#------------------------------------------------------------------------------ #$Date: 2023-12-12 04:18:51 +0200 (Tue, 12 Dec 2023) $ #$Revision: 288240 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/78/7247853.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_7247853 loop_ _publ_author_name 'Saletti, Mario' 'Venditti, Jacopo' 'Paolino, Marco' 'Zacchei, Arianna' 'Giuliani, Germano' 'Giorgi, Gianluca' 'Bonechi, Claudia' 'Donati, Alessandro' 'Cappelli, Andrea' _publ_section_title ; A tri(ethylene glycol)-tethered Morita--Baylis--Hillman dimer in the formation of macrocyclic crown ether-paracyclophane hybrid structures ; _journal_issue 51 _journal_name_full 'RSC Advances' _journal_page_first 35773 _journal_page_last 35780 _journal_paper_doi 10.1039/D3RA06792K _journal_volume 13 _journal_year 2023 _chemical_formula_moiety 'C36 H43 N7 O6' _chemical_formula_sum 'C36 H43 N7 O6' _chemical_formula_weight 669.77 _chemical_name_systematic 'dimethyl (14Z,11Z,3E,8E)-6-butyl-11H,11H-14,17-dioxa-6-aza-1,11(4,1)-ditriazola-2,10(1,4)-dibenzenacyclononadecaphane-3,8-diene-4,8-dicarboxylate' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yab' _space_group_name_H-M_alt 'P 1 21/a 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2019/2 _audit_update_record ; 2023-08-01 deposited with the CCDC. 2023-11-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.531(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.9638(9) _cell_length_b 22.3683(18) _cell_length_c 14.3096(13) _cell_measurement_reflns_used 513 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.28 _cell_measurement_theta_min 2.35 _cell_volume 3425.7(5) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXS-2013/1 (Sheldrick, 2013)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.829 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1588 _diffrn_reflns_av_unetI/netI 0.4356 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.829 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 13701 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.829 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.204 _diffrn_reflns_theta_min 2.318 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.299 _exptl_crystal_description prism _exptl_crystal_F_000 1424 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.150 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.041 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.692 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 445 _refine_ls_number_reflns 6994 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.692 _refine_ls_R_factor_all 0.2632 _refine_ls_R_factor_gt 0.0822 _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^)+(0.0163P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.1019 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2021 _reflns_number_total 6994 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra06792k2.cif _cod_data_source_block VC1972 _cod_depositor_comments ; The following automatic conversions were performed: data item '_space_group_crystal_system' value 'Monoclinic' was changed to 'monoclinic' 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 8170 2020-07-09 18:12:32Z antanas ; _cod_original_sg_symbol_H-M 'P21 /a' _cod_database_code 7247853 _shelx_shelxl_version_number 2019/2 _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_res_file ; TITL VC1972_4lotto in P2(1)/a shelx.res created by SHELXL-2019/2 at 14:14:43 on 01-Aug-2023 CELL 0.71073 10.963822 22.368269 14.309551 90. 102.5305 90. ZERR 4.00 0.000936 0.001764 0.001309 0.0 0.0075 0.0 LATT 1 SYMM -x+1/2, y+1/2,-z SFAC C H N O UNIT 144 172 28 24 MERG 2 FMAP 2 PLAN -25 ACTA BOND $H CONF L.S. 12 WGHT 0.016300 FVAR 1.40081 C1 1 0.363846 -0.027360 0.554560 11.00000 0.02794 0.03705 = 0.02981 -0.00247 0.00637 0.00262 C2 1 0.463298 -0.024858 0.633152 11.00000 0.05157 0.03906 = 0.03818 -0.00990 0.01652 0.00331 AFIX 43 H2 2 0.466411 0.005761 0.677575 11.00000 -1.20000 AFIX 0 C3 1 0.558135 -0.067053 0.646842 11.00000 0.02863 0.04372 = 0.03314 -0.00180 -0.00254 0.00493 AFIX 43 H3 2 0.623531 -0.064236 0.700282 11.00000 -1.20000 AFIX 0 C4 1 0.557272 -0.113217 0.582541 11.00000 0.02870 0.03029 = 0.03237 -0.00181 0.01027 -0.00110 C5 1 0.459184 -0.116349 0.503451 11.00000 0.05175 0.03652 = 0.03665 -0.01021 0.01776 0.00029 AFIX 43 H5 2 0.456496 -0.147101 0.459311 11.00000 -1.20000 AFIX 0 C6 1 0.365153 -0.073999 0.489708 11.00000 0.04007 0.04649 = 0.03244 -0.00649 0.00219 -0.00045 AFIX 43 H6 2 0.300696 -0.076609 0.435599 11.00000 -1.20000 AFIX 0 C7 1 0.654924 -0.159382 0.599088 11.00000 0.04151 0.02556 = 0.03248 -0.00056 0.01906 -0.00114 C8 1 0.729764 -0.178860 0.682925 11.00000 0.05119 0.03718 = 0.04683 -0.00746 0.01960 0.00542 AFIX 43 H8 2 0.732763 -0.164895 0.744598 11.00000 -1.20000 AFIX 0 N9 3 0.768084 -0.231613 0.560916 11.00000 0.06159 0.04369 = 0.04592 -0.00306 0.01927 0.00679 N10 3 0.678488 -0.192632 0.525236 11.00000 0.05943 0.04185 = 0.03754 0.00148 0.01383 0.01603 C11 1 0.889109 -0.261686 0.716265 11.00000 0.05160 0.05222 = 0.06052 0.00654 0.01137 0.00781 AFIX 23 H11A 2 0.903995 -0.247577 0.781864 11.00000 -1.20000 H11B 2 0.967585 -0.259966 0.695506 11.00000 -1.20000 AFIX 0 C12 1 0.843569 -0.325579 0.711936 11.00000 0.06714 0.04973 = 0.04810 0.00899 0.01597 0.02164 AFIX 23 H12A 2 0.828807 -0.340134 0.646590 11.00000 -1.20000 H12B 2 0.906138 -0.350844 0.751412 11.00000 -1.20000 AFIX 0 O13 4 0.731218 -0.327508 0.745559 11.00000 0.09565 0.03429 = 0.08423 -0.00514 0.05579 -0.00280 C14 1 0.683719 -0.385469 0.745847 11.00000 0.07254 0.06047 = 0.06282 -0.00573 0.01719 0.00557 AFIX 23 H14A 2 0.740608 -0.409726 0.792002 11.00000 -1.20000 H14B 2 0.676376 -0.403350 0.683115 11.00000 -1.20000 AFIX 0 C15 1 0.559303 -0.384104 0.770901 11.00000 0.07481 0.04971 = 0.06158 -0.00898 0.01299 -0.00206 AFIX 23 H15A 2 0.499365 -0.368646 0.716200 11.00000 -1.20000 H15B 2 0.535274 -0.424945 0.780920 11.00000 -1.20000 AFIX 0 O16 4 0.548481 -0.349932 0.852819 11.00000 0.05841 0.04429 = 0.05248 0.00095 0.00848 0.00580 C17 1 0.622649 -0.369578 0.939112 11.00000 0.05480 0.03440 = 0.06198 0.01534 0.00330 0.00158 AFIX 23 H17A 2 0.709492 -0.371536 0.934397 11.00000 -1.20000 H17B 2 0.596561 -0.409129 0.954574 11.00000 -1.20000 AFIX 0 C18 1 0.607330 -0.325528 1.015605 11.00000 0.04230 0.03797 = 0.05069 0.01440 0.01474 -0.00542 AFIX 23 H18A 2 0.519854 -0.323018 1.018356 11.00000 -1.20000 H18B 2 0.653826 -0.339335 1.077371 11.00000 -1.20000 AFIX 0 N19 3 0.772335 -0.258424 0.994192 11.00000 0.03192 0.03960 = 0.08216 0.01253 0.01310 0.00176 N20 3 0.785539 -0.201920 0.971405 11.00000 0.03210 0.03602 = 0.07506 0.01116 0.01413 0.00241 C21 1 0.673718 -0.174527 0.958924 11.00000 0.03025 0.03315 = 0.03041 -0.00283 0.00512 -0.00120 C22 1 0.585823 -0.215861 0.973528 11.00000 0.02865 0.03339 = 0.03946 0.00072 0.00681 0.00428 AFIX 43 H22 2 0.500767 -0.210064 0.969121 11.00000 -1.20000 AFIX 0 C23 1 0.658963 -0.111268 0.931553 11.00000 0.03524 0.02911 = 0.03310 0.00163 0.01040 -0.00255 C24 1 0.543308 -0.082748 0.911767 11.00000 0.02525 0.03781 = 0.03968 -0.00203 0.00963 -0.00840 AFIX 43 H24 2 0.472866 -0.104014 0.918579 11.00000 -1.20000 AFIX 0 C25 1 0.529991 -0.023825 0.882325 11.00000 0.03208 0.03543 = 0.03843 0.00436 0.00897 0.00423 AFIX 43 H25 2 0.450977 -0.006542 0.867953 11.00000 -1.20000 AFIX 0 C26 1 0.634216 0.010022 0.873957 11.00000 0.02854 0.03020 = 0.03447 -0.00384 0.00443 -0.00182 C27 1 0.750478 -0.018291 0.897157 11.00000 0.02585 0.03671 = 0.06285 0.00638 0.00724 -0.00556 AFIX 43 H27 2 0.821762 0.003397 0.893775 11.00000 -1.20000 AFIX 0 C28 1 0.762697 -0.077252 0.924841 11.00000 0.02771 0.03691 = 0.05721 0.00880 0.00808 0.00076 AFIX 43 H28 2 0.841631 -0.094615 0.939290 11.00000 -1.20000 AFIX 0 C29 1 0.632391 0.071576 0.837933 11.00000 0.02542 0.03705 = 0.03979 -0.00262 0.00410 -0.00739 AFIX 43 H29 2 0.709454 0.084833 0.829010 11.00000 -1.20000 AFIX 0 C30 1 0.541098 0.112331 0.815435 11.00000 0.02668 0.03131 = 0.03684 -0.00336 0.00337 -0.00169 C31 1 0.572267 0.172212 0.778527 11.00000 0.02750 0.04500 = 0.05907 0.00480 -0.00889 -0.00961 C32 1 0.408418 0.105302 0.826210 11.00000 0.03298 0.03387 = 0.03350 -0.00083 0.00097 0.00793 AFIX 23 H32A 2 0.408707 0.087391 0.887992 11.00000 -1.20000 H32B 2 0.370486 0.144545 0.825128 11.00000 -1.20000 AFIX 0 N33 3 0.331972 0.068211 0.750761 11.00000 0.02783 0.03028 = 0.02276 -0.00369 0.00542 -0.00358 C34 1 0.215924 0.050169 0.776266 11.00000 0.03612 0.03137 = 0.03513 -0.00185 0.00913 -0.00049 AFIX 23 H34A 2 0.237259 0.024021 0.831482 11.00000 -1.20000 H34B 2 0.169182 0.026405 0.723854 11.00000 -1.20000 AFIX 0 C35 1 0.127806 0.098659 0.799394 11.00000 0.03763 0.04925 = 0.03966 -0.01101 0.01201 0.00017 AFIX 23 H35A 2 0.167254 0.118819 0.858214 11.00000 -1.20000 H35B 2 0.112372 0.128089 0.748400 11.00000 -1.20000 AFIX 0 C36 1 0.003369 0.071623 0.810569 11.00000 0.03742 0.08551 = 0.05405 -0.01273 0.02192 -0.00172 AFIX 23 H36A 2 -0.040876 0.100664 0.841150 11.00000 -1.20000 H36B 2 0.019969 0.036913 0.852019 11.00000 -1.20000 AFIX 0 C37 1 -0.079787 0.053057 0.714881 11.00000 0.03515 0.08848 = 0.05857 -0.00108 0.00634 -0.00771 AFIX 137 H37A 2 -0.103057 0.087840 0.675778 11.00000 -1.50000 H37B 2 -0.153591 0.033811 0.726034 11.00000 -1.50000 H37C 2 -0.034934 0.025860 0.682740 11.00000 -1.50000 AFIX 0 C38 1 0.317462 0.097713 0.656511 11.00000 0.02336 0.03447 = 0.03925 0.00198 0.00849 0.00203 AFIX 23 H38A 2 0.399484 0.101938 0.642074 11.00000 -1.20000 H38B 2 0.284568 0.137604 0.661123 11.00000 -1.20000 AFIX 0 C39 1 0.233107 0.065575 0.573764 11.00000 0.02327 0.03997 = 0.02793 0.00639 0.00227 0.00071 C40 1 0.258187 0.014111 0.533377 11.00000 0.03489 0.04176 = 0.03422 0.00027 0.00649 0.00082 AFIX 43 H40 2 0.195882 0.002489 0.481520 11.00000 -1.20000 AFIX 0 C41 1 0.112435 0.094874 0.524260 11.00000 0.03710 0.05013 = 0.03750 0.00905 0.00657 0.00766 N90 3 0.797878 -0.222822 0.655480 11.00000 0.03827 0.03522 = 0.04424 0.00300 0.01021 0.00445 N91 3 0.652283 -0.266367 0.995583 11.00000 0.03304 0.03346 = 0.04599 0.00532 0.01373 -0.00444 O1 4 0.682940 0.173043 0.755100 11.00000 0.04800 0.03699 = 0.09332 0.01939 0.01819 -0.00654 O2 4 0.503903 0.214426 0.771279 11.00000 0.05370 0.03771 = 0.17386 0.02935 0.01811 0.01539 O3 4 0.048352 0.077845 0.451085 11.00000 0.06701 0.09611 = 0.05719 -0.02333 -0.03721 0.03658 O4 4 0.085146 0.142762 0.571594 11.00000 0.04469 0.05526 = 0.05119 0.00195 0.00912 0.02222 C42 1 -0.028184 0.174876 0.525606 11.00000 0.05994 0.06909 = 0.08960 0.01105 0.01544 0.03706 AFIX 137 H42A 2 -0.015420 0.193719 0.468212 11.00000 -1.50000 H42B 2 -0.046974 0.204754 0.568548 11.00000 -1.50000 H42C 2 -0.096561 0.147241 0.509865 11.00000 -1.50000 AFIX 0 C31B 1 0.721328 0.229758 0.720183 11.00000 0.07073 0.05295 = 0.14433 0.04071 0.01779 -0.02268 AFIX 137 H31A 2 0.665651 0.239886 0.660767 11.00000 -1.50000 H31B 2 0.804888 0.226184 0.710333 11.00000 -1.50000 H31C 2 0.718710 0.260534 0.766466 11.00000 -1.50000 AFIX 0 HKLF 4 REM VC1972_4lotto in P2(1)/a REM wR2 = 0.1019, GooF = S = 0.692, Restrained GooF = 0.692 for all data REM R1 = 0.0822 for 2021 Fo > 4sig(Fo) and 0.2632 for all 6994 data REM 445 parameters refined using 0 restraints END WGHT 0.0106 0.0000 REM Highest difference peak 0.150, deepest hole -0.182, 1-sigma level 0.041 Q1 1 0.4991 0.1909 0.8312 11.00000 0.05 0.15 Q2 1 0.0564 0.0002 0.8295 11.00000 0.05 0.14 Q3 1 0.5131 -0.4590 0.6830 11.00000 0.05 0.14 Q4 1 0.8018 -0.3617 0.7936 11.00000 0.05 0.14 Q5 1 0.0398 0.1930 0.8132 11.00000 0.05 0.14 Q6 1 0.3054 0.1452 0.6368 11.00000 0.05 0.14 Q7 1 0.4802 0.1127 0.7874 11.00000 0.05 0.14 Q8 1 0.4051 -0.1269 0.8731 11.00000 0.05 0.14 Q9 1 0.0288 0.2208 0.4992 11.00000 0.05 0.14 Q10 1 0.6325 0.2577 0.7100 11.00000 0.05 0.13 Q11 1 0.4856 -0.0505 0.7374 11.00000 0.05 0.13 Q12 1 0.4946 -0.3228 0.6908 11.00000 0.05 0.13 Q13 1 0.4364 0.0481 0.9224 11.00000 0.05 0.13 Q14 1 0.8824 -0.1723 0.5932 11.00000 0.05 0.13 Q15 1 -0.1461 0.1761 0.5734 11.00000 0.05 0.13 Q16 1 0.0150 0.1585 0.5513 11.00000 0.05 0.13 Q17 1 0.6642 -0.3490 0.6973 11.00000 0.05 0.13 Q18 1 0.9291 -0.0881 0.8749 11.00000 0.05 0.13 Q19 1 0.7178 -0.0160 0.6794 11.00000 0.05 0.12 Q20 1 0.7248 -0.2608 1.0133 11.00000 0.05 0.12 Q21 1 0.3086 -0.0372 0.3703 11.00000 0.05 0.12 Q22 1 0.6939 -0.0070 0.8886 11.00000 0.05 0.12 Q23 1 0.5777 -0.0534 0.9710 11.00000 0.05 0.12 Q24 1 -0.0179 0.1318 0.8019 11.00000 0.05 0.12 Q25 1 0.6744 0.1088 0.8758 11.00000 0.05 0.12 ; _shelx_res_checksum 74775 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, 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 C1 C 0.3638(3) -0.02736(14) 0.5546(3) 0.0316(10) Uani 1 1 d . . . . . C2 C 0.4633(4) -0.02486(15) 0.6332(3) 0.0419(12) Uani 1 1 d . . . . . H2 H 0.466411 0.005761 0.677575 0.050 Uiso 1 1 calc R U . . . C3 C 0.5581(3) -0.06705(14) 0.6468(3) 0.0366(11) Uani 1 1 d . . . . . H3 H 0.623531 -0.064236 0.700282 0.044 Uiso 1 1 calc R U . . . C4 C 0.5573(4) -0.11322(14) 0.5825(3) 0.0299(10) Uani 1 1 d . . . . . C5 C 0.4592(4) -0.11635(15) 0.5035(3) 0.0404(11) Uani 1 1 d . . . . . H5 H 0.456496 -0.147101 0.459311 0.048 Uiso 1 1 calc R U . . . C6 C 0.3652(4) -0.07400(15) 0.4897(3) 0.0405(11) Uani 1 1 d . . . . . H6 H 0.300696 -0.076609 0.435599 0.049 Uiso 1 1 calc R U . . . C7 C 0.6549(4) -0.15938(14) 0.5991(3) 0.0315(10) Uani 1 1 d . . . . . C8 C 0.7298(4) -0.17886(15) 0.6829(3) 0.0437(12) Uani 1 1 d . . . . . H8 H 0.732763 -0.164895 0.744598 0.052 Uiso 1 1 calc R U . . . N9 N 0.7681(3) -0.23161(13) 0.5609(3) 0.0492(10) Uani 1 1 d . . . . . N10 N 0.6785(3) -0.19263(13) 0.5252(2) 0.0458(10) Uani 1 1 d . . . . . C11 C 0.8891(4) -0.26169(15) 0.7163(3) 0.0549(13) Uani 1 1 d . . . . . H11A H 0.903995 -0.247577 0.781864 0.066 Uiso 1 1 calc R U . . . H11B H 0.967585 -0.259966 0.695506 0.066 Uiso 1 1 calc R U . . . C12 C 0.8436(4) -0.32558(15) 0.7119(3) 0.0545(13) Uani 1 1 d . . . . . H12A H 0.828807 -0.340134 0.646590 0.065 Uiso 1 1 calc R U . . . H12B H 0.906138 -0.350844 0.751412 0.065 Uiso 1 1 calc R U . . . O13 O 0.7312(3) -0.32751(10) 0.7456(2) 0.0659(10) Uani 1 1 d . . . . . C14 C 0.6837(4) -0.38547(17) 0.7458(3) 0.0649(15) Uani 1 1 d . . . . . H14A H 0.740608 -0.409726 0.792002 0.078 Uiso 1 1 calc R U . . . H14B H 0.676376 -0.403350 0.683115 0.078 Uiso 1 1 calc R U . . . C15 C 0.5593(4) -0.38410(17) 0.7709(3) 0.0623(15) Uani 1 1 d . . . . . H15A H 0.499365 -0.368646 0.716200 0.075 Uiso 1 1 calc R U . . . H15B H 0.535274 -0.424945 0.780920 0.075 Uiso 1 1 calc R U . . . O16 O 0.5485(3) -0.34993(10) 0.8528(2) 0.0523(9) Uani 1 1 d . . . . . C17 C 0.6226(4) -0.36958(15) 0.9391(3) 0.0518(13) Uani 1 1 d . . . . . H17A H 0.709492 -0.371536 0.934397 0.062 Uiso 1 1 calc R U . . . H17B H 0.596561 -0.409129 0.954574 0.062 Uiso 1 1 calc R U . . . C18 C 0.6073(3) -0.32553(14) 1.0156(3) 0.0429(12) Uani 1 1 d . . . . . H18A H 0.519854 -0.323018 1.018356 0.052 Uiso 1 1 calc R U . . . H18B H 0.653826 -0.339335 1.077371 0.052 Uiso 1 1 calc R U . . . N19 N 0.7723(3) -0.25842(13) 0.9942(3) 0.0511(11) Uani 1 1 d . . . . . N20 N 0.7855(3) -0.20192(12) 0.9714(2) 0.0473(11) Uani 1 1 d . . . . . C21 C 0.6737(3) -0.17453(14) 0.9589(3) 0.0315(10) Uani 1 1 d . . . . . C22 C 0.5858(3) -0.21586(14) 0.9735(3) 0.0339(11) Uani 1 1 d . . . . . H22 H 0.500767 -0.210064 0.969121 0.041 Uiso 1 1 calc R U . . . C23 C 0.6590(4) -0.11127(14) 0.9316(3) 0.0320(10) Uani 1 1 d . . . . . C24 C 0.5433(3) -0.08275(14) 0.9118(3) 0.0339(10) Uani 1 1 d . . . . . H24 H 0.472866 -0.104014 0.918579 0.041 Uiso 1 1 calc R U . . . C25 C 0.5300(3) -0.02382(14) 0.8823(3) 0.0351(11) Uani 1 1 d . . . . . H25 H 0.450977 -0.006542 0.867953 0.042 Uiso 1 1 calc R U . . . C26 C 0.6342(3) 0.01002(14) 0.8740(3) 0.0314(10) Uani 1 1 d . . . . . C27 C 0.7505(3) -0.01829(14) 0.8972(3) 0.0422(12) Uani 1 1 d . . . . . H27 H 0.821762 0.003397 0.893775 0.051 Uiso 1 1 calc R U . . . C28 C 0.7627(3) -0.07725(14) 0.9248(3) 0.0408(12) Uani 1 1 d . . . . . H28 H 0.841631 -0.094615 0.939290 0.049 Uiso 1 1 calc R U . . . C29 C 0.6324(3) 0.07158(14) 0.8379(3) 0.0345(11) Uani 1 1 d . . . . . H29 H 0.709454 0.084833 0.829010 0.041 Uiso 1 1 calc R U . . . C30 C 0.5411(3) 0.11233(14) 0.8154(3) 0.0321(10) Uani 1 1 d . . . . . C31 C 0.5723(4) 0.17221(17) 0.7785(3) 0.0466(13) Uani 1 1 d . . . . . C32 C 0.4084(3) 0.10530(14) 0.8262(3) 0.0344(10) Uani 1 1 d . . . . . H32A H 0.408707 0.087391 0.887992 0.041 Uiso 1 1 calc R U . . . H32B H 0.370486 0.144545 0.825128 0.041 Uiso 1 1 calc R U . . . N33 N 0.3320(3) 0.06821(11) 0.7508(2) 0.0270(8) Uani 1 1 d . . . . . C34 C 0.2159(3) 0.05017(13) 0.7763(3) 0.0340(10) Uani 1 1 d . . . . . H34A H 0.237259 0.024021 0.831482 0.041 Uiso 1 1 calc R U . . . H34B H 0.169182 0.026405 0.723854 0.041 Uiso 1 1 calc R U . . . C35 C 0.1278(3) 0.09866(14) 0.7994(3) 0.0416(11) Uani 1 1 d . . . . . H35A H 0.167254 0.118819 0.858214 0.050 Uiso 1 1 calc R U . . . H35B H 0.112372 0.128089 0.748400 0.050 Uiso 1 1 calc R U . . . C36 C 0.0034(4) 0.07162(17) 0.8106(3) 0.0572(13) Uani 1 1 d . . . . . H36A H -0.040876 0.100664 0.841150 0.069 Uiso 1 1 calc R U . . . H36B H 0.019969 0.036913 0.852019 0.069 Uiso 1 1 calc R U . . . C37 C -0.0798(4) 0.05306(16) 0.7149(3) 0.0613(14) Uani 1 1 d . . . . . H37A H -0.103057 0.087840 0.675778 0.092 Uiso 1 1 calc R U . . . H37B H -0.153591 0.033811 0.726034 0.092 Uiso 1 1 calc R U . . . H37C H -0.034934 0.025860 0.682740 0.092 Uiso 1 1 calc R U . . . C38 C 0.3175(3) 0.09771(14) 0.6565(3) 0.0321(10) Uani 1 1 d . . . . . H38A H 0.399484 0.101938 0.642074 0.039 Uiso 1 1 calc R U . . . H38B H 0.284568 0.137604 0.661123 0.039 Uiso 1 1 calc R U . . . C39 C 0.2331(3) 0.06557(15) 0.5738(3) 0.0309(10) Uani 1 1 d . . . . . C40 C 0.2582(3) 0.01411(14) 0.5334(3) 0.0371(11) Uani 1 1 d . . . . . H40 H 0.195882 0.002489 0.481520 0.045 Uiso 1 1 calc R U . . . C41 C 0.1124(4) 0.09487(17) 0.5243(3) 0.0418(12) Uani 1 1 d . . . . . N90 N 0.7979(3) -0.22282(13) 0.6555(3) 0.0391(9) Uani 1 1 d . . . . . N91 N 0.6523(3) -0.26637(12) 0.9956(2) 0.0367(9) Uani 1 1 d . . . . . O1 O 0.6829(3) 0.17304(10) 0.7551(2) 0.0590(9) Uani 1 1 d . . . . . O2 O 0.5039(3) 0.21443(11) 0.7713(3) 0.0894(14) Uani 1 1 d . . . . . O3 O 0.0484(3) 0.07785(12) 0.4511(2) 0.0811(12) Uani 1 1 d . . . . . O4 O 0.0851(2) 0.14276(11) 0.5716(2) 0.0506(8) Uani 1 1 d . . . . . C42 C -0.0282(4) 0.17488(16) 0.5256(3) 0.0730(16) Uani 1 1 d . . . . . H42A H -0.015420 0.193719 0.468212 0.109 Uiso 1 1 calc R U . . . H42B H -0.046974 0.204754 0.568548 0.109 Uiso 1 1 calc R U . . . H42C H -0.096561 0.147241 0.509865 0.109 Uiso 1 1 calc R U . . . C31B C 0.7213(4) 0.22976(15) 0.7202(4) 0.090(2) Uani 1 1 d . . . . . H31A H 0.665651 0.239886 0.660767 0.135 Uiso 1 1 calc R U . . . H31B H 0.804888 0.226184 0.710333 0.135 Uiso 1 1 calc R U . . . H31C H 0.718710 0.260534 0.766466 0.135 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 C1 0.028(3) 0.037(2) 0.030(3) -0.002(2) 0.006(2) 0.0026(19) C2 0.052(3) 0.039(2) 0.038(3) -0.010(2) 0.017(3) 0.003(2) C3 0.029(3) 0.044(2) 0.033(3) -0.002(2) -0.003(2) 0.005(2) C4 0.029(3) 0.030(2) 0.032(3) -0.002(2) 0.010(2) -0.0011(19) C5 0.052(3) 0.037(2) 0.037(3) -0.010(2) 0.018(3) 0.000(2) C6 0.040(3) 0.046(2) 0.032(3) -0.006(2) 0.002(2) 0.000(2) C7 0.042(3) 0.026(2) 0.032(3) -0.001(2) 0.019(2) -0.0011(19) C8 0.051(3) 0.037(2) 0.047(4) -0.007(2) 0.020(3) 0.005(2) N9 0.062(3) 0.044(2) 0.046(3) -0.003(2) 0.019(2) 0.0068(18) N10 0.059(3) 0.042(2) 0.038(3) 0.0015(18) 0.014(2) 0.0160(18) C11 0.052(3) 0.052(3) 0.061(4) 0.007(3) 0.011(3) 0.008(2) C12 0.067(4) 0.050(3) 0.048(4) 0.009(2) 0.016(3) 0.022(2) O13 0.096(3) 0.0343(17) 0.084(3) -0.0051(16) 0.056(2) -0.0028(16) C14 0.073(4) 0.060(3) 0.063(4) -0.006(3) 0.017(3) 0.006(3) C15 0.075(4) 0.050(3) 0.062(4) -0.009(3) 0.013(3) -0.002(2) O16 0.058(2) 0.0443(17) 0.052(2) 0.0009(16) 0.008(2) 0.0058(14) C17 0.055(3) 0.034(2) 0.062(4) 0.015(3) 0.003(3) 0.002(2) C18 0.042(3) 0.038(2) 0.051(3) 0.014(2) 0.015(3) -0.005(2) N19 0.032(2) 0.040(2) 0.082(3) 0.013(2) 0.013(2) 0.0018(17) N20 0.032(2) 0.036(2) 0.075(3) 0.0112(19) 0.014(2) 0.0024(16) C21 0.030(3) 0.033(2) 0.030(3) -0.003(2) 0.005(2) -0.001(2) C22 0.029(3) 0.033(2) 0.039(3) 0.001(2) 0.007(2) 0.004(2) C23 0.035(3) 0.029(2) 0.033(3) 0.0016(19) 0.010(2) -0.0025(19) C24 0.025(3) 0.038(2) 0.040(3) -0.002(2) 0.010(2) -0.0084(19) C25 0.032(3) 0.035(2) 0.038(3) 0.004(2) 0.009(2) 0.0042(19) C26 0.029(3) 0.030(2) 0.034(3) -0.0038(19) 0.004(2) -0.0018(19) C27 0.026(3) 0.037(2) 0.063(4) 0.006(2) 0.007(3) -0.0056(19) C28 0.028(3) 0.037(2) 0.057(3) 0.009(2) 0.008(2) 0.0008(19) C29 0.025(3) 0.037(2) 0.040(3) -0.003(2) 0.004(2) -0.0074(19) C30 0.027(3) 0.031(2) 0.037(3) -0.0034(19) 0.003(2) -0.0017(19) C31 0.027(3) 0.045(3) 0.059(4) 0.005(2) -0.009(3) -0.010(2) C32 0.033(3) 0.034(2) 0.033(3) -0.001(2) 0.001(2) 0.0079(18) N33 0.028(2) 0.0303(17) 0.023(2) -0.0037(15) 0.0054(18) -0.0036(14) C34 0.036(3) 0.031(2) 0.035(3) -0.0019(19) 0.009(2) -0.0005(18) C35 0.038(3) 0.049(2) 0.040(3) -0.011(2) 0.012(2) 0.000(2) C36 0.037(3) 0.086(3) 0.054(4) -0.013(3) 0.022(3) -0.002(2) C37 0.035(3) 0.088(3) 0.059(4) -0.001(3) 0.006(3) -0.008(2) C38 0.023(3) 0.034(2) 0.039(3) 0.002(2) 0.008(2) 0.0020(18) C39 0.023(3) 0.040(2) 0.028(3) 0.006(2) 0.002(2) 0.0007(19) C40 0.035(3) 0.042(2) 0.034(3) 0.000(2) 0.006(2) 0.001(2) C41 0.037(3) 0.050(3) 0.038(3) 0.009(3) 0.007(3) 0.008(2) N90 0.038(2) 0.0352(19) 0.044(3) 0.0030(19) 0.010(2) 0.0045(16) N91 0.033(2) 0.0335(19) 0.046(3) 0.0053(16) 0.014(2) -0.0044(16) O1 0.048(2) 0.0370(16) 0.093(3) 0.0194(16) 0.018(2) -0.0065(14) O2 0.054(2) 0.0377(17) 0.174(4) 0.029(2) 0.018(2) 0.0154(15) O3 0.067(3) 0.096(2) 0.057(3) -0.023(2) -0.037(2) 0.0366(18) O4 0.045(2) 0.0553(17) 0.051(2) 0.0020(16) 0.0091(18) 0.0222(14) C42 0.060(4) 0.069(3) 0.090(5) 0.011(3) 0.015(3) 0.037(3) C31B 0.071(4) 0.053(3) 0.144(6) 0.041(3) 0.018(4) -0.023(2) 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' 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 C2 C1 C6 116.7(3) . . ? C2 C1 C40 126.1(4) . . ? C6 C1 C40 117.2(4) . . ? C3 C2 C1 121.4(3) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C4 C3 C2 121.2(4) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 118.3(3) . . ? C5 C4 C7 120.4(3) . . ? C3 C4 C7 121.2(4) . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 122.1(4) . . ? C5 C6 H6 118.9 . . ? C1 C6 H6 118.9 . . ? N10 C7 C8 109.1(3) . . ? N10 C7 C4 120.9(4) . . ? C8 C7 C4 129.9(4) . . ? N90 C8 C7 104.0(4) . . ? N90 C8 H8 128.0 . . ? C7 C8 H8 128.0 . . ? N10 N9 N90 106.9(3) . . ? N9 N10 C7 108.0(3) . . ? N90 C11 C12 111.2(3) . . ? N90 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? N90 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? O13 C12 C11 108.6(3) . . ? O13 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? O13 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C14 O13 C12 112.4(3) . . ? O13 C14 C15 110.1(3) . . ? O13 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? O13 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? O16 C15 C14 117.0(4) . . ? O16 C15 H15A 108.0 . . ? C14 C15 H15A 108.0 . . ? O16 C15 H15B 108.0 . . ? C14 C15 H15B 108.0 . . ? H15A C15 H15B 107.3 . . ? C17 O16 C15 115.0(3) . . ? O16 C17 C18 107.5(3) . . ? O16 C17 H17A 110.2 . . ? C18 C17 H17A 110.2 . . ? O16 C17 H17B 110.2 . . ? C18 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? N91 C18 C17 110.7(3) . . ? N91 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? N91 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? N20 N19 N91 107.0(3) . . ? N19 N20 C21 108.8(3) . . ? N20 C21 C22 108.6(3) . . ? N20 C21 C23 121.2(3) . . ? C22 C21 C23 130.1(4) . . ? N91 C22 C21 103.7(3) . . ? N91 C22 H22 128.1 . . ? C21 C22 H22 128.1 . . ? C28 C23 C24 117.3(3) . . ? C28 C23 C21 120.1(3) . . ? C24 C23 C21 122.6(3) . . ? C25 C24 C23 122.0(3) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C24 C25 C26 120.6(3) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C27 117.1(3) . . ? C25 C26 C29 126.1(3) . . ? C27 C26 C29 116.8(3) . . ? C28 C27 C26 122.0(3) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C27 C28 C23 121.0(3) . . ? C27 C28 H28 119.5 . . ? C23 C28 H28 119.5 . . ? C30 C29 C26 132.4(4) . . ? C30 C29 H29 113.8 . . ? C26 C29 H29 113.8 . . ? C29 C30 C32 126.4(3) . . ? C29 C30 C31 118.3(4) . . ? C32 C30 C31 115.3(3) . . ? O2 C31 O1 123.9(4) . . ? O2 C31 C30 123.2(4) . . ? O1 C31 C30 113.0(3) . . ? N33 C32 C30 113.2(3) . . ? N33 C32 H32A 108.9 . . ? C30 C32 H32A 108.9 . . ? N33 C32 H32B 108.9 . . ? C30 C32 H32B 108.9 . . ? H32A C32 H32B 107.8 . . ? C34 N33 C32 111.2(3) . . ? C34 N33 C38 115.2(3) . . ? C32 N33 C38 110.4(3) . . ? N33 C34 C35 118.9(3) . . ? N33 C34 H34A 107.6 . . ? C35 C34 H34A 107.6 . . ? N33 C34 H34B 107.6 . . ? C35 C34 H34B 107.6 . . ? H34A C34 H34B 107.0 . . ? C36 C35 C34 111.1(3) . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C37 112.7(3) . . ? C35 C36 H36A 109.1 . . ? C37 C36 H36A 109.1 . . ? C35 C36 H36B 109.1 . . ? C37 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N33 C38 C39 115.3(3) . . ? N33 C38 H38A 108.4 . . ? C39 C38 H38A 108.4 . . ? N33 C38 H38B 108.4 . . ? C39 C38 H38B 108.4 . . ? H38A C38 H38B 107.5 . . ? C40 C39 C41 114.3(4) . . ? C40 C39 C38 126.5(3) . . ? C41 C39 C38 119.0(3) . . ? C39 C40 C1 132.9(4) . . ? C39 C40 H40 113.5 . . ? C1 C40 H40 113.5 . . ? O3 C41 O4 123.3(4) . . ? O3 C41 C39 124.4(4) . . ? O4 C41 C39 112.4(4) . . ? C8 N90 N9 112.0(3) . . ? C8 N90 C11 127.8(4) . . ? N9 N90 C11 120.0(3) . . ? C22 N91 N19 111.8(3) . . ? C22 N91 C18 128.2(3) . . ? N19 N91 C18 120.0(3) . . ? C31 O1 C31B 116.5(3) . . ? C41 O4 C42 115.3(3) . . ? O4 C42 H42A 109.5 . . ? O4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O1 C31B H31A 109.5 . . ? O1 C31B H31B 109.5 . . ? H31A C31B H31B 109.5 . . ? O1 C31B H31C 109.5 . . ? H31A C31B H31C 109.5 . . ? H31B C31B 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 C1 C2 1.387(5) . ? C1 C6 1.398(4) . ? C1 C40 1.464(4) . ? C2 C3 1.386(4) . ? C2 H2 0.9300 . ? C3 C4 1.382(4) . ? C3 H3 0.9300 . ? C4 C5 1.384(5) . ? C4 C7 1.469(5) . ? C5 C6 1.382(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N10 1.362(4) . ? C7 C8 1.369(5) . ? C8 N90 1.344(4) . ? C8 H8 0.9300 . ? N9 N10 1.330(4) . ? N9 N90 1.336(4) . ? C11 N90 1.461(4) . ? C11 C12 1.511(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O13 1.417(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? O13 C14 1.398(4) . ? C14 C15 1.484(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O16 1.426(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? O16 C17 1.394(4) . ? C17 C18 1.509(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N91 1.462(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? N19 N20 1.321(3) . ? N19 N91 1.333(4) . ? N20 C21 1.347(4) . ? C21 C22 1.384(4) . ? C21 C23 1.468(4) . ? C22 N91 1.344(4) . ? C22 H22 0.9300 . ? C23 C28 1.389(4) . ? C23 C24 1.393(4) . ? C24 C25 1.382(4) . ? C24 H24 0.9300 . ? C25 C26 1.397(4) . ? C25 H25 0.9300 . ? C26 C27 1.397(4) . ? C26 C29 1.469(4) . ? C27 C28 1.375(4) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.340(4) . ? C29 H29 0.9300 . ? C30 C32 1.504(4) . ? C30 C31 1.506(5) . ? C31 O2 1.196(4) . ? C31 O1 1.327(4) . ? C32 N33 1.471(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? N33 C34 1.455(4) . ? N33 C38 1.479(4) . ? C34 C35 1.536(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.532(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.529(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.516(5) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.343(4) . ? C39 C41 1.508(5) . ? C40 H40 0.9300 . ? C41 O3 1.190(5) . ? C41 O4 1.336(4) . ? O1 C31B 1.459(4) . ? O4 C42 1.462(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C31B H31A 0.9600 . ? C31B H31B 0.9600 . ? C31B H31C 0.9600 . ? 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 C6 C1 C2 C3 -0.7(6) . . . . ? C40 C1 C2 C3 179.2(3) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C2 C3 C4 C7 -177.4(3) . . . . ? C3 C4 C5 C6 0.2(6) . . . . ? C7 C4 C5 C6 177.8(3) . . . . ? C4 C5 C6 C1 -0.9(6) . . . . ? C2 C1 C6 C5 1.1(6) . . . . ? C40 C1 C6 C5 -178.8(3) . . . . ? C5 C4 C7 N10 23.8(5) . . . . ? C3 C4 C7 N10 -158.7(4) . . . . ? C5 C4 C7 C8 -152.6(4) . . . . ? C3 C4 C7 C8 24.9(6) . . . . ? N10 C7 C8 N90 1.2(4) . . . . ? C4 C7 C8 N90 177.9(3) . . . . ? N90 N9 N10 C7 0.7(4) . . . . ? C8 C7 N10 N9 -1.2(4) . . . . ? C4 C7 N10 N9 -178.3(3) . . . . ? N90 C11 C12 O13 -61.0(5) . . . . ? C11 C12 O13 C14 -178.8(3) . . . . ? C12 O13 C14 C15 -173.5(4) . . . . ? O13 C14 C15 O16 -48.5(5) . . . . ? C14 C15 O16 C17 -62.3(5) . . . . ? C15 O16 C17 C18 175.3(3) . . . . ? O16 C17 C18 N91 -62.7(4) . . . . ? N91 N19 N20 C21 0.2(5) . . . . ? N19 N20 C21 C22 -0.7(5) . . . . ? N19 N20 C21 C23 -179.1(3) . . . . ? N20 C21 C22 N91 0.8(4) . . . . ? C23 C21 C22 N91 179.0(4) . . . . ? N20 C21 C23 C28 -4.7(6) . . . . ? C22 C21 C23 C28 177.2(4) . . . . ? N20 C21 C23 C24 175.5(4) . . . . ? C22 C21 C23 C24 -2.5(7) . . . . ? C28 C23 C24 C25 2.9(6) . . . . ? C21 C23 C24 C25 -177.3(3) . . . . ? C23 C24 C25 C26 -1.8(6) . . . . ? C24 C25 C26 C27 -0.4(6) . . . . ? C24 C25 C26 C29 175.9(4) . . . . ? C25 C26 C27 C28 1.5(6) . . . . ? C29 C26 C27 C28 -175.1(4) . . . . ? C26 C27 C28 C23 -0.4(6) . . . . ? C24 C23 C28 C27 -1.8(6) . . . . ? C21 C23 C28 C27 178.5(4) . . . . ? C25 C26 C29 C30 8.7(7) . . . . ? C27 C26 C29 C30 -175.0(4) . . . . ? C26 C29 C30 C32 2.9(7) . . . . ? C26 C29 C30 C31 -179.2(4) . . . . ? C29 C30 C31 O2 -167.5(4) . . . . ? C32 C30 C31 O2 10.6(6) . . . . ? C29 C30 C31 O1 12.5(5) . . . . ? C32 C30 C31 O1 -169.4(4) . . . . ? C29 C30 C32 N33 -77.2(5) . . . . ? C31 C30 C32 N33 104.8(4) . . . . ? C30 C32 N33 C34 165.7(3) . . . . ? C30 C32 N33 C38 -65.1(4) . . . . ? C32 N33 C34 C35 56.8(4) . . . . ? C38 N33 C34 C35 -69.9(4) . . . . ? N33 C34 C35 C36 172.0(3) . . . . ? C34 C35 C36 C37 -73.6(4) . . . . ? C34 N33 C38 C39 -49.1(4) . . . . ? C32 N33 C38 C39 -176.1(3) . . . . ? N33 C38 C39 C40 -71.0(5) . . . . ? N33 C38 C39 C41 114.3(4) . . . . ? C41 C39 C40 C1 177.6(4) . . . . ? C38 C39 C40 C1 2.6(7) . . . . ? C2 C1 C40 C39 7.2(7) . . . . ? C6 C1 C40 C39 -172.9(4) . . . . ? C40 C39 C41 O3 -6.2(6) . . . . ? C38 C39 C41 O3 169.1(4) . . . . ? C40 C39 C41 O4 174.1(3) . . . . ? C38 C39 C41 O4 -10.5(5) . . . . ? C7 C8 N90 N9 -0.7(4) . . . . ? C7 C8 N90 C11 -176.6(3) . . . . ? N10 N9 N90 C8 0.0(4) . . . . ? N10 N9 N90 C11 176.2(3) . . . . ? C12 C11 N90 C8 112.6(4) . . . . ? C12 C11 N90 N9 -62.9(5) . . . . ? C21 C22 N91 N19 -0.7(4) . . . . ? C21 C22 N91 C18 -178.1(4) . . . . ? N20 N19 N91 C22 0.3(5) . . . . ? N20 N19 N91 C18 177.9(3) . . . . ? C17 C18 N91 C22 114.1(4) . . . . ? C17 C18 N91 N19 -63.1(5) . . . . ? O2 C31 O1 C31B 1.0(7) . . . . ? C30 C31 O1 C31B -179.0(3) . . . . ? O3 C41 O4 C42 -2.0(6) . . . . ? C39 C41 O4 C42 177.6(3) . . . . ?