#------------------------------------------------------------------------------ #$Date: 2022-09-06 12:58:34 +0300 (Tue, 06 Sep 2022) $ #$Revision: 277664 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/74/1567439.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_1567439 loop_ _publ_author_name 'Mondal, Debashis' 'Dandekar, Bhupendra R.' 'Ahmad, Manzoor' 'Mondal, Abhishek' 'Mondal, Jagannath' 'Talukdar, Pinaki' _publ_section_title ; Selective and rapid water transportation across a self-assembled peptide-diol channel via the formation of a dual water array ; _journal_issue 33 _journal_name_full 'Chemical Science' _journal_page_first 9614 _journal_page_last 9623 _journal_paper_doi 10.1039/D2SC01737G _journal_volume 13 _journal_year 2022 _chemical_formula_moiety '(C25 H40 N2 O4)' _chemical_formula_sum 'C25 H40 N2 O4' _chemical_formula_weight 432.59 _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_creation_date 2021-06-25 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-11-16 deposited with the CCDC. 2022-07-20 downloaded from the CCDC. ; _cell_angle_alpha 81.540(6) _cell_angle_beta 78.191(6) _cell_angle_gamma 89.814(6) _cell_formula_units_Z 2 _cell_length_a 9.3339(19) _cell_length_b 9.6044(18) _cell_length_c 14.535(3) _cell_measurement_reflns_used 4670 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 24.29 _cell_measurement_theta_min 2.23 _cell_volume 1261.1(4) _computing_cell_refinement 'SAINT V8.40A (?, 2016)' _computing_data_reduction 'SAINT V8.40A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_unetI/netI 0.0737 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 16669 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 24.756 _diffrn_reflns_theta_max 24.756 _diffrn_reflns_theta_min 2.145 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_T_max 0.7451 _exptl_absorpt_correction_T_min 0.6755 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1504 before and 0.0582 after correction. The Ratio of minimum to maximum transmission is 0.9066. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.139 _exptl_crystal_description Round _exptl_crystal_F_000 550 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF : Nitrobenzene (10:1)' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.35 _refine_diff_density_max 1.259 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.077 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 284 _refine_ls_number_reflns 4296 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.1553 _refine_ls_R_factor_gt 0.0938 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+3.6567P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2134 _refine_ls_wR_factor_ref 0.2500 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2656 _reflns_number_total 4296 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2sc01737g2.cif _cod_data_source_block Compound_14R _cod_depositor_comments 'Adding full bibliography for 1567439--1567440.cif.' _cod_database_code 1567439 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C12-C11 1.507 with sigma of 0.02 C9-C10 1.507 with sigma of 0.02 C12-C11 = C10-C9 1.507 with sigma of 0.04 C14-C13 \\sim C12-C11 with sigma of 0.02 C8-C7 \\sim C9-C10 with sigma of 0.02 3.a Ternary CH refined with riding coordinates: C16(H16), C6(H6), C5(H5) 3.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C17(H17A,H17B), C4(H4A,H4B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A, H12B), C11(H11A,H11B), C10(H10A,H10B), C13(H13A,H13B) 3.c Aromatic/amide H refined with riding coordinates: N1(H1), N2(H2), C20(H20), C19(H19), C21(H21), C23(H23), C22(H22) 3.d Idealised Me refined as rotating group: C25(H25A,H25B,H25C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C14(H14A,H14B,H14C) ; _shelx_res_file ; TITL DMData52_a.res in P-1 dmdata52_a.res created by SHELXL-2018/3 at 16:25:59 on 25-Jun-2021 CELL 0.71073 9.3339 9.6044 14.5349 81.54 78.191 89.814 ZERR 25 0.0019 0.0018 0.0027 0.006 0.006 0.006 LATT 1 SFAC C H N O UNIT 25 25 25 25 DFIX 1.507 C12 C11 DFIX 1.507 C9 C10 SADI C14 C13 C12 C11 SADI C8 C7 C9 C10 DANG 1.507 C12 C11 C10 C9 L.S. 5 PLAN 20 TEMP 23 BOND $H fmap 2 acta REM REM REM WGHT 0.085100 3.656700 FVAR 0.66164 O4 4 0.414706 0.303914 0.558249 11.00000 0.01873 0.03655 = 0.04590 0.00617 -0.01155 0.00102 O2 4 0.431006 0.991338 0.270309 11.00000 0.03944 0.04245 = 0.02527 0.00595 -0.00879 -0.01405 O3 4 0.089631 0.634253 0.416091 11.00000 0.01739 0.04017 = 0.06611 0.01933 -0.01347 -0.00588 N1 3 0.303703 0.749382 0.406337 11.00000 0.01180 0.02741 = 0.03891 0.00832 -0.00515 0.00039 AFIX 43 H1 2 0.396968 0.741830 0.399674 11.00000 -1.20000 AFIX 0 N2 3 0.217395 0.423806 0.531709 11.00000 0.01431 0.02987 = 0.02963 0.00830 -0.00412 -0.00008 AFIX 43 H2 2 0.127859 0.443536 0.552815 11.00000 -1.20000 AFIX 0 O1 4 0.334736 0.950927 0.144042 11.00000 0.06286 0.07968 = 0.03297 -0.00256 -0.02126 -0.02543 C16 1 0.294770 0.493769 0.439024 11.00000 0.01723 0.02630 = 0.03213 0.00599 -0.00621 -0.00369 AFIX 13 H16 2 0.396850 0.512218 0.441879 11.00000 -1.20000 AFIX 0 C15 1 0.221093 0.633554 0.419193 11.00000 0.01932 0.03419 = 0.02813 0.00783 -0.00464 -0.00284 C24 1 0.284515 0.329357 0.584040 11.00000 0.02073 0.02291 = 0.02865 0.00003 -0.01099 -0.00161 C6 1 0.242219 0.889134 0.403078 11.00000 0.01961 0.02760 = 0.03460 0.00601 -0.00394 0.00270 AFIX 13 H6 2 0.135537 0.877658 0.422776 11.00000 -1.20000 AFIX 0 C5 1 0.276983 0.972829 0.303934 11.00000 0.03352 0.02753 = 0.03725 0.00423 -0.01507 -0.00016 AFIX 13 H5 2 0.232713 1.065356 0.305339 11.00000 -1.20000 AFIX 0 C3 1 0.457585 1.011357 0.168961 11.00000 0.05104 0.02677 = 0.02524 0.00099 -0.01195 -0.00692 C7 1 0.296596 0.968232 0.473977 11.00000 0.03280 0.03845 = 0.03333 0.00205 -0.00620 0.00334 AFIX 23 H7A 2 0.247614 1.057354 0.475383 11.00000 -1.20000 H7B 2 0.400661 0.988773 0.451726 11.00000 -1.20000 AFIX 0 C25 1 0.192750 0.257775 0.675699 11.00000 0.03324 0.04041 = 0.02886 0.00558 -0.00897 -0.00178 AFIX 137 H25A 2 0.194092 0.157662 0.676475 11.00000 -1.50000 H25B 2 0.093881 0.288797 0.681318 11.00000 -1.50000 H25C 2 0.231529 0.281038 0.727986 11.00000 -1.50000 AFIX 0 C17 1 0.291379 0.401865 0.362629 11.00000 0.03808 0.02969 = 0.03619 0.00534 -0.01218 -0.00905 AFIX 23 H17A 2 0.322053 0.308040 0.383712 11.00000 -1.20000 H17B 2 0.191780 0.394164 0.353524 11.00000 -1.20000 AFIX 0 C18 1 0.389791 0.460745 0.269273 11.00000 0.04492 0.02540 = 0.03183 -0.00267 -0.01167 -0.00568 C20 1 0.332665 0.523369 0.192541 11.00000 0.05950 0.03147 = 0.03441 -0.00371 -0.01721 -0.00207 AFIX 43 H20 2 0.231803 0.528615 0.198171 11.00000 -1.20000 AFIX 0 C19 1 0.539519 0.455466 0.258784 11.00000 0.04741 0.03737 = 0.03975 0.00099 -0.00841 -0.00325 AFIX 43 H19 2 0.579316 0.414752 0.309695 11.00000 -1.20000 AFIX 0 C4 1 0.230478 0.903883 0.226995 11.00000 0.03936 0.04149 = 0.04469 0.00071 -0.02174 -0.00069 AFIX 23 H4A 2 0.230293 0.802105 0.242300 11.00000 -1.20000 H4B 2 0.133231 0.932333 0.219452 11.00000 -1.20000 AFIX 0 C21 1 0.425138 0.577823 0.107980 11.00000 0.09276 0.03415 = 0.02965 0.00008 -0.01428 -0.00465 AFIX 43 H21 2 0.386051 0.619965 0.057116 11.00000 -1.20000 AFIX 0 C23 1 0.573405 0.570286 0.098466 11.00000 0.08057 0.03614 = 0.03639 -0.00428 0.00711 -0.01253 AFIX 43 H23 2 0.634804 0.606147 0.041028 11.00000 -1.20000 AFIX 0 C2 1 0.467806 1.165565 0.129104 11.00000 0.09504 0.03158 = 0.03588 0.00576 -0.01073 -0.00069 AFIX 137 H2A 2 0.379393 1.209923 0.154952 11.00000 -1.50000 H2B 2 0.480875 1.176458 0.061155 11.00000 -1.50000 H2C 2 0.549672 1.208697 0.145775 11.00000 -1.50000 AFIX 0 C22 1 0.632118 0.509641 0.173832 11.00000 0.05269 0.04212 = 0.05183 -0.00757 0.00771 -0.00812 AFIX 43 H22 2 0.733096 0.505079 0.167767 11.00000 -1.20000 AFIX 0 C8 1 0.270711 0.887472 0.575472 11.00000 0.06847 0.05710 = 0.02800 0.00019 -0.00073 0.03236 AFIX 23 H8A 2 0.323333 0.800293 0.574136 11.00000 -1.20000 H8B 2 0.312344 0.942979 0.614658 11.00000 -1.20000 AFIX 0 C1 1 0.594171 0.934672 0.134297 11.00000 0.06862 0.04925 = 0.04771 -0.01283 -0.02045 0.00566 AFIX 137 H1A 2 0.674776 0.972029 0.155678 11.00000 -1.50000 H1B 2 0.614956 0.946793 0.066086 11.00000 -1.50000 H1C 2 0.579969 0.836246 0.159000 11.00000 -1.50000 AFIX 0 C9 1 0.113992 0.852986 0.621535 11.00000 0.11056 0.04183 = 0.05235 0.00595 0.04589 -0.00786 AFIX 23 H9A 2 0.073967 0.811414 0.574977 11.00000 -1.20000 H9B 2 0.068468 0.943537 0.624895 11.00000 -1.20000 AFIX 0 C12 1 0.020377 0.733533 0.889881 11.00000 0.07142 0.13735 = 0.02668 -0.02715 -0.00905 0.04170 AFIX 23 H12A 2 -0.084334 0.730839 0.892732 11.00000 -1.20000 H12B 2 0.052279 0.637299 0.900089 11.00000 -1.20000 AFIX 0 C14 1 -0.001281 0.745537 1.063908 11.00000 0.09697 0.13869 = 0.03537 -0.01684 -0.00512 -0.04282 AFIX 137 H14A 2 -0.104895 0.757144 1.082349 11.00000 -1.50000 H14B 2 0.048572 0.794630 1.101641 11.00000 -1.50000 H14C 2 0.019862 0.647220 1.073688 11.00000 -1.50000 AFIX 0 C11 1 0.109769 0.816104 0.778075 11.00000 0.07049 0.04574 = 0.20738 0.02530 -0.08730 -0.00972 AFIX 23 H11A 2 0.096061 0.916986 0.770652 11.00000 -1.20000 H11B 2 0.213694 0.797812 0.766364 11.00000 -1.20000 AFIX 0 C10 1 0.044673 0.757054 0.723232 11.00000 0.13344 0.06874 = 0.55121 -0.11792 -0.22167 0.04117 AFIX 23 H10A 2 -0.060830 0.764501 0.740131 11.00000 -1.20000 H10B 2 0.069518 0.658878 0.723450 11.00000 -1.20000 AFIX 0 C13 1 0.049670 0.804298 0.960884 11.00000 0.36542 0.10486 = 0.04298 -0.02021 0.07545 -0.09118 AFIX 23 H13A 2 0.009161 0.897185 0.951363 11.00000 -1.20000 H13B 2 0.155112 0.817714 0.949749 11.00000 -1.20000 AFIX 0 HKLF 4 REM DMData52_a.res in P-1 REM wR2 = 0.2500, GooF = S = 1.035, Restrained GooF = 1.080 for all data REM R1 = 0.0938 for 2656 Fo > 4sig(Fo) and 0.1553 for all 4296 data REM 284 parameters refined using 6 restraints END WGHT 0.0888 3.7348 REM Highest difference peak 1.259, deepest hole -0.965, 1-sigma level 0.077 Q1 1 -0.0048 0.7297 0.7994 11.00000 0.05 1.26 Q2 1 0.1439 0.8053 0.7261 11.00000 0.05 0.61 Q3 1 0.0874 0.7888 0.9831 11.00000 0.05 0.47 Q4 1 -0.0246 0.6594 0.9095 11.00000 0.05 0.36 Q5 1 -0.0471 0.8017 0.9657 11.00000 0.05 0.33 Q6 1 0.0813 0.8917 0.9642 11.00000 0.05 0.23 Q7 1 0.1156 0.8764 0.7836 11.00000 0.05 0.23 Q8 1 0.1525 0.9030 0.7838 11.00000 0.05 0.22 Q9 1 0.0900 0.4950 0.3371 11.00000 0.05 0.21 Q10 1 0.2306 0.6919 0.7258 11.00000 0.05 0.20 Q11 1 -0.0591 0.6823 0.7256 11.00000 0.05 0.20 Q12 1 -0.1027 0.8256 0.8167 11.00000 0.05 0.19 Q13 1 0.5347 0.8395 0.1751 11.00000 0.05 0.19 Q14 1 0.3988 0.1372 0.6231 11.00000 0.05 0.19 Q15 1 0.4746 0.9170 0.3611 11.00000 0.05 0.19 Q16 1 0.2165 1.1398 0.5563 11.00000 0.05 0.18 Q17 1 0.1992 0.7260 0.9430 11.00000 0.05 0.18 Q18 1 0.1819 0.6886 0.2377 11.00000 0.05 0.18 Q19 1 0.1046 0.7562 0.4187 11.00000 0.05 0.18 Q20 1 0.1294 0.1667 0.6040 11.00000 0.05 0.18 ; _shelx_res_checksum 42920 _shelx_hkl_file ; -1 0 0 929.21 25.70 -1 0 0 901.51 25.20 1 0 0 819.82 25.80 1 0 0 920.41 25.20 1 0 0 890.61 25.20 -2 0 0 176.28 6.90 -2 0 0 180.18 7.80 -2 0 0 188.08 8.40 -2 0 0 172.58 6.90 2 0 0 170.78 7.10 2 0 0 178.28 7.90 2 0 0 185.08 8.30 2 0 0 177.38 6.90 -3 0 0 629.84 23.20 -3 0 0 651.43 22.10 -3 0 0 634.54 20.60 -3 0 0 682.33 20.90 -3 0 0 626.44 20.30 3 0 0 636.14 22.20 3 0 0 576.14 22.00 3 0 0 669.03 20.60 3 0 0 620.94 20.70 3 0 0 628.84 20.30 -4 0 0 101.69 6.40 -4 0 0 109.99 6.60 -4 0 0 100.19 9.30 -4 0 0 97.09 9.20 -4 0 0 108.59 6.90 4 0 0 92.09 6.70 4 0 0 100.19 6.70 4 0 0 99.99 9.00 4 0 0 97.79 9.30 4 0 0 110.29 6.60 -5 0 0 -4.10 2.80 -5 0 0 2.90 3.40 -5 0 0 -5.20 4.90 -5 0 0 3.80 3.20 5 0 0 0.00 3.50 5 0 0 4.40 3.50 5 0 0 1.50 5.10 5 0 0 6.60 4.80 -6 0 0 355.56 16.00 -6 0 0 332.07 19.10 -6 0 0 347.47 16.40 -6 0 0 352.96 15.40 6 0 0 381.16 16.30 6 0 0 320.97 17.30 6 0 0 315.67 15.50 -7 0 0 82.19 12.40 -7 0 0 87.99 9.90 -7 0 0 66.39 8.80 7 0 0 78.89 12.70 7 0 0 91.99 9.70 -8 0 0 29.40 10.40 -8 0 0 35.80 7.70 -8 0 0 22.60 7.50 8 0 0 44.70 8.40 8 0 0 28.50 9.40 -9 0 0 19.70 7.50 -9 0 0 21.40 12.00 -9 0 0 14.60 7.20 9 0 0 15.30 9.60 9 0 0 22.60 7.90 -10 0 0 36.60 15.00 -10 0 0 64.99 11.20 -10 0 0 59.39 14.80 10 0 0 101.69 15.80 10 0 0 52.99 13.30 10 -1 0 29.50 12.70 10 -1 0 32.00 9.70 -10 1 0 38.00 10.70 -10 1 0 50.69 10.90 -10 1 0 15.00 13.40 9 -1 0 9.70 9.60 9 -1 0 2.70 7.60 -9 1 0 -10.40 9.50 -9 1 0 -9.00 6.80 -9 1 0 5.90 8.10 8 -1 0 52.89 11.60 8 -1 0 48.20 8.60 -8 1 0 33.30 9.70 -8 1 0 50.69 8.20 -8 1 0 49.90 8.50 7 -1 0 60.69 8.40 7 -1 0 55.29 9.80 -7 1 0 83.39 9.70 -7 1 0 46.30 9.60 -7 1 0 53.89 7.60 6 -1 0 7.50 5.40 6 -1 0 13.40 4.50 -6 1 0 13.60 5.10 -6 1 0 7.50 3.80 -6 1 0 9.00 4.60 -6 1 0 4.50 5.10 5 -1 0 101.49 10.20 5 -1 0 118.09 10.00 5 -1 0 108.89 7.90 5 -1 0 99.89 8.00 -5 1 0 94.29 7.10 -5 1 0 103.69 10.50 -5 1 0 82.79 10.00 -5 1 0 94.99 7.60 -5 1 0 93.99 7.80 4 -1 0 209.68 10.10 4 -1 0 214.38 11.50 4 -1 0 205.98 10.10 4 -1 0 219.48 12.40 -4 1 0 178.18 14.00 -4 1 0 205.78 9.50 -4 1 0 207.98 11.50 -4 1 0 210.08 11.60 -4 1 0 220.18 10.10 3 -1 0 41.60 5.60 3 -1 0 42.80 5.40 3 -1 0 44.40 4.20 3 -1 0 48.30 4.70 -3 1 0 53.09 4.80 -3 1 0 43.40 5.20 -3 1 0 49.60 4.20 -3 1 0 45.60 3.70 -3 1 0 38.10 5.90 2 -1 0 752.32 24.60 2 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950.10 31.20 -4 -1 0 906.11 29.30 4 1 0 1027.70 29.60 4 1 0 952.70 30.90 4 1 0 925.01 30.50 4 1 0 927.31 31.80 4 1 0 936.31 33.20 -5 -1 0 18.70 4.00 -5 -1 0 12.50 6.40 -5 -1 0 18.00 6.10 -5 -1 0 16.90 4.90 -5 -1 0 21.40 3.90 5 1 0 23.20 4.50 5 1 0 21.20 5.70 5 1 0 21.80 4.60 5 1 0 18.10 4.00 5 1 0 20.80 6.50 -6 -1 0 15.20 5.00 -6 -1 0 12.30 5.50 -6 -1 0 16.80 4.60 -6 -1 0 13.10 5.80 6 1 0 11.60 4.70 6 1 0 6.60 4.70 6 1 0 12.70 4.30 -7 -1 0 17.20 7.80 -7 -1 0 10.00 5.10 -7 -1 0 9.60 5.10 7 1 0 11.90 6.00 7 1 0 4.70 6.00 7 1 0 4.60 4.70 -8 -1 0 21.90 6.60 -8 -1 0 24.20 7.60 -8 -1 0 28.70 10.30 8 1 0 28.20 9.20 8 1 0 23.90 6.90 -9 -1 0 -0.50 7.20 -9 -1 0 2.20 6.60 -9 -1 0 10.30 12.20 9 1 0 5.70 7.20 -10 -1 0 23.80 10.50 -10 -1 0 31.60 16.40 10 1 0 15.40 9.30 10 -2 0 1.50 8.90 10 -2 0 9.10 10.90 -10 2 0 -3.80 13.20 -10 2 0 11.80 10.10 -10 2 0 9.10 9.30 9 -2 0 2.70 7.40 -9 2 0 11.60 7.70 -9 2 0 -19.00 10.20 -9 2 0 7.80 7.90 8 -2 0 46.30 10.90 8 -2 0 40.70 8.20 -8 2 0 41.90 8.50 -8 2 0 34.40 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5.70 4.70 -4 -6 0 12.00 5.00 4 6 0 8.90 5.40 -5 -6 0 83.09 12.20 -5 -6 0 88.29 9.60 5 6 0 78.09 12.40 -6 -6 0 6.00 7.60 -6 -6 0 -0.10 5.40 -7 -6 0 3.70 8.70 -7 -6 0 -13.00 12.60 -8 -6 0 -12.90 10.10 -8 -6 0 -8.90 7.70 8 -7 0 2.90 12.70 8 -7 0 9.50 9.50 -8 7 0 2.10 9.50 -8 7 0 0.50 11.20 7 -7 0 -8.40 7.60 7 -7 0 15.30 10.00 -7 7 0 0.40 9.90 -7 7 0 -1.00 5.40 -7 7 0 -13.90 7.50 6 -7 0 9.80 8.80 6 -7 0 3.80 6.30 -6 7 0 -10.50 6.50 -6 7 0 -0.60 8.20 -6 7 0 7.70 4.50 5 -7 0 126.39 11.20 5 -7 0 114.09 14.00 5 -7 0 126.49 10.60 -5 7 0 112.39 8.10 -5 7 0 115.69 7.30 -5 7 0 149.49 14.80 4 -7 0 11.60 5.20 4 -7 0 -0.90 3.40 -4 7 0 -9.40 4.60 -4 7 0 1.60 6.60 -4 7 0 8.40 3.60 3 -7 0 50.09 7.50 3 -7 0 33.90 3.70 3 -7 0 25.40 5.80 -3 7 0 31.50 6.70 -3 7 0 41.80 5.50 -3 7 0 29.70 4.60 2 -7 0 11.60 2.70 2 -7 0 12.40 3.60 2 -7 0 4.50 3.50 -2 7 0 11.30 3.80 -2 7 0 6.80 5.30 1 -7 0 21.60 3.40 1 -7 0 30.00 5.60 1 -7 0 14.00 3.50 -1 7 0 27.70 5.60 -1 7 0 25.90 4.80 0 -7 0 13.40 3.80 0 -7 0 21.20 3.70 0 -7 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-8 4 2.90 4.90 3 -8 4 19.80 6.30 4 -8 4 2.30 6.20 4 -8 4 6.70 6.00 5 -8 4 7.80 10.40 5 -8 4 27.30 7.90 -6 8 -4 8.00 6.80 6 -8 4 30.60 11.40 6 -8 4 8.00 8.90 -7 8 -4 16.10 8.60 7 -8 4 24.20 11.30 7 -8 4 32.50 13.80 -6 -7 4 6.90 9.80 -5 -7 4 166.28 15.90 -5 -7 4 181.88 17.60 -4 -7 4 2.90 3.00 -4 -7 4 -2.70 6.00 -4 -7 4 -0.40 6.00 -3 -7 4 24.80 6.50 -3 -7 4 18.20 3.60 -2 -7 4 3.50 2.50 -2 -7 4 0.70 3.80 -2 -7 4 -2.70 4.20 -2 -7 4 2.80 1.70 -2 -7 4 -2.60 3.70 1 7 -4 45.00 7.30 -1 -7 4 46.00 5.00 -1 -7 4 56.49 7.30 0 7 -4 5.00 4.20 0 -7 4 8.60 4.90 0 -7 4 5.60 2.70 0 -7 4 5.10 3.60 1 -7 4 221.38 9.50 1 -7 4 226.38 12.90 1 -7 4 238.18 11.50 1 -7 4 208.78 13.00 2 -7 4 2.80 3.60 2 -7 4 0.00 1.50 3 -7 4 14.80 4.50 3 -7 4 17.70 5.60 3 -7 4 25.40 6.40 4 -7 4 23.30 6.20 4 -7 4 34.10 7.60 4 -7 4 33.80 6.60 -5 7 -4 -6.10 4.40 5 -7 4 -5.30 5.40 5 -7 4 0.70 6.80 5 -7 4 -9.00 6.00 -6 7 -4 14.90 7.10 6 -7 4 19.80 9.30 -7 7 -4 -6.00 8.30 7 -7 4 -8.60 10.40 7 -7 4 -0.40 9.70 -7 -6 4 2.80 9.90 -7 -6 4 2.50 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7.50 6 -5 4 3.70 7.80 6 -5 4 17.10 6.10 -7 5 -4 15.00 8.30 7 -5 4 -4.50 8.00 7 -5 4 13.00 7.50 -8 5 -4 15.90 4.30 -8 5 -4 2.50 8.70 8 -5 4 34.10 10.40 9 -5 4 -21.50 10.20 9 -5 4 1.80 11.30 -8 -4 4 0.80 9.10 -8 -4 4 -2.10 6.70 -7 -4 4 18.20 8.90 -7 -4 4 25.80 8.70 -7 -4 4 31.80 7.40 6 4 -4 2.60 2.90 -6 -4 4 -1.40 7.50 -6 -4 4 6.70 5.80 -6 -4 4 6.70 4.70 5 4 -4 4.10 2.20 -5 -4 4 -7.50 5.80 -5 -4 4 3.30 6.00 -5 -4 4 -4.40 4.70 -5 -4 4 1.10 3.20 4 4 -4 129.29 10.20 -4 -4 4 135.69 11.70 -4 -4 4 149.29 9.90 -4 -4 4 142.29 7.20 -4 -4 4 133.29 10.20 3 4 -4 3.00 2.50 -3 -4 4 8.50 3.40 -3 -4 4 3.90 4.10 -3 -4 4 0.20 2.00 -3 -4 4 0.40 3.50 2 4 -4 72.79 6.80 2 4 -4 69.89 4.80 -2 -4 4 75.19 3.70 -2 -4 4 65.59 6.90 -2 -4 4 70.09 6.50 -1 -4 4 159.08 8.00 -1 -4 4 160.78 6.30 -1 -4 4 152.58 8.70 -1 -4 4 172.78 6.80 0 -4 4 393.86 12.80 0 -4 4 381.16 14.20 0 -4 4 381.96 12.90 0 -4 4 373.36 13.60 -1 4 -4 17.70 2.50 1 -4 4 18.50 2.30 1 -4 4 17.90 2.80 1 -4 4 20.00 3.60 1 -4 4 24.80 4.30 1 -4 4 21.80 3.10 -2 4 -4 -1.00 1.50 2 -4 4 -3.70 1.80 2 -4 4 -0.90 3.60 2 -4 4 -1.00 2.40 -3 4 -4 44.70 5.70 -3 4 -4 35.90 4.60 3 -4 4 31.80 4.80 3 -4 4 43.50 7.30 3 -4 4 33.30 5.10 3 -4 4 36.60 6.20 -4 4 -4 41.40 7.00 4 -4 4 47.90 6.80 4 -4 4 48.30 8.70 4 -4 4 40.90 6.60 5 -4 4 25.10 7.90 5 -4 4 43.20 7.70 5 -4 4 37.10 7.10 -6 4 -4 497.35 24.60 6 -4 4 508.55 24.60 6 -4 4 484.55 23.70 -7 4 -4 378.16 21.80 -7 4 -4 355.96 13.50 7 -4 4 336.27 21.60 7 -4 4 367.86 21.50 -8 4 -4 -5.10 4.00 8 -4 4 1.90 9.10 8 -4 4 -3.80 7.40 -9 4 -4 9.70 5.80 9 -4 4 -4.80 8.70 9 -4 4 19.30 10.80 10 -4 4 -4.50 11.20 10 -4 4 -15.00 11.20 -9 -3 4 -5.90 10.10 -9 -3 4 14.90 8.80 -9 -3 4 7.80 13.10 -8 -3 4 199.18 17.90 -8 -3 4 212.78 14.80 -8 -3 4 194.08 24.80 7 3 -4 5.90 4.40 -7 -3 4 5.40 6.40 -7 -3 4 3.60 5.50 -7 -3 4 -6.30 7.70 6 3 -4 109.49 7.50 -6 -3 4 123.29 12.80 -6 -3 4 123.99 11.60 -6 -3 4 113.99 9.40 -6 -3 4 156.48 16.10 5 3 -4 141.99 6.80 -5 -3 4 139.39 14.10 -5 -3 4 130.09 10.30 -5 -3 4 129.59 8.50 -5 -3 4 110.29 10.90 4 3 -4 19.80 2.70 4 3 -4 12.80 4.50 -4 -3 4 15.40 4.60 -4 -3 4 14.90 3.20 -4 -3 4 14.90 5.80 -4 -3 4 20.90 4.40 3 3 -4 174.28 6.80 3 3 -4 168.28 9.30 -3 -3 4 168.98 11.00 -3 -3 4 177.98 10.40 -3 -3 4 177.38 7.60 -3 -3 4 182.28 8.70 2 3 -4 582.34 18.50 -2 -3 4 557.14 20.70 -2 -3 4 563.64 17.30 -2 -3 4 572.04 20.70 -1 -3 4 26.10 3.70 -1 -3 4 37.20 4.30 -1 -3 4 31.30 2.50 0 -3 4 54.09 3.30 0 -3 4 54.49 4.30 0 -3 4 55.09 3.20 0 -3 4 55.99 4.10 -1 3 -4 9.80 1.60 1 -3 4 11.40 2.40 1 -3 4 9.20 1.90 1 -3 4 10.80 2.80 1 -3 4 9.40 1.70 -2 3 -4 249.38 10.60 -2 3 -4 250.77 9.00 2 -3 4 239.78 11.20 2 -3 4 238.98 11.20 2 -3 4 241.28 11.40 2 -3 4 231.98 10.10 -3 3 -4 21.40 3.80 -3 3 -4 23.80 3.80 3 -3 4 26.20 4.90 3 -3 4 17.30 4.10 -4 3 -4 7.80 3.60 -4 3 -4 5.10 1.20 -4 3 -4 3.60 4.20 -4 3 -4 5.60 3.30 4 -3 4 2.70 4.30 4 -3 4 11.20 3.90 4 -3 4 9.40 4.20 4 -3 4 3.70 4.60 -5 3 -4 2.50 2.20 -5 3 -4 7.10 4.90 5 -3 4 4.20 5.50 5 -3 4 4.40 4.40 5 -3 4 3.80 4.90 -6 3 -4 159.98 14.10 -6 3 -4 153.88 7.60 6 -3 4 162.58 14.00 6 -3 4 173.98 13.50 -7 3 -4 114.49 14.80 7 -3 4 119.39 11.60 7 -3 4 133.69 15.30 -8 3 -4 181.38 19.50 -8 3 -4 162.98 10.30 8 -3 4 142.89 15.30 8 -3 4 156.08 16.80 -9 3 -4 76.29 9.40 -9 3 -4 76.79 14.90 9 -3 4 72.99 12.70 -10 3 -4 32.80 14.10 -10 3 -4 13.60 7.70 10 -3 4 8.50 12.30 10 -3 4 5.20 10.70 9 2 -4 8.50 5.50 -9 -2 4 -0.40 9.10 -9 -2 4 4.40 13.00 -9 -2 4 -1.20 8.80 8 2 -4 31.70 5.50 -8 -2 4 27.50 7.80 -8 -2 4 39.50 13.40 7 2 -4 3.00 3.50 -7 -2 4 -0.20 5.70 -7 -2 4 1.20 5.40 -7 -2 4 7.30 6.90 -7 -2 4 2.80 9.20 6 2 -4 268.47 11.90 6 2 -4 276.17 11.30 -6 -2 4 261.87 19.60 -6 -2 4 262.17 14.10 -6 -2 4 267.27 15.90 -6 -2 4 247.48 12.90 5 2 -4 25.40 3.90 -5 -2 4 25.60 5.90 -5 -2 4 22.90 4.80 -5 -2 4 31.00 5.10 -5 -2 4 37.50 7.50 4 2 -4 10.00 4.40 4 2 -4 16.20 2.70 -4 -2 4 18.70 5.90 -4 -2 4 22.60 4.40 -4 -2 4 14.80 3.60 -4 -2 4 20.20 5.40 -4 -2 4 12.00 4.30 3 2 -4 12.30 2.00 3 2 -4 13.10 3.60 -3 -2 4 10.70 2.70 -3 -2 4 9.20 3.40 -3 -2 4 11.30 2.80 -3 -2 4 11.30 3.70 2 2 -4 393.06 12.40 2 2 -4 390.06 13.90 -2 -2 4 398.06 12.70 -2 -2 4 373.16 15.40 -2 -2 4 390.96 12.80 -1 -2 4 4.10 2.20 -1 -2 4 4.60 1.80 -1 -2 4 3.60 1.30 0 -2 4 34.90 3.30 0 -2 4 38.80 2.20 0 -2 4 42.10 3.30 -1 2 -4 174.48 5.90 -1 2 -4 168.08 7.20 1 -2 4 159.08 7.70 1 -2 4 166.48 6.50 -2 2 -4 139.89 6.00 -2 2 -4 146.69 7.30 2 -2 4 137.09 4.80 2 -2 4 143.19 8.00 2 -2 4 139.09 7.00 2 -2 4 134.49 7.80 -3 2 -4 47.00 2.50 -3 2 -4 55.09 5.80 -3 2 -4 57.49 4.80 -3 2 -4 53.89 6.30 3 -2 4 50.49 3.10 3 -2 4 54.49 5.30 3 -2 4 55.59 7.20 3 -2 4 48.60 5.70 3 -2 4 55.29 5.90 -4 2 -4 376.76 15.20 -4 2 -4 346.87 15.20 -4 2 -4 420.16 17.10 4 -2 4 374.66 18.10 4 -2 4 365.96 12.40 4 -2 4 359.06 16.20 4 -2 4 356.16 16.30 4 -2 4 345.57 15.90 -5 2 -4 -3.50 3.90 -5 2 -4 -2.70 2.00 -5 2 -4 0.10 3.70 5 -2 4 1.80 5.10 5 -2 4 -2.10 3.80 5 -2 4 -2.90 2.50 5 -2 4 -6.20 3.30 -6 2 -4 28.70 7.40 -6 2 -4 37.50 5.10 6 -2 4 27.40 7.00 6 -2 4 39.30 8.40 6 -2 4 41.90 5.80 -7 2 -4 75.99 7.00 -7 2 -4 57.59 10.90 7 -2 4 88.29 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5.80 -4 -6 -13 28.60 6.80 -4 -6 -13 32.70 5.00 4 6 13 36.60 7.20 4 6 13 38.30 7.90 -5 -6 -13 7.50 6.10 -5 -6 -13 10.50 3.20 5 6 13 12.30 5.80 5 6 13 10.40 8.70 -6 -6 -13 12.80 3.50 -6 -6 -13 15.90 7.30 6 6 13 -1.50 6.30 6 6 13 -5.10 7.70 2 -7 -13 -12.10 8.80 -2 7 13 10.00 10.30 1 -7 -13 -2.00 7.80 -1 7 13 -2.20 12.40 -1 7 13 -4.70 8.60 0 -7 -13 -5.20 7.70 0 7 13 -0.40 12.60 0 7 13 14.70 6.60 -1 -7 -13 9.10 6.10 1 7 13 24.00 5.70 1 7 13 23.40 13.40 -2 -7 -13 3.20 6.70 -2 -7 -13 4.90 4.70 2 7 13 15.70 7.80 -3 -7 -13 -0.70 3.60 -3 -7 -13 -0.10 6.10 3 7 13 4.60 6.70 -4 -7 -13 -0.90 6.40 4 7 13 4.30 6.50 -5 -7 -13 -5.20 7.10 -5 -7 -13 5.00 3.40 5 7 13 6.00 7.30 5 7 13 3.10 7.00 1 -8 -13 -2.50 8.40 -1 8 13 2.70 7.70 -1 8 13 -6.50 10.10 0 -8 -13 -0.80 8.10 0 8 13 -6.10 9.50 -1 -8 -13 6.50 6.70 1 8 13 30.60 10.10 1 8 13 7.00 6.20 -2 -8 -13 -3.60 5.30 -2 -8 -13 -0.80 6.60 2 8 13 7.60 9.20 -3 -8 -13 6.10 4.70 -3 -8 -13 -11.40 7.60 3 8 13 11.80 10.10 -4 -8 -13 8.40 4.40 -4 -8 -13 2.00 7.60 4 8 13 -1.30 7.50 2 -5 14 -0.60 5.20 2 -5 14 9.20 10.20 2 -5 14 6.40 5.30 -1 -4 14 14.20 8.80 -1 -4 14 12.00 9.40 -1 -4 14 16.00 9.20 0 -4 14 10.90 7.70 0 -4 14 -0.90 6.90 0 -4 14 -10.50 7.40 1 -4 14 -1.20 7.30 1 -4 14 -3.00 8.40 1 -4 14 4.70 5.30 1 -4 14 4.50 5.90 2 -4 14 32.10 10.00 2 -4 14 17.50 6.80 2 -4 14 1.50 5.10 3 -4 14 -8.70 5.10 3 -4 14 -5.40 9.90 4 -4 14 7.50 6.00 4 -4 14 -4.90 12.00 5 -4 14 -7.20 6.20 5 -4 14 -9.20 11.00 -2 -3 14 8.40 7.50 -2 -3 14 3.00 7.70 -2 -3 14 2.30 8.80 -1 -3 14 10.30 8.50 -1 -3 14 9.40 6.10 -1 -3 14 -5.40 6.70 0 -3 14 4.20 6.00 0 -3 14 -8.50 7.00 0 -3 14 18.80 5.90 0 -3 14 6.10 7.20 1 -3 14 -4.70 4.30 1 -3 14 -5.00 4.80 1 -3 14 -12.80 13.90 2 -3 14 -7.20 8.00 2 -3 14 3.70 7.70 3 -3 14 5.40 9.10 3 -3 14 6.00 5.10 4 -3 14 31.10 7.00 4 -3 14 27.00 11.10 5 -3 14 -8.30 5.80 6 -3 14 -7.60 10.00 -3 -2 14 -9.60 6.40 -3 -2 14 0.30 8.30 -3 -2 14 -2.20 9.30 -2 -2 14 2.50 6.90 -2 -2 14 5.30 8.20 -2 -2 14 3.00 6.70 -1 -2 14 6.30 5.30 0 -2 14 21.70 6.20 0 -2 14 9.10 5.60 0 -2 14 18.50 6.70 1 -2 14 0.10 4.20 1 -2 14 0.90 6.90 1 -2 14 5.30 5.00 2 -2 14 13.90 5.50 2 -2 14 0.40 7.10 3 -2 14 -4.10 7.90 3 -2 14 1.40 6.90 4 -2 14 61.29 12.00 4 -2 14 73.99 12.50 5 -2 14 9.50 10.50 5 -2 14 20.30 6.40 6 -2 14 75.19 14.40 6 -2 14 88.09 12.10 7 -2 14 -3.60 11.40 -3 -1 14 4.70 8.10 -3 -1 14 4.20 7.10 -3 -1 14 -0.30 8.00 -2 -1 14 -11.70 6.10 -1 -1 14 4.70 5.30 0 -1 14 38.00 6.90 0 -1 14 22.50 5.50 1 -1 14 18.90 5.50 1 -1 14 20.00 7.10 2 -1 14 19.50 5.20 2 -1 14 16.60 8.00 3 -1 14 11.50 7.80 3 -1 14 7.90 4.70 4 -1 14 5.50 8.30 4 -1 14 8.90 4.60 5 -1 14 -1.30 4.70 5 -1 14 3.40 9.20 6 -1 14 19.90 7.30 7 -1 14 -4.60 11.20 -4 0 14 11.30 9.40 -4 0 14 5.60 9.60 -4 0 14 -2.10 8.90 -3 0 14 -1.40 7.10 -3 0 14 -5.40 8.30 -2 0 14 6.10 7.20 -1 0 14 -5.50 5.10 0 0 14 1.90 4.60 0 0 14 2.00 4.40 0 0 14 4.20 4.40 1 0 14 6.70 5.60 1 0 14 9.50 5.10 2 0 14 37.10 7.80 2 0 14 32.40 5.80 3 0 14 187.18 15.30 3 0 14 168.38 11.80 4 0 14 3.60 7.50 5 0 14 18.20 5.50 5 0 14 11.20 9.40 6 0 14 3.20 5.60 6 0 14 -3.00 9.50 -7 0 -14 15.30 7.50 7 0 14 6.00 11.30 -4 1 14 12.30 10.10 -4 1 14 11.30 9.30 -3 1 14 5.50 7.70 -3 1 14 2.80 7.60 -2 1 14 6.80 5.60 -1 1 14 49.80 8.10 0 1 14 6.10 4.80 0 1 14 1.40 3.50 0 1 14 -0.80 4.90 1 1 14 52.59 6.90 1 1 14 46.50 7.30 2 1 14 88.69 10.50 2 1 14 93.29 9.40 3 1 14 29.40 8.20 3 1 14 39.70 6.20 4 1 14 33.70 8.50 4 1 14 22.30 5.40 5 1 14 51.39 9.10 5 1 14 79.19 12.40 -6 -1 -14 -1.50 6.30 6 1 14 -7.70 5.20 6 1 14 6.70 9.30 -7 -1 -14 9.10 7.00 7 1 14 -2.70 6.20 7 1 14 15.30 11.50 8 1 14 -4.70 6.30 -4 2 14 17.60 10.60 -4 2 14 2.00 9.00 -3 2 14 15.40 8.20 -3 2 14 -8.60 8.20 -2 2 14 -4.60 5.90 -2 2 14 14.50 6.50 -1 2 14 12.80 6.90 0 2 14 2.10 5.20 0 2 14 5.40 4.20 0 2 14 2.90 3.00 1 2 14 26.40 5.40 1 2 14 30.00 6.20 2 2 14 142.99 10.70 2 2 14 123.89 10.60 3 2 14 15.50 5.10 3 2 14 17.10 6.60 4 2 14 18.30 7.50 4 2 14 19.50 5.40 -5 -2 -14 59.99 8.70 5 2 14 75.79 12.20 -6 -2 -14 1.90 6.80 6 2 14 3.30 5.30 6 2 14 9.40 10.10 -7 -2 -14 -1.60 7.00 7 2 14 -2.30 5.90 7 2 14 9.40 10.10 -4 3 14 15.30 10.20 -4 3 14 -15.50 7.60 -3 3 14 -2.00 7.80 -3 3 14 17.10 8.50 -2 3 14 -4.00 6.10 -2 3 14 -6.10 7.10 -1 3 14 -7.50 5.90 -1 3 14 -4.80 4.90 0 3 14 6.10 5.40 0 3 14 7.30 9.20 1 3 14 2.10 5.30 1 3 14 -2.00 3.90 2 3 14 6.50 4.90 2 3 14 7.70 4.70 3 3 14 1.20 4.90 3 3 14 2.60 5.70 -4 -3 -14 5.10 5.90 4 3 14 4.10 5.60 4 3 14 16.60 7.20 -5 -3 -14 -1.80 6.50 5 3 14 1.20 9.00 -6 -3 -14 -6.50 9.40 6 3 14 -4.30 14.10 6 3 14 3.80 5.30 -7 -3 -14 22.30 7.60 7 3 14 11.70 10.40 7 3 14 8.50 5.80 -3 4 14 0.20 9.40 -3 4 14 7.20 8.60 -2 4 14 14.80 9.20 -2 4 14 23.50 8.60 -1 4 14 -3.10 6.60 -1 4 14 6.90 5.90 0 4 14 34.50 7.30 1 4 14 26.80 7.90 2 4 14 22.70 5.70 2 4 14 23.90 6.60 3 4 14 10.70 6.00 3 4 14 9.10 5.60 4 4 14 3.70 5.60 4 4 14 -3.30 5.90 -5 -4 -14 12.30 7.00 5 4 14 -1.40 7.10 -6 -4 -14 9.10 7.40 6 4 14 16.30 8.70 6 4 14 -1.30 5.80 -7 -4 -14 -4.50 8.20 7 4 14 5.90 6.80 7 4 14 5.70 9.00 -3 5 14 1.30 9.30 -3 5 14 -9.90 9.40 -2 5 14 5.60 8.80 -2 5 14 -2.30 7.60 -1 5 14 4.70 6.40 -1 5 14 7.40 7.50 0 5 14 4.60 7.00 0 5 14 8.40 5.40 1 5 14 3.00 6.60 -3 -5 -14 2.70 6.50 3 5 14 4.50 6.10 3 5 14 -0.70 5.50 -4 -5 -14 2.90 6.10 4 5 14 8.80 6.30 4 5 14 -4.30 6.20 -5 -5 -14 0.00 6.60 5 5 14 -2.30 6.90 -6 -5 -14 6.10 7.50 6 5 14 -15.20 7.30 6 5 14 -10.40 5.60 -2 6 14 -6.50 8.40 -2 6 14 3.40 9.50 -1 6 14 10.20 7.90 -1 6 14 4.30 9.10 0 6 14 -0.80 5.80 0 6 14 2.30 8.20 1 6 14 7.50 5.50 1 6 14 11.90 7.40 2 6 14 20.50 7.40 -3 -6 -14 1.00 6.80 3 6 14 7.10 10.10 -4 -6 -14 -4.10 6.80 4 6 14 10.10 6.20 -5 -6 -14 3.70 7.90 5 6 14 -0.10 7.40 5 6 14 4.10 7.30 -1 7 14 -23.20 9.70 -1 7 14 8.20 9.20 0 7 14 20.20 9.40 0 7 14 4.60 6.90 1 7 14 -1.00 5.00 1 7 14 -2.80 7.90 2 7 14 1.00 8.00 -3 -7 -14 -10.50 6.30 3 7 14 -4.70 7.50 -4 -7 -14 9.20 8.20 4 7 14 -1.70 7.30 0 -3 15 16.60 7.20 0 -3 15 16.40 6.50 0 -3 15 6.30 8.70 1 -3 15 1.90 5.60 1 -3 15 10.30 9.40 1 -3 15 -0.70 5.40 2 -3 15 0.40 5.00 2 -3 15 10.10 10.10 3 -3 15 18.40 11.10 3 -3 15 18.00 6.40 4 -3 15 31.80 11.70 4 -3 15 16.90 6.60 -1 -2 15 10.40 8.40 -1 -2 15 -5.20 5.90 0 -2 15 -4.30 6.10 0 -2 15 -3.50 4.90 1 -2 15 9.90 5.20 1 -2 15 7.10 7.30 1 -2 15 -0.60 7.50 2 -2 15 -8.10 4.80 2 -2 15 13.10 9.20 3 -2 15 4.10 9.10 3 -2 15 -1.50 5.20 4 -2 15 23.50 11.10 4 -2 15 12.40 5.60 5 -2 15 -6.70 5.80 6 -2 15 87.79 12.40 -2 -1 15 22.70 9.90 -2 -1 15 7.00 6.80 -1 -1 15 3.20 6.00 -1 -1 15 -9.20 6.30 0 -1 15 1.50 5.50 0 -1 15 -9.10 4.90 1 -1 15 17.00 7.70 1 -1 15 21.20 6.20 1 -1 15 21.50 6.10 2 -1 15 63.99 10.80 2 -1 15 58.79 8.80 3 -1 15 9.90 8.50 3 -1 15 14.80 5.60 4 -1 15 60.99 8.50 4 -1 15 64.29 11.00 5 -1 15 28.30 7.40 5 -1 15 32.10 10.30 6 -1 15 -6.10 6.40 6 -1 15 14.80 11.90 -2 0 15 -11.10 7.10 -2 0 15 1.60 6.80 -1 0 15 9.60 7.40 -1 0 15 4.80 5.90 0 0 15 9.30 5.70 0 0 15 13.50 5.60 1 0 15 23.50 6.50 1 0 15 8.00 6.60 2 0 15 0.60 5.50 2 0 15 14.20 7.70 3 0 15 0.90 7.90 3 0 15 -6.40 5.10 4 0 15 -1.20 4.40 4 0 15 7.00 8.60 5 0 15 -8.70 9.40 5 0 15 16.10 6.20 6 0 15 -4.00 9.60 6 0 15 5.10 6.30 -3 1 15 7.40 9.80 -3 1 15 6.20 8.10 -2 1 15 -4.00 6.90 -2 1 15 8.60 8.30 -1 1 15 -2.80 6.10 -1 1 15 -9.80 5.50 0 1 15 14.10 5.90 0 1 15 6.00 5.30 1 1 15 23.60 6.20 1 1 15 22.20 5.80 2 1 15 2.00 6.20 3 1 15 15.70 5.80 3 1 15 11.20 7.50 4 1 15 0.40 8.30 4 1 15 -4.60 4.90 5 1 15 9.00 4.70 5 1 15 -3.50 8.70 6 1 15 1.30 10.30 6 1 15 7.80 6.40 -7 -1 -15 -7.80 7.80 7 1 15 3.40 10.50 7 1 15 0.40 6.70 -3 2 15 8.90 9.50 -3 2 15 -8.40 8.50 -2 2 15 6.30 7.80 -2 2 15 22.40 7.70 -1 2 15 0.90 6.60 -1 2 15 7.60 6.60 0 2 15 -9.30 5.70 0 2 15 -2.30 5.00 1 2 15 11.60 5.60 1 2 15 5.00 5.00 2 2 15 37.50 7.30 2 2 15 23.20 5.90 3 2 15 -9.70 5.20 4 2 15 61.99 10.40 4 2 15 69.59 9.10 5 2 15 12.70 9.40 5 2 15 0.80 5.90 -6 -2 -15 5.70 8.30 6 2 15 3.40 5.20 6 2 15 4.10 8.70 -7 -2 -15 15.00 8.30 7 2 15 -0.60 10.20 7 2 15 2.60 6.70 -3 3 15 4.50 9.90 -3 3 15 7.10 9.20 -2 3 15 -4.20 8.00 -2 3 15 -0.70 7.80 -1 3 15 35.10 8.70 -1 3 15 7.30 7.40 0 3 15 1.40 5.30 0 3 15 -8.20 4.90 1 3 15 5.20 4.20 1 3 15 -8.10 5.00 2 3 15 -7.80 4.90 2 3 15 2.00 4.90 3 3 15 7.50 6.30 3 3 15 8.80 6.50 4 3 15 -2.90 5.30 4 3 15 -9.60 6.30 -5 -3 -15 7.50 6.70 5 3 15 11.10 5.80 5 3 15 -0.40 8.10 -6 -3 -15 12.00 7.20 6 3 15 -15.90 7.80 6 3 15 -1.10 5.90 -2 4 15 29.40 10.10 -2 4 15 17.00 9.90 -1 4 15 5.60 6.50 -1 4 15 10.30 7.10 0 4 15 22.30 7.20 0 4 15 24.70 6.80 1 4 15 -1.70 6.20 2 4 15 -3.40 5.20 2 4 15 -1.20 5.30 3 4 15 23.80 7.30 3 4 15 11.90 5.80 4 4 15 -12.20 5.80 4 4 15 4.80 6.70 -5 -4 -15 -10.90 7.70 5 4 15 -14.00 5.50 5 4 15 12.70 8.30 -6 -4 -15 29.80 8.90 6 4 15 16.60 7.00 6 4 15 13.40 9.00 -2 5 15 -8.80 8.40 -2 5 15 3.20 9.80 -1 5 15 13.70 8.30 -1 5 15 0.40 7.40 0 5 15 13.40 6.50 0 5 15 1.50 8.10 1 5 15 2.10 7.20 1 5 15 16.00 5.90 2 5 15 1.70 6.60 3 5 15 0.60 6.40 3 5 15 10.20 6.50 -4 -5 -15 -10.20 6.70 4 5 15 -3.40 6.30 4 5 15 -0.30 7.00 -5 -5 -15 11.60 7.00 5 5 15 -1.50 6.60 5 5 15 -10.30 7.40 0 6 15 2.70 9.50 0 6 15 19.00 7.60 1 6 15 1.90 5.50 1 6 15 1.00 7.90 2 6 15 -1.40 7.30 3 6 15 4.50 7.70 -4 -6 -15 9.10 8.60 4 6 15 -9.60 10.30 4 6 15 5.90 7.20 1 -2 16 21.50 7.20 1 -2 16 30.90 7.60 2 -2 16 8.30 9.70 2 -2 16 5.00 6.30 3 -2 16 3.10 6.40 3 -2 16 9.60 10.20 0 -1 16 12.70 7.10 0 -1 16 -7.10 11.60 1 -1 16 -3.40 6.00 1 -1 16 10.50 5.90 2 -1 16 -6.00 8.00 2 -1 16 1.50 6.00 3 -1 16 13.60 9.10 3 -1 16 13.80 6.70 4 -1 16 5.10 6.10 4 -1 16 -5.80 9.20 5 -1 16 -9.50 13.40 5 -1 16 -1.50 5.80 -1 0 16 11.00 8.00 -1 0 16 -8.60 7.40 0 0 16 9.30 6.90 0 0 16 4.70 6.50 1 0 16 -8.00 5.40 2 0 16 40.40 7.30 2 0 16 30.80 7.80 3 0 16 9.20 9.10 3 0 16 1.70 5.50 4 0 16 21.60 10.30 4 0 16 29.20 7.80 5 0 16 7.80 6.80 5 0 16 2.90 11.10 -1 1 16 9.10 7.20 -1 1 16 26.90 9.40 0 1 16 -5.00 5.80 0 1 16 -2.00 6.10 1 1 16 -2.80 6.00 1 1 16 1.30 5.10 2 1 16 13.20 6.50 2 1 16 10.20 7.10 3 1 16 4.50 5.50 3 1 16 5.10 7.60 4 1 16 9.90 9.40 4 1 16 5.40 6.30 5 1 16 0.30 6.20 5 1 16 -1.80 8.60 -1 2 16 19.20 9.00 -1 2 16 8.00 7.70 0 2 16 10.00 7.10 0 2 16 4.60 6.30 1 2 16 33.40 7.60 1 2 16 33.10 7.50 2 2 16 -4.90 5.80 2 2 16 4.10 6.30 3 2 16 19.90 6.40 3 2 16 20.50 7.70 4 2 16 14.70 9.50 4 2 16 8.30 5.90 5 2 16 -17.00 8.60 5 2 16 -14.80 6.50 -1 3 16 9.70 8.60 -1 3 16 -7.60 6.70 0 3 16 29.30 7.90 0 3 16 28.20 8.60 1 3 16 35.90 8.40 1 3 16 30.60 8.00 1 3 16 23.10 7.10 2 3 16 3.30 6.30 2 3 16 18.50 6.50 3 3 16 3.40 6.40 3 3 16 -8.10 5.70 4 3 16 -0.20 5.40 4 3 16 9.10 8.40 5 3 16 6.40 7.30 5 3 16 11.60 10.00 -1 4 16 8.50 7.80 0 4 16 29.80 8.90 0 4 16 22.00 7.90 1 4 16 36.30 9.00 1 4 16 38.90 7.70 2 4 16 24.70 7.70 2 4 16 22.80 6.50 3 4 16 4.30 6.80 3 4 16 25.00 7.90 4 4 16 -6.50 6.30 4 4 16 13.80 8.30 5 4 16 18.70 7.20 1 5 16 36.50 9.60 1 5 16 44.90 8.10 2 5 16 6.00 8.00 3 5 16 -7.60 6.50 3 5 16 -8.00 7.30 2 1 17 -10.20 6.30 3 1 17 -0.10 6.60 2 2 17 -11.00 6.60 3 2 17 22.40 7.50 3 2 17 9.80 7.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 51824 _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 O4 O 0.4147(3) 0.3039(3) 0.5582(2) 0.0343(8) Uani 1 1 d . . . . . O2 O 0.4310(3) 0.9913(3) 0.2703(2) 0.0365(8) Uani 1 1 d . . . . . O3 O 0.0896(3) 0.6343(3) 0.4161(2) 0.0433(9) Uani 1 1 d . . . . . N1 N 0.3037(4) 0.7494(3) 0.4063(2) 0.0274(9) Uani 1 1 d . . . . . H1 H 0.396968 0.741830 0.399674 0.033 Uiso 1 1 calc R . . . . N2 N 0.2174(3) 0.4238(3) 0.5317(2) 0.0260(8) Uani 1 1 d . . . . . H2 H 0.127859 0.443536 0.552815 0.031 Uiso 1 1 calc R . . . . O1 O 0.3347(4) 0.9509(4) 0.1440(2) 0.0574(11) Uani 1 1 d . . . . . C16 C 0.2948(4) 0.4938(4) 0.4390(3) 0.0261(10) Uani 1 1 d . . . . . H16 H 0.396850 0.512218 0.441879 0.031 Uiso 1 1 calc R . . . . C15 C 0.2211(4) 0.6336(4) 0.4192(3) 0.0285(10) Uani 1 1 d . . . . . C24 C 0.2845(4) 0.3294(4) 0.5840(3) 0.0236(9) Uani 1 1 d . . . . . C6 C 0.2422(5) 0.8891(4) 0.4031(3) 0.0286(10) Uani 1 1 d . . . . . H6 H 0.135537 0.877658 0.422776 0.034 Uiso 1 1 calc R . . . . C5 C 0.2770(5) 0.9728(5) 0.3039(3) 0.0326(11) Uani 1 1 d . . . . . H5 H 0.232713 1.065356 0.305339 0.039 Uiso 1 1 calc R . . . . C3 C 0.4576(5) 1.0114(4) 0.1690(3) 0.0342(11) Uani 1 1 d . . . . . C7 C 0.2966(5) 0.9682(5) 0.4740(3) 0.0357(11) Uani 1 1 d D . . . . H7A H 0.247614 1.057354 0.475383 0.043 Uiso 1 1 calc R . . . . H7B H 0.400661 0.988773 0.451726 0.043 Uiso 1 1 calc R . . . . C25 C 0.1928(5) 0.2578(5) 0.6757(3) 0.0349(11) Uani 1 1 d . . . . . H25A H 0.194092 0.157662 0.676475 0.052 Uiso 1 1 calc GR . . . . H25B H 0.093881 0.288797 0.681318 0.052 Uiso 1 1 calc GR . . . . H25C H 0.231529 0.281038 0.727986 0.052 Uiso 1 1 calc GR . . . . C17 C 0.2914(5) 0.4019(5) 0.3626(3) 0.0350(11) Uani 1 1 d . . . . . H17A H 0.322053 0.308040 0.383712 0.042 Uiso 1 1 calc R . . . . H17B H 0.191780 0.394164 0.353524 0.042 Uiso 1 1 calc R . . . . C18 C 0.3898(5) 0.4607(4) 0.2693(3) 0.0337(11) Uani 1 1 d . . . . . C20 C 0.3327(6) 0.5234(5) 0.1925(3) 0.0408(12) Uani 1 1 d . . . . . H20 H 0.231803 0.528615 0.198171 0.049 Uiso 1 1 calc R . . . . C19 C 0.5395(6) 0.4555(5) 0.2588(3) 0.0423(12) Uani 1 1 d . . . . . H19 H 0.579316 0.414752 0.309695 0.051 Uiso 1 1 calc R . . . . C4 C 0.2305(5) 0.9039(5) 0.2270(3) 0.0407(12) Uani 1 1 d . . . . . H4A H 0.230293 0.802105 0.242300 0.049 Uiso 1 1 calc R . . . . H4B H 0.133231 0.932333 0.219452 0.049 Uiso 1 1 calc R . . . . C21 C 0.4251(7) 0.5778(5) 0.1080(3) 0.0524(15) Uani 1 1 d . . . . . H21 H 0.386051 0.619965 0.057116 0.063 Uiso 1 1 calc R . . . . C23 C 0.5734(7) 0.5703(5) 0.0985(4) 0.0539(15) Uani 1 1 d . . . . . H23 H 0.634804 0.606147 0.041028 0.065 Uiso 1 1 calc R . . . . C2 C 0.4678(7) 1.1656(5) 0.1291(4) 0.0557(16) Uani 1 1 d . . . . . H2A H 0.379393 1.209923 0.154952 0.084 Uiso 1 1 calc GR . . . . H2B H 0.480875 1.176458 0.061155 0.084 Uiso 1 1 calc GR . . . . H2C H 0.549672 1.208697 0.145775 0.084 Uiso 1 1 calc GR . . . . C22 C 0.6321(6) 0.5096(5) 0.1738(4) 0.0515(14) Uani 1 1 d . . . . . H22 H 0.733096 0.505079 0.167767 0.062 Uiso 1 1 calc R . . . . C8 C 0.2707(6) 0.8875(6) 0.5755(3) 0.0533(15) Uani 1 1 d D . . . . H8A H 0.323333 0.800293 0.574136 0.064 Uiso 1 1 calc R . . . . H8B H 0.312344 0.942979 0.614658 0.064 Uiso 1 1 calc R . . . . C1 C 0.5942(6) 0.9347(6) 0.1343(4) 0.0534(14) Uani 1 1 d . . . . . H1A H 0.674776 0.972029 0.155678 0.080 Uiso 1 1 calc GR . . . . H1B H 0.614956 0.946793 0.066086 0.080 Uiso 1 1 calc GR . . . . H1C H 0.579969 0.836246 0.159000 0.080 Uiso 1 1 calc GR . . . . C9 C 0.1140(8) 0.8530(6) 0.6215(4) 0.079(2) Uani 1 1 d D . . . . H9A H 0.073967 0.811414 0.574977 0.094 Uiso 1 1 calc R . . . . H9B H 0.068468 0.943537 0.624895 0.094 Uiso 1 1 calc R . . . . C12 C 0.0204(7) 0.7335(8) 0.8899(4) 0.077(2) Uani 1 1 d D . . . . H12A H -0.084334 0.730839 0.892732 0.093 Uiso 1 1 calc R . . . . H12B H 0.052279 0.637299 0.900089 0.093 Uiso 1 1 calc R . . . . C14 C -0.0013(8) 0.7455(9) 1.0639(4) 0.091(3) Uani 1 1 d D . . . . H14A H -0.104895 0.757144 1.082349 0.137 Uiso 1 1 calc GR . . . . H14B H 0.048572 0.794630 1.101641 0.137 Uiso 1 1 calc GR . . . . H14C H 0.019862 0.647220 1.073688 0.137 Uiso 1 1 calc GR . . . . C11 C 0.1098(7) 0.8161(7) 0.7781(6) 0.104(3) Uani 1 1 d D . . . . H11A H 0.096061 0.916986 0.770652 0.125 Uiso 1 1 calc R . . . . H11B H 0.213694 0.797812 0.766364 0.125 Uiso 1 1 calc R . . . . C10 C 0.0447(10) 0.7571(8) 0.7232(9) 0.222(9) Uani 1 1 d D . . . . H10A H -0.060830 0.764501 0.740131 0.267 Uiso 1 1 calc R . . . . H10B H 0.069518 0.658878 0.723450 0.267 Uiso 1 1 calc R . . . . C13 C 0.0497(15) 0.8043(9) 0.9609(5) 0.187(7) Uani 1 1 d D . . . . H13A H 0.009161 0.897185 0.951363 0.224 Uiso 1 1 calc R . . . . H13B H 0.155112 0.817714 0.949749 0.224 Uiso 1 1 calc R . . . . 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 O4 0.0187(17) 0.0366(18) 0.0459(19) 0.0062(14) -0.0115(14) 0.0010(13) O2 0.0394(19) 0.0425(19) 0.0253(16) 0.0060(13) -0.0088(14) -0.0141(15) O3 0.0174(17) 0.0402(19) 0.066(2) 0.0193(16) -0.0135(15) -0.0059(14) N1 0.0118(17) 0.027(2) 0.039(2) 0.0083(16) -0.0052(15) 0.0004(15) N2 0.0143(17) 0.0299(19) 0.030(2) 0.0083(15) -0.0041(15) -0.0001(15) O1 0.063(3) 0.080(3) 0.033(2) -0.0026(18) -0.0213(18) -0.025(2) C16 0.017(2) 0.026(2) 0.032(2) 0.0060(18) -0.0062(18) -0.0037(17) C15 0.019(2) 0.034(3) 0.028(2) 0.0078(18) -0.0046(18) -0.0028(19) C24 0.021(2) 0.023(2) 0.029(2) 0.0000(18) -0.0110(19) -0.0016(18) C6 0.020(2) 0.028(2) 0.035(3) 0.0060(19) -0.0039(19) 0.0027(18) C5 0.034(3) 0.028(2) 0.037(3) 0.0042(19) -0.015(2) 0.000(2) C3 0.051(3) 0.027(2) 0.025(2) 0.0010(18) -0.012(2) -0.007(2) C7 0.033(3) 0.038(3) 0.033(3) 0.002(2) -0.006(2) 0.003(2) C25 0.033(3) 0.040(3) 0.029(2) 0.006(2) -0.009(2) -0.002(2) C17 0.038(3) 0.030(2) 0.036(3) 0.005(2) -0.012(2) -0.009(2) C18 0.045(3) 0.025(2) 0.032(3) -0.0027(19) -0.012(2) -0.006(2) C20 0.060(3) 0.031(3) 0.034(3) -0.004(2) -0.017(3) -0.002(2) C19 0.047(3) 0.037(3) 0.040(3) 0.001(2) -0.008(2) -0.003(2) C4 0.039(3) 0.041(3) 0.045(3) 0.001(2) -0.022(2) -0.001(2) C21 0.093(5) 0.034(3) 0.030(3) 0.000(2) -0.014(3) -0.005(3) C23 0.081(5) 0.036(3) 0.036(3) -0.004(2) 0.007(3) -0.013(3) C2 0.095(5) 0.032(3) 0.036(3) 0.006(2) -0.011(3) -0.001(3) C22 0.053(3) 0.042(3) 0.052(3) -0.008(3) 0.008(3) -0.008(3) C8 0.068(4) 0.057(3) 0.028(3) 0.000(2) -0.001(3) 0.032(3) C1 0.069(4) 0.049(3) 0.048(3) -0.013(3) -0.020(3) 0.006(3) C9 0.111(6) 0.042(3) 0.052(4) 0.006(3) 0.046(4) -0.008(4) C12 0.071(4) 0.137(6) 0.027(3) -0.027(4) -0.009(3) 0.042(4) C14 0.097(6) 0.139(7) 0.035(3) -0.017(4) -0.005(3) -0.043(5) C11 0.070(5) 0.046(4) 0.207(9) 0.025(5) -0.087(6) -0.010(3) C10 0.133(9) 0.069(6) 0.55(3) -0.118(11) -0.222(14) 0.041(6) C13 0.365(18) 0.105(7) 0.043(5) -0.020(4) 0.075(7) -0.091(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C5 O2 C3 107.2(3) . . ? C15 N1 H1 118.8 . . ? C15 N1 C6 122.3(3) . . ? C6 N1 H1 118.8 . . ? C16 N2 H2 119.8 . . ? C24 N2 H2 119.8 . . ? C24 N2 C16 120.5(3) . . ? C4 O1 C3 109.2(3) . . ? N2 C16 H16 109.0 . . ? N2 C16 C15 107.0(3) . . ? N2 C16 C17 110.8(3) . . ? C15 C16 H16 109.0 . . ? C17 C16 H16 109.0 . . ? C17 C16 C15 111.9(3) . . ? O3 C15 N1 123.4(4) . . ? O3 C15 C16 119.6(4) . . ? N1 C15 C16 117.0(3) . . ? O4 C24 N2 121.5(4) . . ? O4 C24 C25 122.3(4) . . ? N2 C24 C25 116.2(4) . . ? N1 C6 H6 107.9 . . ? N1 C6 C5 112.3(4) . . ? N1 C6 C7 109.7(3) . . ? C5 C6 H6 107.9 . . ? C5 C6 C7 110.9(3) . . ? C7 C6 H6 107.9 . . ? O2 C5 C6 110.8(3) . . ? O2 C5 H5 109.2 . . ? O2 C5 C4 102.5(4) . . ? C6 C5 H5 109.2 . . ? C6 C5 C4 115.8(4) . . ? C4 C5 H5 109.2 . . ? O2 C3 C2 110.9(4) . . ? O2 C3 C1 107.7(4) . . ? O1 C3 O2 106.6(3) . . ? O1 C3 C2 108.1(4) . . ? O1 C3 C1 110.4(4) . . ? C1 C3 C2 112.9(4) . . ? C6 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? C6 C7 C8 114.0(4) . . ? H7A C7 H7B 107.6 . . ? C8 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C16 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C18 C17 C16 112.0(3) . . ? C18 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? C20 C18 C17 121.3(4) . . ? C19 C18 C17 120.3(4) . . ? C19 C18 C20 118.4(4) . . ? C18 C20 H20 119.9 . . ? C21 C20 C18 120.3(5) . . ? C21 C20 H20 119.9 . . ? C18 C19 H19 119.4 . . ? C18 C19 C22 121.3(5) . . ? C22 C19 H19 119.4 . . ? O1 C4 C5 105.0(4) . . ? O1 C4 H4A 110.7 . . ? O1 C4 H4B 110.7 . . ? C5 C4 H4A 110.7 . . ? C5 C4 H4B 110.7 . . ? H4A C4 H4B 108.8 . . ? C20 C21 H21 119.7 . . ? C23 C21 C20 120.6(5) . . ? C23 C21 H21 119.7 . . ? C21 C23 H23 120.0 . . ? C21 C23 C22 120.1(5) . . ? C22 C23 H23 120.0 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C19 C22 H22 120.3 . . ? C23 C22 C19 119.4(5) . . ? C23 C22 H22 120.3 . . ? C7 C8 H8A 108.5 . . ? C7 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C9 C8 C7 115.3(5) . . ? C9 C8 H8A 108.5 . . ? C9 C8 H8B 108.5 . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C8 C9 H9A 104.9 . . ? C8 C9 H9B 104.9 . . ? C8 C9 C10 129.5(6) . . ? H9A C9 H9B 105.8 . . ? C10 C9 H9A 104.9 . . ? C10 C9 H9B 104.9 . . ? H12A C12 H12B 108.0 . . ? C11 C12 H12A 109.4 . . ? C11 C12 H12B 109.5 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.4 . . ? C13 C12 C11 110.9(6) . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? C12 C11 H11A 111.5 . . ? C12 C11 H11B 111.5 . . ? H11A C11 H11B 109.3 . . ? C10 C11 C12 101.4(7) . . ? C10 C11 H11A 111.5 . . ? C10 C11 H11B 111.5 . . ? C9 C10 H10A 111.8 . . ? C9 C10 H10B 111.8 . . ? C11 C10 C9 99.7(7) . . ? C11 C10 H10A 111.8 . . ? C11 C10 H10B 111.8 . . ? H10A C10 H10B 109.6 . . ? C12 C13 C14 121.2(7) . . ? C12 C13 H13A 107.0 . . ? C12 C13 H13B 107.0 . . ? C14 C13 H13A 107.0 . . ? C14 C13 H13B 107.0 . . ? H13A C13 H13B 106.8 . . ? 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 O4 C24 1.231(5) . ? O2 C5 1.423(5) . ? O2 C3 1.427(5) . ? O3 C15 1.237(5) . ? N1 H1 0.8600 . ? N1 C15 1.324(5) . ? N1 C6 1.456(5) . ? N2 H2 0.8600 . ? N2 C16 1.458(5) . ? N2 C24 1.335(5) . ? O1 C3 1.421(5) . ? O1 C4 1.403(6) . ? C16 H16 0.9800 . ? C16 C15 1.523(6) . ? C16 C17 1.522(6) . ? C24 C25 1.499(6) . ? C6 H6 0.9800 . ? C6 C5 1.516(6) . ? C6 C7 1.531(6) . ? C5 H5 0.9800 . ? C5 C4 1.515(6) . ? C3 C2 1.505(6) . ? C3 C1 1.504(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.535(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C18 1.507(6) . ? C18 C20 1.391(6) . ? C18 C19 1.376(7) . ? C20 H20 0.9300 . ? C20 C21 1.382(7) . ? C19 H19 0.9300 . ? C19 C22 1.385(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C21 H21 0.9300 . ? C21 C23 1.365(8) . ? C23 H23 0.9300 . ? C23 C22 1.377(8) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C22 H22 0.9300 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C9 1.495(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C10 1.632(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C11 1.742(8) . ? C12 C13 1.387(10) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C14 C13 1.500(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C10 1.288(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ?