H18 . . 120.1 ? C23 C24 C25 . . 120.32(11) ? C23 C24 H15 . . 119.8 ? C25 C24 H15 . . 119.8 ? C24 C25 C26 . . 120.02(11) ? C24 C25 H16 . . 120.0 ? C26 C25 H16 . . 120.0 ? C25 C26 C21 . . 119.98(11) ? C25 C26 H17 . . 120.0 ? C21 C26 H17 . . 120.0 ? C29 C27 C30 . . 106.79(10) ? C29 C27 C28 . . 110.46(11) ? C30 C27 C28 . . 107.09(10) ? C29 C27 C14 . . 111.94(10) ? C30 C27 C14 . . 111.70(9) ? C28 C27 C14 . . 108.75(9) ? C27 C28 H22 . . 109.5 ? C27 C28 H23 . . 109.5 ? H22 C28 H23 . . 109.5 ? C27 C28 H21 . . 109.5 ? H22 C28 H21 . . 109.5 ? H23 C28 H21 . . 109.5 ? C27 C29 H24 . . 109.5 ? C27 C29 H25 . . 109.5 ? H24 C29 H25 . . 109.5 ? C27 C29 H26 . . 109.5 ? H24 C29 H26 . . 109.5 ? H25 C29 H26 . . 109.5 ? C27 C30 H27 . . 109.5 ? C27 C30 H29 . . 109.5 ? H27 C30 H29 . . 109.5 ? C27 C30 H28 . . 109.5 ? H27 C30 H28 . . 109.5 ? H29 C30 H28 . . 109.5 ? C2 C31 H30 . . 109.5 ? C2 C31 H31 . . 109.5 ? H30 C31 H31 . . 109.5 ? C2 C31 H32 . . 109.5 ? H30 C31 H32 . . 109.5 ? H31 C31 H32 . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C16 . 1.2257(14) ? O2 C20 . 1.2145(14) ? O3 C13 . 1.3742(13) ? O3 H3A . 0.869(17) ? N1 C16 . 1.3644(14) ? N1 C9 . 1.4063(15) ? N1 C19 . 1.4484(15) ? C1 C2 . 1.5409(15) ? C1 H4 . 0.98 ? C1 H1 . 0.98 ? C1 H3 . 0.98 ? C2 C31 . 1.5350(15) ? C2 C12 . 1.5356(16) ? C2 C3 . 1.5389(14) ? C3 C4 . 1.3946(15) ? C3 C13 . 1.4116(15) ? C4 C5 . 1.3916(15) ? C4 H19 . 0.95 ? C5 C15 . 1.3906(15) ? C5 C6 . 1.4890(14) ? C6 C7 . 1.3411(15) ? C6 C20 . 1.5192(14) ? C7 C8 . 1.4692(15) ? C7 C16 . 1.4983(15) ? C8 C18 . 1.3899(16) ? C8 C9 . 1.4024(16) ? C9 C10 . 1.3834(16) ? C10 C11 . 1.392(2) ? C10 H8 . 0.95 ? C11 C17 . 1.385(2) ? C11 H2 . 0.95 ? C12 H7 . 0.98 ? C12 H6 . 0.98 ? C12 H5 . 0.98 ? C13 C14 . 1.4129(15) ? C14 C15 . 1.3946(15) ? C14 C27 . 1.5417(15) ? C15 H20 . 0.95 ? C17 C18 . 1.3977(17) ? C17 H9 . 0.95 ? C18 H10 . 0.95 ? C19 H13 . 0.98 ? C19 H11 . 0.98 ? C19 H12 . 0.98 ? C20 C21 . 1.4929(15) ? C21 C22 . 1.3907(16) ? C21 C26 . 1.3965(15) ? C22 C23 . 1.3903(16) ? C22 H14 . 0.95 ? C23 C24 . 1.3855(17) ? C23 H18 . 0.95 ? C24 C25 . 1.3869(18) ? C24 H15 . 0.95 ? C25 C26 . 1.3870(17) ? C25 H16 . 0.95 ? C26 H17 . 0.95 ? C27 C29 . 1.5322(17) ? C27 C30 . 1.5335(16) ? C27 C28 . 1.5406(18) ? C28 H22 . 0.98 ? C28 H23 . 0.98 ? C28 H21 . 0.98 ? C29 H24 . 0.98 ? C29 H25 . 0.98 ? C29 H26 . 0.98 ? C30 H27 . 0.98 ? C30 H29 . 0.98 ? C30 H28 . 0.98 ? C31 H30 . 0.98 ? C31 H31 . 0.98 ? C31 H32 . 0.98 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O3 H3A O1 1_465 0.87 1.89 2.7454(12) 167.4 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C31 C2 C3 C4 . . . . 0.00(14) ? C12 C2 C3 C4 . . . . -118.65(11) ? C1 C2 C3 C4 . . . . 119.14(11) ? C31 C2 C3 C13 . . . . 178.66(10) ? C12 C2 C3 C13 . . . . 60.01(13) ? C1 C2 C3 C13 . . . . -62.20(13) ? C13 C3 C4 C5 . . . . 2.99(15) ? C2 C3 C4 C5 . . . . -178.29(9) ? C3 C4 C5 C15 . . . . -4.46(16) ? C3 C4 C5 C6 . . . . 177.65(9) ? C15 C5 C6 C7 . . . . 69.17(14) ? C4 C5 C6 C7 . . . . -112.97(12) ? C15 C5 C6 C20 . . . . -112.49(11) ? C4 C5 C6 C20 . . . . 65.37(12) ? C5 C6 C7 C8 . . . . 2.70(18) ? C20 C6 C7 C8 . . . . -175.47(10) ? C5 C6 C7 C16 . . . . -179.61(9) ? C20 C6 C7 C16 . . . . 2.23(16) ? C6 C7 C8 C18 . . . . -1.6(2) ? C16 C7 C8 C18 . . . . -179.56(12) ? C6 C7 C8 C9 . . . . 177.93(11) ? C16 C7 C8 C9 . . . . -0.06(11) ? C18 C8 C9 C10 . . . . -0.44(16) ? C7 C8 C9 C10 . . . . 179.97(10) ? C18 C8 C9 N1 . . . . 179.48(9) ? C7 C8 C9 N1 . . . . -0.12(12) ? C16 N1 C9 C10 . . . . -179.83(11) ? C19 N1 C9 C10 . . . . 0.66(18) ? C16 N1 C9 C8 . . . . 0.27(12) ? C19 N1 C9 C8 . . . . -179.25(10) ? C8 C9 C10 C11 . . . . 0.44(17) ? N1 C9 C10 C11 . . . . -179.46(11) ? C9 C10 C11 C17 . . . . -0.22(18) ? C4 C3 C13 O3 . . . . 177.04(9) ? C2 C3 C13 O3 . . . . -1.66(15) ? C4 C3 C13 C14 . . . . 2.14(15) ? C2 C3 C13 C14 . . . . -176.56(9) ? O3 C13 C14 C15 . . . . 179.59(9) ? C3 C13 C14 C15 . . . . -5.60(15) ? O3 C13 C14 C27 . . . . -4.22(15) ? C3 C13 C14 C27 . . . . 170.59(10) ? C4 C5 C15 C14 . . . . 0.74(16) ? C6 C5 C15 C14 . . . . 178.61(10) ? C13 C14 C15 C5 . . . . 4.12(15) ? C27 C14 C15 C5 . . . . -172.13(10) ? C9 N1 C16 O1 . . . . 179.60(10) ? C19 N1 C16 O1 . . . . -0.88(18) ? C9 N1 C16 C7 . . . . -0.29(12) ? C19 N1 C16 C7 . . . . 179.23(10) ? C6 C7 C16 O1 . . . . 2.11(17) ? C8 C7 C16 O1 . . . . -179.68(10) ? C6 C7 C16 N1 . . . . -178.00(10) ? C8 C7 C16 N1 . . . . 0.21(11) ? C10 C11 C17 C18 . . . . -0.01(19) ? C9 C8 C18 C17 . . . . 0.19(16) ? C7 C8 C18 C17 . . . . 179.65(11) ? C11 C17 C18 C8 . . . . 0.02(17) ? C7 C6 C20 O2 . . . . 91.92(13) ? C5 C6 C20 O2 . . . . -86.42(12) ? C7 C6 C20 C21 . . . . -96.06(12) ? C5 C6 C20 C21 . . . . 85.60(11) ? O2 C20 C21 C22 . . . . -175.42(10) ? C6 C20 C21 C22 . . . . 12.88(15) ? O2 C20 C21 C26 . . . . 7.67(16) ? C6 C20 C21 C26 . . . . -164.03(10) ? C26 C21 C22 C23 . . . . 1.25(16) ? C20 C21 C22 C23 . . . . -175.64(10) ? C21 C22 C23 C24 . . . . 0.51(18) ? C22 C23 C24 C25 . . . . -1.76(18) ? C23 C24 C25 C26 . . . . 1.23(18) ? C24 C25 C26 C21 . . . . 0.55(17) ? C22 C21 C26 C25 . . . . -1.78(16) ? C20 C21 C26 C25 . . . . 175.17(10) ? C15 C14 C27 C29 . . . . -118.24(12) ? C13 C14 C27 C29 . . . . 65.68(14) ? C15 C14 C27 C30 . . . . 1.46(15) ? C13 C14 C27 C30 . . . . -174.62(10) ? C15 C14 C27 C28 . . . . 119.43(11) ? C13 C14 C27 C28 . . . . -56.64(14) ?