#------------------------------------------------------------------------------ #$Date: 2020-05-07 19:55:00 +0300 (Thu, 07 May 2020) $ #$Revision: 251868 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/83/4038336.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_4038336 loop_ _publ_author_name 'Schmidt, Elena Yu' 'Tatarinova, Inna V.' 'Ushakov, Igor A.' 'Vashchenko, Alexander Valentine' 'Trofimov, Boris A.' _publ_section_title ; Oxaazabicyclooctene Oxides, Another Type of Bridgehead Nitrones: Diastereoselective Assembly from Acetylene gas, Ketones and Hydroxyl Amine. ; _journal_name_full 'The Journal of organic chemistry' _journal_paper_doi 10.1021/acs.joc.0c00742 _journal_year 2020 _chemical_formula_moiety '2(C25 H23 N O2), H2 O' _chemical_formula_sum 'C50 H48 N2 O5' _chemical_formula_weight 756.90 _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 mixed _atom_sites_solution_primary dual _audit_creation_date 2019-06-05 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-06-05 # Formatted by publCIF ; _cell_angle_alpha 102.72(2) _cell_angle_beta 92.22(4) _cell_angle_gamma 109.91(3) _cell_formula_units_Z 2 _cell_length_a 10.384(8) _cell_length_b 10.986(8) _cell_length_c 19.425(14) _cell_measurement_reflns_used 871 _cell_measurement_temperature 293 _cell_measurement_theta_max 24.5 _cell_measurement_theta_min 2.5 _cell_volume 2017(3) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.910 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\w and \f' _diffrn_radiation_monochromator No _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_unetI/netI 0.0478 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.910 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 71221 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.910 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.170 _diffrn_reflns_theta_min 2.166 _diffrn_source IuS _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0970 before and 0.0566 after correction. The Ratio of minimum to maximum transmission is 0.9222. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.246 _exptl_crystal_description prism _exptl_crystal_F_000 804 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.187 _exptl_crystal_size_min 0.123 _refine_diff_density_max 0.187 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.041 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 519 _refine_ls_number_reflns 8164 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.1074 _refine_ls_R_factor_gt 0.0539 _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^)+(0.0476P)^2^+0.7664P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1121 _refine_ls_wR_factor_ref 0.1309 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5200 _reflns_number_total 8164 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo0c00742_si_002.cif _cod_data_source_block a_a _cod_database_code 4038336 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.990 _shelx_estimated_absorpt_t_min 0.985 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2.a Free rotating group: O5(H5A,H5B) 2.b Ternary CH refined with riding coordinates: C12(H12), C40(H40) 2.c Secondary CH2 refined with riding coordinates: C11(H11A,H11B), C13(H13A,H13B), C39(H39A,H39B), C41(H41A,H41B) 2.d Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50) 2.e Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C48(H48A,H48B,H48C) ; _shelx_res_file ; a_a.res created by SHELXL-2014/7 TITL a_a.res in P-1 CELL 0.71073 10.3841 10.9859 19.4247 102.72 92.216 109.909 ZERR 2 0.0076 0.0083 0.0141 0.024 0.036 0.026 LATT 1 SFAC C H N O UNIT 100 96 4 10 L.S. 10 PLAN -5 0 0 SIZE 0.123 0.187 0.19 TEMP 20 HTAB BOND $H CONF fmap 2 acta OMIT -1 1 0 REM REM REM WGHT 0.047600 0.766400 FVAR 0.74179 O1 4 0.620379 0.684232 0.030523 11.00000 0.03075 0.04037 = 0.03177 0.00766 0.00266 0.01519 O2 4 0.936943 0.850343 0.136282 11.00000 0.03061 0.05238 = 0.04804 0.01042 -0.00571 0.00621 O3 4 0.601820 0.637865 0.473080 11.00000 0.03148 0.04060 = 0.03566 0.01329 0.00833 0.01273 O4 4 0.740664 0.722026 0.322654 11.00000 0.06191 0.06475 = 0.04178 0.02823 0.01732 0.02188 AFIX 6 O5 4 0.972009 0.724805 0.245975 11.00000 0.05480 0.11223 = 0.07694 0.04043 0.00518 0.03518 H5A 2 0.961749 0.760920 0.212707 11.00000 -1.50000 H5B 2 0.904106 0.724023 0.269169 11.00000 -1.50000 AFIX 0 N1 3 0.805866 0.798536 0.112437 11.00000 0.03439 0.03310 = 0.03499 0.00903 -0.00012 0.00894 N2 3 0.724115 0.697914 0.384847 11.00000 0.04030 0.03814 = 0.04095 0.01795 0.01386 0.01398 C1 1 0.993725 0.739064 -0.121559 11.00000 0.05366 0.11317 = 0.04910 0.03290 0.01877 0.03383 AFIX 43 H1 2 1.046780 0.752808 -0.158568 11.00000 -1.20000 AFIX 0 C2 1 0.944829 0.835742 -0.088183 11.00000 0.05085 0.07479 = 0.05322 0.03065 0.00939 0.01210 AFIX 43 H2 2 0.964117 0.914728 -0.102621 11.00000 -1.20000 AFIX 0 C3 1 0.867035 0.814255 -0.033177 11.00000 0.04517 0.05311 = 0.04388 0.01511 0.00750 0.01502 AFIX 43 H3 2 0.833633 0.879344 -0.010742 11.00000 -1.20000 AFIX 0 C4 1 0.837617 0.697630 -0.010648 11.00000 0.02896 0.04647 = 0.03481 0.00962 0.00172 0.01216 C5 1 0.751155 0.678854 0.049478 11.00000 0.02753 0.03573 = 0.03365 0.00602 0.00000 0.01190 C6 1 0.571571 0.723003 0.097810 11.00000 0.03735 0.03424 = 0.03154 0.00842 0.00790 0.01595 C7 1 0.456917 0.774228 0.085546 11.00000 0.03231 0.03221 = 0.04604 0.00814 0.00481 0.01318 C8 1 0.441758 0.818139 0.025772 11.00000 0.05537 0.05762 = 0.05028 0.01698 0.00842 0.03194 AFIX 43 H8 2 0.506307 0.821729 -0.006333 11.00000 -1.20000 AFIX 0 C9 1 0.331414 0.857089 0.012840 11.00000 0.07640 0.07350 = 0.06591 0.01724 -0.00443 0.04671 AFIX 43 H9 2 0.322462 0.886099 -0.027986 11.00000 -1.20000 AFIX 0 C10 1 0.235613 0.853406 0.059316 11.00000 0.04713 0.05614 = 0.10319 0.01140 -0.00545 0.02867 AFIX 43 H10 2 0.160590 0.877784 0.049879 11.00000 -1.20000 AFIX 0 C11 1 0.730635 0.554812 0.076809 11.00000 0.03747 0.03722 = 0.03812 0.00883 0.00385 0.01714 AFIX 23 H11A 2 0.819976 0.552503 0.091439 11.00000 -1.20000 H11B 2 0.683497 0.475769 0.038707 11.00000 -1.20000 AFIX 0 C12 1 0.645648 0.552746 0.140216 11.00000 0.03841 0.03472 = 0.03465 0.00824 0.00128 0.01405 AFIX 13 H12 2 0.706971 0.618835 0.181309 11.00000 -1.20000 AFIX 0 C13 1 0.525696 0.598918 0.127660 11.00000 0.03738 0.03728 = 0.04004 0.01197 0.00808 0.01470 AFIX 23 H13A 2 0.489017 0.619261 0.172170 11.00000 -1.20000 H13B 2 0.452697 0.527318 0.094521 11.00000 -1.20000 AFIX 0 C14 1 0.361258 0.774617 0.132901 11.00000 0.06158 0.07295 = 0.07849 0.03967 0.03194 0.04085 AFIX 43 H14 2 0.370908 0.748165 0.174515 11.00000 -1.20000 AFIX 0 C15 1 0.251467 0.813563 0.119632 11.00000 0.05201 0.07405 = 0.11946 0.04156 0.03817 0.03923 AFIX 43 H15 2 0.187921 0.812549 0.152152 11.00000 -1.20000 AFIX 0 C16 1 0.704467 0.824565 0.140527 11.00000 0.03978 0.03232 = 0.03577 0.00965 0.00356 0.01535 C17 1 0.721738 0.921754 0.208538 11.00000 0.06518 0.04857 = 0.04621 -0.00136 0.00089 0.02654 AFIX 137 H17A 2 0.814674 0.985048 0.218002 11.00000 -1.50000 H17B 2 0.703236 0.876036 0.245905 11.00000 -1.50000 H17C 2 0.658618 0.967845 0.206262 11.00000 -1.50000 AFIX 0 C18 1 0.603091 0.418236 0.159077 11.00000 0.05128 0.03944 = 0.03149 0.01091 0.00923 0.02134 C19 1 0.468943 0.327852 0.146414 11.00000 0.05558 0.03923 = 0.04977 0.01328 0.00285 0.01369 AFIX 43 H19 2 0.399861 0.348726 0.125371 11.00000 -1.20000 AFIX 0 C20 1 0.435861 0.206996 0.164524 11.00000 0.07020 0.04318 = 0.06807 0.02077 0.01191 0.01320 AFIX 43 H20 2 0.345011 0.147473 0.155443 11.00000 -1.20000 AFIX 0 C21 1 0.535031 0.174290 0.195528 11.00000 0.09407 0.04987 = 0.07544 0.03226 0.03095 0.03435 AFIX 43 H21 2 0.512324 0.092818 0.207615 11.00000 -1.20000 AFIX 0 C22 1 0.669384 0.262983 0.208848 11.00000 0.08660 0.06873 = 0.06281 0.03236 0.02299 0.05333 AFIX 43 H22 2 0.737545 0.240916 0.229889 11.00000 -1.20000 AFIX 0 C23 1 0.704019 0.384956 0.191174 11.00000 0.05632 0.05553 = 0.05334 0.02201 0.01490 0.03034 AFIX 43 H23 2 0.794867 0.444479 0.200822 11.00000 -1.20000 AFIX 0 C24 1 0.886671 0.601249 -0.044941 11.00000 0.05216 0.06605 = 0.04773 0.01595 0.01263 0.03231 AFIX 43 H24 2 0.867458 0.522005 -0.030773 11.00000 -1.20000 AFIX 0 C25 1 0.964215 0.622467 -0.100245 11.00000 0.06471 0.10613 = 0.05338 0.01999 0.02188 0.05211 AFIX 43 H25 2 0.996744 0.557117 -0.123262 11.00000 -1.20000 AFIX 0 C26 1 0.843934 0.907171 0.708204 11.00000 0.06983 0.05992 = 0.04455 -0.00040 0.00580 0.00626 AFIX 43 H26 2 0.865933 0.961059 0.754364 11.00000 -1.20000 AFIX 0 C27 1 0.815877 0.956314 0.652639 11.00000 0.07155 0.04371 = 0.05764 0.00410 0.01159 0.01125 AFIX 43 H27 2 0.817424 1.043518 0.661175 11.00000 -1.20000 AFIX 0 C28 1 0.785487 0.877025 0.584387 11.00000 0.05751 0.04115 = 0.04567 0.01039 0.00584 0.01302 AFIX 43 H28 2 0.766280 0.911259 0.547125 11.00000 -1.20000 AFIX 0 C29 1 0.782979 0.747288 0.570176 11.00000 0.03117 0.03829 = 0.04044 0.01124 0.00772 0.00626 C30 1 0.745869 0.662514 0.494816 11.00000 0.02834 0.03756 = 0.03878 0.01238 0.00662 0.00984 C31 1 0.587247 0.602221 0.397984 11.00000 0.03529 0.03729 = 0.03311 0.01357 0.00866 0.01250 C32 1 0.465563 0.627169 0.368747 11.00000 0.03627 0.04092 = 0.04280 0.02049 0.00764 0.01313 C33 1 0.418456 0.719855 0.409452 11.00000 0.05325 0.04910 = 0.06045 0.01366 0.00205 0.02506 AFIX 43 H33 2 0.465630 0.769774 0.454004 11.00000 -1.20000 AFIX 0 C34 1 0.302974 0.738905 0.384815 11.00000 0.06194 0.07166 = 0.08720 0.02494 0.00663 0.04066 AFIX 43 H34 2 0.271433 0.800077 0.413281 11.00000 -1.20000 AFIX 0 C35 1 0.233738 0.668827 0.318794 11.00000 0.04975 0.08536 = 0.09384 0.04561 0.00587 0.03316 AFIX 43 H35 2 0.155878 0.682502 0.302131 11.00000 -1.20000 AFIX 0 C36 1 0.814737 0.732006 0.439921 11.00000 0.03444 0.03554 = 0.04219 0.01218 0.00865 0.00922 C37 1 0.395341 0.557132 0.302355 11.00000 0.05287 0.06710 = 0.04481 0.01751 0.00528 0.02507 AFIX 43 H37 2 0.425479 0.494862 0.273851 11.00000 -1.20000 AFIX 0 C38 1 0.280221 0.578821 0.277785 11.00000 0.05555 0.08407 = 0.05798 0.02880 -0.00735 0.02045 AFIX 43 H38 2 0.234024 0.531341 0.232706 11.00000 -1.20000 AFIX 0 C39 1 0.587866 0.461449 0.372928 11.00000 0.03981 0.03645 = 0.04354 0.01133 0.00589 0.01220 AFIX 23 H39A 2 0.581552 0.437820 0.321442 11.00000 -1.20000 H39B 2 0.507549 0.399340 0.386592 11.00000 -1.20000 AFIX 0 C40 1 0.719122 0.447966 0.404550 11.00000 0.03960 0.03595 = 0.04423 0.01248 0.01122 0.01328 AFIX 13 H40 2 0.794159 0.488935 0.378390 11.00000 -1.20000 AFIX 0 C41 1 0.760174 0.525628 0.483092 11.00000 0.03470 0.03997 = 0.04461 0.01488 0.00433 0.01352 AFIX 23 H41A 2 0.701742 0.474582 0.512349 11.00000 -1.20000 H41B 2 0.854951 0.537337 0.497596 11.00000 -1.20000 AFIX 0 C42 1 0.709645 0.304598 0.397082 11.00000 0.05055 0.03916 = 0.03868 0.00919 0.00646 0.02017 C43 1 0.587953 0.203333 0.399049 11.00000 0.06158 0.04691 = 0.11206 0.02856 0.03547 0.02514 AFIX 43 H43 2 0.507105 0.221685 0.403037 11.00000 -1.20000 AFIX 0 C44 1 0.584141 0.074984 0.395189 11.00000 0.08185 0.04573 = 0.12584 0.02958 0.03968 0.02318 AFIX 43 H44 2 0.501238 0.008227 0.397109 11.00000 -1.20000 AFIX 0 C45 1 0.701418 0.045664 0.388573 11.00000 0.10183 0.04696 = 0.06103 0.01111 0.01202 0.04095 AFIX 43 H45 2 0.698730 -0.040669 0.386173 11.00000 -1.20000 AFIX 0 C46 1 0.822001 0.143503 0.385525 11.00000 0.06911 0.06010 = 0.07557 0.00885 -0.00149 0.04006 AFIX 43 H46 2 0.902023 0.123938 0.380497 11.00000 -1.20000 AFIX 0 C47 1 0.826119 0.271498 0.389854 11.00000 0.04700 0.04996 = 0.07212 0.01013 -0.00170 0.02203 AFIX 43 H47 2 0.909581 0.337450 0.387858 11.00000 -1.20000 AFIX 0 C48 1 0.961506 0.806552 0.440521 11.00000 0.03936 0.06450 = 0.06526 0.01740 0.00920 0.00279 AFIX 137 H48A 2 1.002667 0.749290 0.412709 11.00000 -1.50000 H48B 2 1.006255 0.837747 0.488569 11.00000 -1.50000 H48C 2 0.971958 0.881562 0.420679 11.00000 -1.50000 AFIX 0 C49 1 0.810072 0.698625 0.626892 11.00000 0.05540 0.04883 = 0.04315 0.01280 0.00488 0.01471 AFIX 43 H49 2 0.808553 0.611482 0.618882 11.00000 -1.20000 AFIX 0 C50 1 0.839253 0.778705 0.695102 11.00000 0.07576 0.07265 = 0.04171 0.01684 -0.00139 0.01657 AFIX 43 H50 2 0.856037 0.744487 0.732832 11.00000 -1.20000 AFIX 0 HKLF 4 REM a_a.res in P-1 REM R1 = 0.0539 for 5200 Fo > 4sig(Fo) and 0.1074 for all 8164 data REM 519 parameters refined using 0 restraints END WGHT 0.0476 0.7660 REM Instructions for potential hydrogen bonds HTAB O5 O2 HTAB O5 N1 HTAB O5 O4 HTAB C17 O4 REM Highest difference peak 0.187, deepest hole -0.219, 1-sigma level 0.041 Q1 1 0.5160 0.2628 0.4471 11.00000 0.05 0.19 Q2 1 0.9914 0.8015 0.3831 11.00000 0.05 0.18 Q3 1 0.6256 0.9020 0.2252 11.00000 0.05 0.18 Q4 1 0.4597 0.2019 0.3584 11.00000 0.05 0.17 Q5 1 0.8106 0.9178 0.2451 11.00000 0.05 0.16 ; 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63.79 7.40 -2 -5 0 56.09 6.90 2 5 0 55.79 7.90 2 5 0 62.79 7.90 2 5 0 63.99 7.40 2 5 0 59.59 3.50 2 5 0 67.49 8.20 2 5 0 80.49 7.70 2 5 0 68.39 7.60 2 5 0 61.99 6.20 2 5 0 65.49 6.70 2 5 0 73.79 8.70 2 5 0 65.09 15.20 2 5 0 68.89 5.20 2 5 0 54.39 8.30 2 5 0 60.29 4.60 -3 -5 0 260.07 13.80 -3 -5 0 278.67 10.60 -3 -5 0 277.67 14.70 -3 -5 0 214.88 18.80 -3 -5 0 247.18 13.50 -3 -5 0 259.97 11.80 3 5 0 269.37 14.90 3 5 0 261.27 13.90 3 5 0 287.27 15.90 3 5 0 277.67 14.50 3 5 0 255.97 13.10 3 5 0 253.37 12.80 3 5 0 261.27 12.60 3 5 0 235.68 12.50 3 5 0 270.87 10.30 -4 -5 0 18.30 4.40 -4 -5 0 6.30 6.70 -4 -5 0 12.50 14.60 -4 -5 0 14.30 5.00 -4 -5 0 13.50 6.40 4 5 0 7.40 4.70 4 5 0 15.90 3.60 4 5 0 8.40 5.80 4 5 0 15.30 6.20 4 5 0 10.10 6.30 -5 -5 0 -0.80 7.10 -5 -5 0 2.10 15.30 -5 -5 0 -4.70 5.10 -5 -5 0 6.60 3.30 -5 -5 0 0.20 6.40 5 5 0 -9.60 5.80 5 5 0 1.30 6.40 5 5 0 -4.30 3.80 5 5 0 3.20 6.90 5 5 0 -9.30 4.30 -6 -5 0 -1.00 17.60 -6 -5 0 1.70 8.00 -6 -5 0 8.40 7.30 6 5 0 -8.00 7.90 6 5 0 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42.40 8.50 -4 -6 0 55.89 9.90 -4 -6 0 61.59 10.80 -4 -6 0 47.00 6.90 -4 -6 0 58.19 7.30 -4 -6 0 80.79 19.40 4 6 0 51.89 7.10 4 6 0 36.10 8.70 4 6 0 48.50 8.60 4 6 0 59.19 10.60 4 6 0 41.10 7.30 4 6 0 82.89 11.00 -5 -6 0 14.40 7.70 -5 -6 0 3.50 5.00 -5 -6 0 -5.80 5.00 -5 -6 0 7.90 18.20 -5 -6 0 10.70 8.10 5 6 0 -11.40 5.40 5 6 0 -0.50 5.00 5 6 0 3.00 7.40 5 6 0 18.50 7.90 5 6 0 6.10 7.90 5 6 0 -3.30 8.70 -6 -6 0 29.80 9.50 -6 -6 0 30.90 23.20 -6 -6 0 39.10 9.90 6 6 0 29.40 9.30 6 6 0 28.10 9.60 6 6 0 26.00 9.90 6 6 0 38.10 11.70 -7 -6 0 55.39 23.40 -7 -6 0 22.30 10.30 -7 -6 0 11.50 11.70 7 6 0 -10.00 10.90 7 6 0 -13.00 11.40 7 6 0 17.30 10.60 -8 -6 0 25.10 13.60 -8 -6 0 8.80 12.10 -8 -6 0 54.09 28.00 8 6 0 4.20 13.30 8 6 0 6.00 13.10 8 6 0 9.00 11.50 12 -7 0 9.60 13.00 12 -7 0 21.30 15.20 12 -7 0 1.00 10.20 -12 7 0 -0.50 12.90 -12 7 0 18.80 12.00 -12 7 0 6.40 13.40 11 -7 0 -6.40 11.70 11 -7 0 2.10 9.60 11 -7 0 -6.10 9.10 11 -7 0 -0.10 9.90 -11 7 0 -7.70 9.20 -11 7 0 3.70 11.20 -11 7 0 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2 7 0 69.29 9.60 -3 -7 0 29.90 17.00 -3 -7 0 67.39 11.30 -3 -7 0 65.19 6.70 -3 -7 0 60.29 8.70 3 7 0 53.59 8.90 3 7 0 52.09 6.80 3 7 0 61.19 9.00 3 7 0 55.79 8.90 3 7 0 56.49 11.60 3 7 0 56.89 10.50 -4 -7 0 25.50 8.20 -4 -7 0 16.80 17.10 -4 -7 0 10.50 6.20 -4 -7 0 15.00 5.20 -4 -7 0 6.60 8.70 4 7 0 12.10 7.80 4 7 0 27.60 9.30 4 7 0 12.70 7.20 4 7 0 9.80 7.90 4 7 0 0.90 8.50 4 7 0 10.70 5.80 -5 -7 0 -10.30 6.10 -5 -7 0 0.20 8.60 -5 -7 0 10.60 9.90 -5 -7 0 3.90 27.80 5 7 0 -5.90 10.70 5 7 0 4.90 8.50 5 7 0 2.20 8.80 5 7 0 -3.50 8.10 -6 -7 0 17.20 9.90 -6 -7 0 19.70 19.40 -6 -7 0 7.60 12.10 6 7 0 -9.10 12.70 6 7 0 -4.10 10.40 6 7 0 3.10 10.20 6 7 0 0.70 10.00 -7 -7 0 14.00 25.20 -7 -7 0 -12.00 13.20 -7 -7 0 17.30 11.60 7 7 0 13.90 12.90 7 7 0 -10.50 12.20 -8 -7 0 23.90 32.10 12 -8 0 -21.20 12.20 12 -8 0 -23.60 12.40 12 -8 0 17.50 14.30 -12 8 0 -0.60 13.50 -12 8 0 -7.10 12.60 -12 8 0 -2.90 11.80 11 -8 0 7.90 12.00 11 -8 0 6.10 11.00 11 -8 0 40.10 13.80 -11 8 0 12.30 12.80 -11 8 0 18.90 11.80 -11 8 0 9.30 10.70 -11 8 0 -17.70 10.70 10 -8 0 10.90 10.80 10 -8 0 12.90 9.20 10 -8 0 14.00 10.70 10 -8 0 17.70 6.70 -10 8 0 9.80 8.90 -10 8 0 -2.60 10.10 -10 8 0 3.00 9.60 9 -8 0 78.59 10.40 9 -8 0 75.49 8.60 9 -8 0 88.89 13.90 9 -8 0 49.70 10.10 -9 8 0 80.99 12.50 -9 8 0 84.39 12.70 8 -8 0 21.70 8.00 8 -8 0 23.50 7.90 8 -8 0 28.80 3.70 8 -8 0 29.90 8.90 8 -8 0 37.90 6.60 8 -8 0 25.90 9.80 -8 8 0 27.00 9.00 -8 8 0 25.00 8.50 -8 8 0 30.10 5.70 -8 8 0 19.90 8.90 7 -8 0 100.29 14.50 7 -8 0 84.59 13.50 7 -8 0 117.29 13.70 7 -8 0 96.09 9.10 7 -8 0 96.09 4.20 -7 8 0 96.19 12.90 -7 8 0 106.69 15.90 -7 8 0 102.59 15.10 -7 8 0 87.29 6.00 6 -8 0 133.59 14.10 6 -8 0 155.48 5.70 6 -8 0 164.08 9.60 6 -8 0 137.79 12.40 -6 8 0 161.28 13.40 -6 8 0 127.89 14.20 -6 8 0 153.78 13.90 5 -8 0 80.79 7.30 5 -8 0 85.99 10.70 5 -8 0 71.39 11.30 5 -8 0 71.49 4.80 -5 8 0 67.19 9.70 -5 8 0 70.99 10.10 -5 8 0 77.49 7.80 -5 8 0 61.79 9.50 -5 8 0 55.29 9.60 -5 8 0 73.99 4.90 -5 8 0 56.39 9.10 4 -8 0 -1.40 5.00 4 -8 0 -8.40 12.60 4 -8 0 0.60 2.90 4 -8 0 6.30 3.40 4 -8 0 -6.30 6.20 -4 8 0 -7.40 4.50 -4 8 0 4.40 5.70 -4 8 0 2.40 6.50 -4 8 0 2.80 3.90 -4 8 0 7.20 3.00 -4 8 0 -5.60 4.60 3 -8 0 80.09 12.20 3 -8 0 102.99 9.40 3 -8 0 99.39 7.20 3 -8 0 98.39 6.70 -3 8 0 90.49 10.20 -3 8 0 83.99 8.40 -3 8 0 89.79 10.50 -3 8 0 84.69 11.10 -3 8 0 84.09 7.70 -3 8 0 79.49 8.70 -3 8 0 91.49 8.00 2 -8 0 142.09 9.90 2 -8 0 142.49 8.80 2 -8 0 154.28 8.90 2 -8 0 131.79 12.30 -2 8 0 154.28 13.70 -2 8 0 139.69 10.80 -2 8 0 123.49 8.20 -2 8 0 131.49 6.60 -2 8 0 135.39 11.50 -2 8 0 136.39 12.00 -2 8 0 142.39 13.90 -2 8 0 137.69 9.30 -2 8 0 128.69 9.00 -2 8 0 131.99 10.50 -2 8 0 133.89 8.50 1 -8 0 8.40 5.20 1 -8 0 -0.30 3.70 1 -8 0 5.80 6.70 1 -8 0 8.10 4.70 1 -8 0 11.90 6.00 1 -8 0 4.80 10.30 -1 8 0 4.00 4.80 -1 8 0 -2.40 4.50 -1 8 0 -4.40 5.00 -1 8 0 7.50 4.30 -1 8 0 2.40 6.30 -1 8 0 13.20 6.80 -1 8 0 4.20 4.10 -1 8 0 5.80 3.80 -1 8 0 9.40 5.90 -1 8 0 4.80 8.00 0 -8 0 271.17 11.90 0 -8 0 242.68 14.80 0 -8 0 251.97 15.60 0 8 0 249.48 12.70 0 8 0 279.87 13.30 0 8 0 257.77 14.40 0 8 0 241.78 16.20 0 8 0 234.08 10.40 0 8 0 251.27 13.70 0 8 0 262.37 15.80 0 8 0 240.88 12.30 0 8 0 262.17 14.40 -1 -8 0 98.09 11.00 -1 -8 0 94.49 12.30 -1 -8 0 92.29 7.70 -1 -8 0 82.39 10.40 -1 -8 0 104.59 9.20 1 8 0 93.99 8.80 1 8 0 92.69 11.10 1 8 0 93.09 8.70 1 8 0 92.59 10.30 1 8 0 96.69 12.40 1 8 0 99.59 10.60 1 8 0 76.09 12.30 1 8 0 73.69 9.20 1 8 0 92.09 10.40 -2 -8 0 3.20 15.60 -2 -8 0 30.30 8.30 -2 -8 0 12.60 7.60 -2 -8 0 26.50 9.10 2 8 0 17.60 4.10 2 8 0 30.40 7.90 2 8 0 31.10 5.60 2 8 0 28.40 8.70 2 8 0 16.20 9.80 2 8 0 11.10 7.30 2 8 0 21.60 6.80 2 8 0 34.70 6.80 2 8 0 20.50 7.70 -3 -8 0 114.19 12.20 -3 -8 0 101.19 13.70 -3 -8 0 104.99 11.90 3 8 0 117.39 11.60 3 8 0 85.69 12.20 3 8 0 134.49 13.90 3 8 0 106.69 12.70 3 8 0 87.09 12.10 3 8 0 126.69 17.30 -4 -8 0 33.10 11.50 -4 -8 0 -19.20 18.10 -4 -8 0 1.60 7.40 -4 -8 0 -5.10 8.10 4 8 0 -5.10 7.90 4 8 0 26.80 11.50 4 8 0 10.40 10.20 4 8 0 10.00 8.70 -5 -8 0 4.20 9.60 -5 -8 0 14.10 11.80 -5 -8 0 62.99 25.20 5 8 0 -9.30 9.60 5 8 0 7.60 13.10 5 8 0 -5.70 10.10 -6 -8 0 14.80 13.90 -6 -8 0 29.20 12.10 -6 -8 0 53.59 28.30 6 8 0 1.60 12.50 6 8 0 21.20 15.30 6 8 0 8.70 12.20 -7 -8 0 109.99 34.30 11 -9 0 9.30 9.40 11 -9 0 -21.80 13.20 11 -9 0 9.30 11.40 11 -9 0 6.70 15.10 -11 9 0 4.30 12.30 -11 9 0 8.00 11.20 10 -9 0 -11.30 7.80 10 -9 0 13.00 11.40 10 -9 0 -2.80 10.50 10 -9 0 6.10 9.90 -10 9 0 -10.80 9.90 -10 9 0 -11.00 10.30 -10 9 0 9.20 11.10 9 -9 0 5.50 9.70 9 -9 0 2.90 7.10 9 -9 0 4.10 10.70 9 -9 0 12.20 10.00 -9 9 0 -13.50 9.00 -9 9 0 8.20 8.80 -9 9 0 8.00 9.40 8 -9 0 146.39 11.60 8 -9 0 186.58 15.90 8 -9 0 158.78 18.30 -8 9 0 160.68 16.90 -8 9 0 153.48 16.40 -8 9 0 146.29 16.80 7 -9 0 257.47 17.20 7 -9 0 300.67 20.00 7 -9 0 266.77 13.00 -7 9 0 291.67 19.80 -7 9 0 292.47 18.40 -7 9 0 286.57 18.90 6 -9 0 19.90 5.00 6 -9 0 20.90 2.70 6 -9 0 18.60 10.70 -6 9 0 14.30 7.90 -6 9 0 10.20 7.80 -6 9 0 15.60 7.90 5 -9 0 141.29 9.00 5 -9 0 136.89 7.00 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6.90 -4 7 -4 35.80 5.10 4 -7 4 35.20 6.40 4 -7 4 38.50 6.10 4 -7 4 39.70 5.70 4 -7 4 40.80 8.90 4 -7 4 36.40 3.20 -5 7 -4 96.89 10.00 -5 7 -4 103.99 5.60 -5 7 -4 72.49 13.20 -5 7 -4 95.99 10.10 -5 7 -4 104.09 7.60 -5 7 -4 103.09 10.50 5 -7 4 84.59 9.50 5 -7 4 102.29 7.00 5 -7 4 104.39 11.40 5 -7 4 90.79 6.80 5 -7 4 90.09 9.80 -6 7 -4 163.58 13.00 -6 7 -4 160.88 9.70 -6 7 -4 164.68 12.90 -6 7 -4 166.48 14.10 -6 7 -4 162.58 13.60 6 -7 4 148.79 8.50 6 -7 4 176.58 13.70 6 -7 4 144.89 6.40 6 -7 4 163.08 13.80 6 -7 4 177.88 13.50 -7 7 -4 639.24 26.70 -7 7 -4 613.94 26.30 -7 7 -4 646.84 25.60 7 -7 4 602.74 25.80 7 -7 4 637.34 19.30 7 -7 4 596.94 26.00 7 -7 4 618.34 26.30 -8 7 -4 12.20 8.80 -8 7 -4 15.20 5.00 -8 7 -4 16.20 9.30 -8 7 -4 17.30 7.80 8 -7 4 13.10 8.40 8 -7 4 3.60 7.90 8 -7 4 10.00 5.20 8 -7 4 16.30 5.30 -9 7 -4 236.08 18.40 -9 7 -4 212.78 13.40 -9 7 -4 264.47 20.20 -9 7 -4 246.68 19.10 9 -7 4 228.68 18.00 9 -7 4 297.27 22.10 9 -7 4 223.78 13.40 -10 7 -4 6.60 9.70 -10 7 -4 4.20 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10.70 -5 4 -10 82.29 8.30 5 -4 10 70.99 6.90 5 -4 10 82.99 12.20 5 -4 10 71.89 11.40 5 -4 10 76.39 7.80 5 -4 10 65.69 8.50 -6 4 -10 134.79 11.30 -6 4 -10 125.69 13.20 -6 4 -10 162.38 13.90 -6 4 -10 115.49 10.40 6 -4 10 127.29 10.90 6 -4 10 146.49 15.80 6 -4 10 141.59 15.90 6 -4 10 139.69 10.00 6 -4 10 138.29 11.50 -7 4 -10 -8.80 6.40 -7 4 -10 -1.30 7.60 -7 4 -10 2.50 7.30 -7 4 -10 -5.60 5.90 7 -4 10 -2.90 7.80 7 -4 10 4.80 6.80 7 -4 10 6.70 9.20 7 -4 10 13.70 8.90 7 -4 10 -8.30 9.50 -8 4 -10 9.50 6.00 -8 4 -10 7.80 9.30 -8 4 -10 3.00 7.40 -8 4 -10 9.50 7.20 -8 4 -10 18.30 8.30 -8 4 -10 10.10 8.50 8 -4 10 -1.50 9.80 8 -4 10 1.70 8.40 8 -4 10 16.60 9.00 8 -4 10 20.50 11.10 -9 4 -10 -15.10 9.60 -9 4 -10 -6.40 9.10 -9 4 -10 1.30 6.40 -9 4 -10 -4.40 7.90 -9 4 -10 -1.40 9.70 9 -4 10 10.10 8.90 9 -4 10 0.50 12.70 9 -4 10 6.10 8.50 9 -4 10 13.50 11.90 -10 4 -10 13.80 11.30 -10 4 -10 14.80 11.00 -10 4 -10 -1.90 11.00 -10 4 -10 -13.20 9.90 10 -4 10 -22.50 10.20 10 -4 10 -14.10 12.20 10 -4 10 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-3 -5 22 -12.50 10.60 -3 -5 22 29.70 16.40 2 5 -22 1.60 10.90 2 5 -22 3.30 11.60 -2 -5 22 -15.70 14.80 -2 -5 22 7.20 9.80 -2 -5 22 7.40 17.10 -2 -5 22 -15.50 48.70 1 5 -22 1.00 9.00 1 5 -22 0.80 10.30 1 5 -22 22.10 11.70 1 5 -22 3.00 10.00 -1 -5 22 7.30 11.00 -1 -5 22 -34.90 34.20 -1 -5 22 14.90 14.10 -1 -5 22 31.90 16.60 0 5 -22 23.10 11.20 0 5 -22 1.20 9.00 0 5 -22 16.00 12.10 0 -5 22 -17.80 15.90 0 -5 22 2.20 11.20 0 -5 22 -7.00 13.90 -1 5 -22 -0.10 12.00 -1 5 -22 31.10 10.60 -1 5 -22 28.20 12.20 1 -5 22 21.40 14.50 1 -5 22 15.50 31.80 1 -5 22 -10.90 15.60 1 -5 22 -2.80 11.70 -2 5 -22 32.00 12.20 -2 5 -22 8.50 11.50 -2 5 -22 14.50 10.70 2 -5 22 17.50 16.20 2 -5 22 12.00 15.90 2 -5 22 16.20 12.40 -3 5 -22 -6.20 11.90 -3 5 -22 17.20 12.70 -3 5 -22 0.40 11.60 3 -5 22 -0.70 13.80 3 -5 22 0.10 15.80 3 -5 22 22.00 14.30 -4 5 -22 -14.80 12.60 -4 5 -22 17.80 12.40 -4 5 -22 -19.20 13.40 4 -5 22 11.10 11.10 4 -5 22 21.70 14.40 4 -5 22 -3.30 15.80 4 4 -22 28.60 10.00 4 4 -22 30.80 12.80 -4 -4 22 9.80 11.30 -4 -4 22 2.60 16.50 -4 -4 22 -12.20 13.20 3 4 -22 13.30 9.60 3 4 -22 13.90 8.40 -3 -4 22 -19.70 10.40 -3 -4 22 5.80 14.80 -3 -4 22 0.20 12.70 2 4 -22 -6.50 8.20 2 4 -22 -4.90 10.40 -2 -4 22 -8.90 14.50 -2 -4 22 5.90 10.90 -2 -4 22 -6.70 12.70 1 4 -22 14.70 8.20 1 4 -22 17.70 11.80 1 4 -22 14.40 11.80 -1 -4 22 -11.80 15.90 -1 -4 22 27.70 11.30 -1 -4 22 7.00 13.30 0 4 -22 24.00 10.10 0 4 -22 29.50 11.60 0 -4 22 19.50 11.40 0 -4 22 38.10 15.90 0 -4 22 -33.10 36.00 0 -4 22 12.90 14.90 -1 4 -22 -10.00 10.90 -1 4 -22 10.40 10.70 -1 4 -22 -0.50 10.40 1 -4 22 -18.20 13.50 1 -4 22 0.20 10.60 -2 4 -22 -2.70 10.20 -2 4 -22 0.50 9.50 -2 4 -22 2.60 11.30 -2 4 -22 -1.70 12.20 2 -4 22 5.10 15.20 2 -4 22 4.60 11.30 2 -4 22 -18.50 14.50 -3 4 -22 18.20 10.90 -3 4 -22 7.10 11.20 -3 4 -22 20.60 12.50 -3 4 -22 14.50 11.90 3 -4 22 -4.40 14.60 3 -4 22 49.20 16.10 3 -4 22 24.20 14.60 -4 4 -22 69.39 15.10 -4 4 -22 116.39 16.00 -4 4 -22 103.69 17.70 4 -4 22 93.19 14.00 4 -4 22 102.99 16.90 4 -4 22 86.89 20.50 5 3 -22 12.70 10.70 5 3 -22 9.50 10.90 -5 -3 22 -7.50 19.30 -5 -3 22 22.90 11.50 -5 -3 22 -28.10 15.10 4 3 -22 9.70 10.30 4 3 -22 19.80 9.70 -4 -3 22 15.70 11.00 -4 -3 22 -5.90 15.80 -4 -3 22 18.60 15.30 3 3 -22 19.10 9.00 3 3 -22 5.50 11.00 -3 -3 22 25.40 11.10 -3 -3 22 18.80 15.20 -3 -3 22 -10.70 13.10 2 3 -22 2.10 12.00 2 3 -22 -5.20 9.10 2 3 -22 4.90 8.50 -2 -3 22 14.80 9.50 -2 -3 22 8.80 13.60 -2 -3 22 -10.90 13.00 1 3 -22 -4.20 8.00 1 3 -22 -7.60 10.30 1 3 -22 -0.80 10.40 -1 -3 22 -12.60 12.50 -1 -3 22 -15.60 9.00 -1 -3 22 27.90 15.10 0 3 -22 20.60 10.10 0 3 -22 23.50 11.60 0 3 -22 35.00 9.40 0 -3 22 21.40 14.30 0 -3 22 11.40 13.50 0 -3 22 41.00 12.20 -1 3 -22 7.00 9.90 -1 3 -22 18.90 11.80 -1 3 -22 -8.60 8.70 1 -3 22 3.60 13.90 1 -3 22 15.30 13.80 1 -3 22 19.30 12.60 -2 3 -22 -6.10 10.10 -2 3 -22 17.60 12.00 -2 3 -22 12.90 9.90 2 -3 22 -10.70 15.40 2 -3 22 12.90 13.60 2 -3 22 26.70 15.40 -3 3 -22 35.00 14.20 -3 3 -22 1.80 14.70 -3 3 -22 29.80 11.70 3 -3 22 9.20 14.30 3 -3 22 39.20 14.70 3 -3 22 -15.20 14.70 -4 3 -22 36.80 13.40 -4 3 -22 72.09 16.00 4 -3 22 25.50 14.90 4 -3 22 23.40 19.40 4 -3 22 9.10 13.00 5 2 -22 1.40 10.00 5 2 -22 -10.70 9.30 -5 -2 22 -11.50 11.80 -5 -2 22 14.90 19.00 -5 -2 22 -2.50 13.90 4 2 -22 10.40 12.40 4 2 -22 7.10 10.00 4 2 -22 -10.60 9.30 -4 -2 22 2.90 10.90 -4 -2 22 -17.40 14.60 -4 -2 22 -7.40 12.50 3 2 -22 -11.50 11.30 3 2 -22 -1.10 9.20 3 2 -22 2.60 9.20 -3 -2 22 18.00 10.50 -3 -2 22 -21.80 13.70 -3 -2 22 5.70 14.50 2 2 -22 2.60 9.00 2 2 -22 -5.00 10.90 2 2 -22 19.20 9.20 -2 -2 22 -13.90 13.30 -2 -2 22 -20.70 10.30 -2 -2 22 -15.50 12.30 1 2 -22 4.40 9.10 1 2 -22 11.40 9.20 1 2 -22 -25.70 10.70 -1 -2 22 19.90 9.90 -1 -2 22 -0.60 14.40 -1 -2 22 -0.60 15.00 0 2 -22 -0.10 9.90 0 2 -22 -4.60 9.90 0 2 -22 19.20 11.30 0 2 -22 17.50 9.40 0 -2 22 9.00 13.20 0 -2 22 23.80 15.50 0 -2 22 0.00 10.40 -1 2 -22 22.40 12.30 -1 2 -22 0.90 8.60 -1 2 -22 -9.00 12.10 -1 2 -22 -2.20 9.40 1 -2 22 -0.70 12.50 1 -2 22 -8.10 13.10 1 -2 22 -6.00 10.70 -2 2 -22 9.40 14.20 -2 2 -22 -19.20 10.30 -2 2 -22 -0.30 13.40 2 -2 22 -3.90 13.80 2 -2 22 9.10 12.70 -3 2 -22 -8.10 11.80 -3 2 -22 24.60 14.30 -3 2 -22 8.30 12.50 3 -2 22 22.00 11.20 3 -2 22 6.10 15.20 3 -2 22 10.50 13.90 3 -2 22 13.30 13.50 -4 2 -22 26.90 16.30 4 -2 22 3.60 19.40 4 -2 22 -18.90 16.10 5 1 -22 5.60 9.60 5 1 -22 -5.00 9.60 5 1 -22 -11.70 12.90 -5 -1 22 -3.80 13.40 -5 -1 22 -35.60 15.40 -5 -1 22 -3.10 12.20 4 1 -22 -10.30 11.60 4 1 -22 12.30 10.80 4 1 -22 25.20 10.60 -4 -1 22 17.30 10.80 -4 -1 22 -23.80 12.90 -4 -1 22 12.20 14.80 3 1 -22 -0.90 11.00 3 1 -22 -9.90 10.10 3 1 -22 -3.20 8.50 -3 -1 22 -8.00 9.90 -3 -1 22 -18.10 12.80 -3 -1 22 -0.50 14.20 2 1 -22 6.60 11.20 2 1 -22 20.60 8.50 2 1 -22 2.60 10.20 -2 -1 22 -26.90 10.90 -2 -1 22 10.70 14.20 -2 -1 22 -17.00 13.60 1 1 -22 6.90 9.80 1 1 -22 9.50 11.00 1 1 -22 5.20 9.20 1 1 -22 24.10 11.60 -1 -1 22 1.50 10.40 -1 -1 22 5.50 13.80 -1 -1 22 -9.10 14.50 0 1 -22 -6.80 11.50 0 1 -22 -4.70 9.80 0 1 -22 8.10 11.30 0 1 -22 3.00 8.80 0 -1 22 -14.10 12.40 0 -1 22 2.80 10.60 0 -1 22 -10.80 14.00 -1 1 -22 8.80 12.20 -1 1 -22 1.00 9.40 -1 1 -22 9.80 11.00 1 -1 22 -20.20 11.30 1 -1 22 -8.60 15.00 1 -1 22 -18.10 12.10 -2 1 -22 30.20 12.70 -2 1 -22 9.00 13.90 -2 1 -22 6.80 11.40 2 -1 22 5.00 13.70 2 -1 22 3.50 13.90 2 -1 22 7.20 12.90 -3 1 -22 16.00 15.20 -3 1 -22 -11.70 12.30 -3 1 -22 -2.00 13.90 3 -1 22 -10.20 14.00 3 -1 22 -14.90 11.20 3 -1 22 0.60 16.00 5 0 -22 9.50 12.80 5 0 -22 39.90 10.30 5 0 -22 -6.20 10.60 -5 0 22 -12.60 14.50 -5 0 22 14.90 11.60 -5 0 22 -16.20 18.50 4 0 -22 14.50 12.70 4 0 -22 6.70 10.20 4 0 -22 -2.60 10.00 -4 0 22 7.40 10.50 -4 0 22 -13.60 14.90 -4 0 22 -10.10 13.20 3 0 -22 -19.70 9.90 3 0 -22 9.00 10.20 3 0 -22 9.90 13.00 -3 0 22 15.90 10.30 -3 0 22 -12.70 12.60 -3 0 22 5.00 14.00 2 0 -22 16.90 9.30 2 0 -22 -12.50 11.60 2 0 -22 10.40 10.30 -2 0 22 -3.00 10.60 -2 0 22 -2.40 12.60 1 0 -22 9.90 12.00 1 0 -22 -5.60 10.10 1 0 -22 -6.70 10.70 -1 0 22 -13.90 15.00 -1 0 22 1.70 13.60 -1 0 22 -2.70 10.70 0 0 -22 5.00 9.60 0 0 -22 1.70 12.20 0 0 -22 0.90 12.10 0 0 22 -13.80 13.00 0 0 22 -9.10 12.70 0 0 22 -9.00 14.70 -1 0 -22 30.00 11.10 -1 0 -22 7.10 11.70 -1 0 -22 15.60 12.50 1 0 22 9.00 13.70 1 0 22 4.40 13.80 1 0 22 -7.10 13.00 -2 0 -22 -15.90 12.40 -2 0 -22 12.10 13.80 -2 0 -22 -2.20 12.50 2 0 22 -10.10 14.90 2 0 22 -1.90 11.10 2 0 22 12.00 15.70 5 -1 -22 9.40 12.20 5 -1 -22 13.10 12.30 -5 1 22 -17.00 16.10 -5 1 22 -9.10 14.00 -5 1 22 7.70 13.50 4 -1 -22 9.90 10.30 4 -1 -22 4.60 12.30 4 -1 -22 18.20 10.60 -4 1 22 14.00 11.40 -4 1 22 12.70 13.50 -4 1 22 -20.70 16.90 3 -1 -22 43.10 13.00 3 -1 -22 29.50 10.90 3 -1 -22 30.00 10.50 -3 1 22 33.90 11.80 -3 1 22 9.80 15.10 -3 1 22 11.20 13.70 2 -1 -22 -1.20 12.20 2 -1 -22 -19.60 9.40 -2 1 22 -0.20 12.70 -2 1 22 9.40 12.30 -2 1 22 -1.90 14.60 1 -1 -22 4.80 9.90 1 -1 -22 7.50 12.90 -1 1 22 -6.20 15.10 -1 1 22 1.50 11.20 -1 1 22 -0.80 14.00 0 -1 -22 22.20 14.70 0 -1 -22 14.40 10.30 0 -1 -22 36.10 12.20 0 1 22 -11.70 14.80 0 1 22 5.90 14.60 0 1 22 17.90 12.40 -1 -1 -22 11.30 13.20 -1 -1 -22 20.90 11.50 -1 -1 -22 -3.20 13.70 1 1 22 5.60 13.20 1 1 22 -32.70 14.60 1 1 22 -18.50 14.80 4 -2 -22 -17.10 11.90 -4 2 22 12.00 12.20 -4 2 22 -13.80 15.40 -4 2 22 0.10 18.00 3 -2 -22 18.70 11.20 3 -2 -22 2.30 13.80 -3 2 22 9.20 12.00 -3 2 22 -15.10 15.20 -3 2 22 17.40 16.20 2 -2 -22 16.20 14.20 2 -2 -22 10.40 10.80 -2 2 22 -24.20 16.40 -2 2 22 -20.20 11.20 -2 2 22 -15.20 15.40 1 -2 -22 17.20 11.50 1 -2 -22 14.40 13.80 -1 2 22 10.60 14.60 -1 2 22 -7.20 12.50 -1 2 22 -12.50 15.80 0 -2 -22 4.00 13.30 0 2 22 19.60 25.70 0 2 22 -1.10 15.20 0 2 22 -10.70 16.00 0 -7 23 13.90 35.80 1 -7 23 56.59 51.49 -2 -6 23 -65.29 43.20 1 6 -23 -8.90 12.10 -1 -6 23 -25.40 17.30 -1 -6 23 13.50 16.60 -1 -6 23 -24.00 12.60 -1 -6 23 -46.60 38.40 0 6 -23 4.20 14.20 0 6 -23 -1.10 13.30 0 6 -23 -26.80 11.00 0 -6 23 -11.00 12.40 0 -6 23 56.69 38.80 0 -6 23 -8.30 15.50 0 -6 23 15.90 17.40 -1 6 -23 14.80 13.60 -1 6 -23 15.30 14.20 -1 6 -23 23.90 12.30 1 -6 23 7.20 13.60 1 -6 23 23.80 17.30 1 -6 23 24.10 17.20 -2 6 -23 -0.60 12.90 -2 6 -23 -2.20 12.30 -2 6 -23 -13.00 13.20 2 -6 23 -3.30 14.00 2 -6 23 -10.10 16.40 2 -6 23 5.80 17.80 -4 -5 23 -67.39 49.10 -3 -5 23 -59.89 46.10 2 5 -23 -4.30 11.20 -2 -5 23 -21.10 15.70 -2 -5 23 13.20 11.70 -2 -5 23 -8.70 38.00 -2 -5 23 -21.10 14.10 1 5 -23 -3.70 14.00 1 5 -23 -9.30 10.50 -1 -5 23 -17.10 16.00 -1 -5 23 -6.10 11.90 -1 -5 23 -4.90 16.00 0 5 -23 -14.40 13.00 0 -5 23 -8.90 35.00 0 -5 23 -18.00 11.80 0 -5 23 -20.60 16.90 0 -5 23 0.70 16.20 -1 5 -23 30.10 13.60 -1 5 -23 -11.30 12.80 1 -5 23 24.60 16.50 1 -5 23 15.50 13.80 1 -5 23 -0.20 17.60 -2 5 -23 6.70 13.20 -2 5 -23 12.80 12.00 -2 5 -23 1.40 19.80 2 -5 23 11.60 15.30 2 -5 23 -0.80 13.90 2 -5 23 -11.70 18.00 -3 5 -23 8.70 16.20 3 -5 23 2.90 32.60 3 -5 23 -0.80 14.50 3 -5 23 27.90 18.00 3 4 -23 -6.80 10.90 3 4 -23 4.70 9.90 -3 -4 23 12.30 14.60 -3 -4 23 40.10 13.30 -3 -4 23 -10.10 16.90 2 4 -23 -6.60 9.50 2 4 -23 -14.20 10.30 2 4 -23 -14.90 13.10 -2 -4 23 3.10 13.80 -2 -4 23 2.70 16.90 -2 -4 23 -6.90 11.40 1 4 -23 -22.40 14.20 1 4 -23 -3.90 8.90 1 4 -23 -19.60 11.10 -1 -4 23 -13.10 14.10 -1 -4 23 16.10 16.90 -1 -4 23 -10.30 11.20 0 4 -23 36.30 10.70 0 4 -23 38.80 13.20 0 4 -23 53.99 11.80 0 -4 23 -18.00 43.30 0 -4 23 46.30 14.00 0 -4 23 16.40 17.30 0 -4 23 27.70 17.20 -1 4 -23 6.40 10.80 -1 4 -23 26.50 11.00 -1 4 -23 19.40 12.60 1 -4 23 2.40 16.70 1 -4 23 -17.50 13.50 1 -4 23 7.50 16.30 -2 4 -23 31.70 12.00 -2 4 -23 19.50 13.30 -2 4 -23 -3.40 11.20 2 -4 23 15.20 16.40 2 -4 23 2.80 14.20 2 -4 23 9.00 16.40 -3 4 -23 -18.30 11.90 3 -4 23 5.80 16.60 3 -4 23 -17.60 21.40 3 -4 23 -17.90 15.00 3 3 -23 -4.10 11.00 3 3 -23 -27.50 13.70 3 3 -23 24.40 10.50 -3 -3 23 -2.90 15.70 -3 -3 23 8.80 18.90 -3 -3 23 8.20 12.30 2 3 -23 3.10 12.80 2 3 -23 -8.30 11.30 2 3 -23 -0.20 9.00 -2 -3 23 -2.30 14.50 -2 -3 23 -8.80 11.60 -2 -3 23 8.00 16.00 1 3 -23 16.90 11.20 1 3 -23 15.80 12.80 1 3 -23 -1.20 9.40 -1 -3 23 6.80 14.70 -1 -3 23 -14.70 12.00 -1 -3 23 -11.40 13.30 0 3 -23 13.30 11.50 0 3 -23 -5.40 12.20 0 3 -23 -16.40 9.60 0 -3 23 11.30 15.00 0 -3 23 -0.10 14.10 0 -3 23 1.20 11.40 -1 3 -23 7.90 10.40 -1 3 -23 1.30 13.10 -1 3 -23 -9.30 10.80 1 -3 23 11.30 16.10 1 -3 23 -26.40 15.20 1 -3 23 -28.20 11.50 -2 3 -23 15.70 11.80 -2 3 -23 16.80 13.30 -2 3 -23 7.50 15.20 -2 3 -23 14.80 12.10 2 -3 23 21.70 15.50 2 -3 23 17.40 16.50 2 -3 23 -11.70 15.30 -3 3 -23 2.60 14.30 3 -3 23 12.70 14.60 3 -3 23 -9.30 20.90 4 2 -23 3.20 11.00 4 2 -23 -4.20 10.30 -4 -2 23 1.90 15.00 -4 -2 23 5.70 12.60 -4 -2 23 -35.10 19.20 3 2 -23 17.70 10.50 3 2 -23 16.90 10.00 3 2 -23 21.60 13.40 -3 -2 23 -35.50 15.50 -3 -2 23 24.50 13.20 -3 -2 23 -14.70 15.80 2 2 -23 27.10 13.50 2 2 -23 -11.00 10.20 2 2 -23 29.30 10.60 -2 -2 23 -2.10 17.40 -2 -2 23 24.40 16.30 -2 -2 23 6.90 12.40 1 2 -23 13.90 10.30 1 2 -23 -7.50 10.00 1 2 -23 -6.00 12.30 1 2 -23 1.40 12.20 -1 -2 23 -30.50 13.50 -1 -2 23 -15.50 10.60 -1 -2 23 4.70 14.90 0 2 -23 4.90 12.90 0 2 -23 2.50 12.80 0 2 -23 11.10 10.90 0 2 -23 34.90 11.40 0 -2 23 -1.10 14.50 0 -2 23 -0.90 13.30 0 -2 23 4.90 16.00 -1 2 -23 21.10 12.00 -1 2 -23 40.70 14.80 -1 2 -23 33.90 13.30 1 -2 23 14.90 13.00 1 -2 23 6.40 16.00 1 -2 23 49.80 16.60 -2 2 -23 -4.30 13.70 -2 2 -23 10.00 12.30 -2 2 -23 39.10 15.40 2 -2 23 -1.10 13.30 2 -2 23 -18.90 14.70 2 -2 23 -17.10 15.80 4 1 -23 -1.20 10.10 4 1 -23 16.70 10.20 -4 -1 23 -21.20 14.30 -4 -1 23 1.80 11.00 -4 -1 23 -9.50 16.70 3 1 -23 17.70 10.00 3 1 -23 15.70 12.70 3 1 -23 22.80 12.30 -3 -1 23 13.20 15.60 -3 -1 23 11.60 12.70 -3 -1 23 -2.90 15.60 2 1 -23 5.80 12.90 2 1 -23 21.20 11.00 2 1 -23 3.30 11.50 -2 -1 23 -17.90 15.50 -2 -1 23 -1.90 14.00 -2 -1 23 -21.20 10.60 1 1 -23 18.80 10.90 1 1 -23 14.10 12.90 1 1 -23 18.40 12.50 -1 -1 23 3.90 14.80 -1 -1 23 -4.80 14.70 -1 -1 23 5.50 11.60 0 1 -23 5.50 9.80 0 1 -23 22.30 12.60 0 1 -23 9.40 13.70 0 -1 23 25.30 16.50 0 -1 23 -33.20 14.30 0 -1 23 17.40 12.30 -1 1 -23 29.80 14.90 -1 1 -23 0.10 12.00 -1 1 -23 2.30 13.70 1 -1 23 22.10 15.90 1 -1 23 21.60 14.60 2 -1 23 -16.80 19.40 3 0 -23 17.20 13.70 3 0 -23 29.10 11.40 3 0 -23 22.00 11.90 -3 0 23 -30.20 15.50 -3 0 23 -2.00 17.70 -3 0 23 7.00 13.20 2 0 -23 -2.40 12.00 2 0 -23 6.20 13.60 2 0 -23 8.10 10.50 -2 0 23 -20.80 12.80 -2 0 23 -12.80 14.70 -2 0 23 -26.60 16.50 1 0 -23 7.80 13.90 1 0 -23 7.80 11.30 -1 0 23 -26.30 16.40 -1 0 23 -4.10 11.80 -1 0 23 6.00 15.20 0 0 -23 7.00 14.50 0 0 -23 12.50 12.00 0 0 -23 36.50 16.30 0 0 23 -6.90 16.60 0 0 23 -3.70 15.60 0 0 23 4.30 14.70 -2 1 23 7.00 13.20 -2 -5 24 -2.30 48.40 -1 -5 24 5.80 45.50 -1 -4 24 -68.69 47.60 -1 -3 24 -8.60 18.90 -1 -3 24 -6.80 13.90 0 -3 24 23.30 13.30 0 -3 24 31.40 21.50 -1 -2 24 10.40 19.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 28011 _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 O1 O 0.62038(12) 0.68423(12) 0.03052(6) 0.0339(3) Uani 1 1 d . . . . . O2 O 0.93694(14) 0.85034(14) 0.13628(7) 0.0466(4) Uani 1 1 d . . . . . O3 O 0.60182(13) 0.63786(13) 0.47308(7) 0.0352(3) Uani 1 1 d . . . . . O4 O 0.74066(16) 0.72203(16) 0.32265(8) 0.0536(4) Uani 1 1 d . . . . . O5 O 0.97201(19) 0.7248(2) 0.24598(11) 0.0772(6) Uani 1 1 d . . . . . H5A H 0.9617 0.7609 0.2127 0.116 Uiso 1 1 d G . . . . H5B H 0.9041 0.7240 0.2692 0.116 Uiso 1 1 d G . . . . N1 N 0.80587(16) 0.79854(15) 0.11244(8) 0.0350(4) Uani 1 1 d . . . . . N2 N 0.72412(17) 0.69791(16) 0.38485(9) 0.0382(4) Uani 1 1 d . . . . . C1 C 0.9937(3) 0.7391(3) -0.12156(13) 0.0684(8) Uani 1 1 d . . . . . H1 H 1.0468 0.7528 -0.1586 0.082 Uiso 1 1 calc R . . . . C2 C 0.9448(2) 0.8357(3) -0.08818(13) 0.0599(7) Uani 1 1 d . . . . . H2 H 0.9641 0.9147 -0.1026 0.072 Uiso 1 1 calc R . . . . C3 C 0.8670(2) 0.8143(2) -0.03318(11) 0.0475(5) Uani 1 1 d . . . . . H3 H 0.8336 0.8793 -0.0107 0.057 Uiso 1 1 calc R . . . . C4 C 0.83762(19) 0.6976(2) -0.01065(10) 0.0372(5) Uani 1 1 d . . . . . C5 C 0.75116(19) 0.67885(18) 0.04948(10) 0.0327(4) Uani 1 1 d . . . . . C6 C 0.5716(2) 0.72300(19) 0.09781(10) 0.0334(4) Uani 1 1 d . . . . . C7 C 0.4569(2) 0.77423(19) 0.08555(11) 0.0367(5) Uani 1 1 d . . . . . C8 C 0.4418(2) 0.8181(2) 0.02577(12) 0.0506(6) Uani 1 1 d . . . . . H8 H 0.5063 0.8217 -0.0063 0.061 Uiso 1 1 calc R . . . . C9 C 0.3314(3) 0.8571(3) 0.01284(14) 0.0670(7) Uani 1 1 d . . . . . H9 H 0.3225 0.8861 -0.0280 0.080 Uiso 1 1 calc R . . . . C10 C 0.2356(3) 0.8534(3) 0.05932(17) 0.0679(8) Uani 1 1 d . . . . . H10 H 0.1606 0.8778 0.0499 0.081 Uiso 1 1 calc R . . . . C11 C 0.7306(2) 0.55481(19) 0.07681(10) 0.0367(5) Uani 1 1 d . . . . . H11A H 0.8200 0.5525 0.0914 0.044 Uiso 1 1 calc R . . . . H11B H 0.6835 0.4758 0.0387 0.044 Uiso 1 1 calc R . . . . C12 C 0.6456(2) 0.55275(19) 0.14022(10) 0.0358(5) Uani 1 1 d . . . . . H12 H 0.7070 0.6188 0.1813 0.043 Uiso 1 1 calc R . . . . C13 C 0.5257(2) 0.59892(19) 0.12766(11) 0.0374(5) Uani 1 1 d . . . . . H13A H 0.4890 0.6193 0.1722 0.045 Uiso 1 1 calc R . . . . H13B H 0.4527 0.5273 0.0945 0.045 Uiso 1 1 calc R . . . . C14 C 0.3613(3) 0.7746(3) 0.13290(15) 0.0624(7) Uani 1 1 d . . . . . H14 H 0.3709 0.7482 0.1745 0.075 Uiso 1 1 calc R . . . . C15 C 0.2515(3) 0.8136(3) 0.11963(18) 0.0737(8) Uani 1 1 d . . . . . H15 H 0.1879 0.8125 0.1522 0.088 Uiso 1 1 calc R . . . . C16 C 0.7045(2) 0.82456(19) 0.14053(10) 0.0351(5) Uani 1 1 d . . . . . C17 C 0.7217(3) 0.9218(2) 0.20854(12) 0.0540(6) Uani 1 1 d . . . . . H17A H 0.8147 0.9850 0.2180 0.081 Uiso 1 1 calc GR . . . . H17B H 0.7032 0.8760 0.2459 0.081 Uiso 1 1 calc GR . . . . H17C H 0.6586 0.9678 0.2063 0.081 Uiso 1 1 calc GR . . . . C18 C 0.6031(2) 0.4182(2) 0.15908(10) 0.0389(5) Uani 1 1 d . . . . . C19 C 0.4689(2) 0.3279(2) 0.14641(12) 0.0488(6) Uani 1 1 d . . . . . H19 H 0.3999 0.3487 0.1254 0.059 Uiso 1 1 calc R . . . . C20 C 0.4359(3) 0.2070(2) 0.16452(13) 0.0611(7) Uani 1 1 d . . . . . H20 H 0.3450 0.1475 0.1554 0.073 Uiso 1 1 calc R . . . . C21 C 0.5350(3) 0.1743(3) 0.19553(14) 0.0675(8) Uani 1 1 d . . . . . H21 H 0.5123 0.0928 0.2076 0.081 Uiso 1 1 calc R . . . . C22 C 0.6694(3) 0.2630(3) 0.20885(13) 0.0628(7) Uani 1 1 d . . . . . H22 H 0.7375 0.2409 0.2299 0.075 Uiso 1 1 calc R . . . . C23 C 0.7040(3) 0.3850(2) 0.19117(12) 0.0507(6) Uani 1 1 d . . . . . H23 H 0.7949 0.4445 0.2008 0.061 Uiso 1 1 calc R . . . . C24 C 0.8867(2) 0.6012(2) -0.04494(12) 0.0518(6) Uani 1 1 d . . . . . H24 H 0.8675 0.5220 -0.0308 0.062 Uiso 1 1 calc R . . . . C25 C 0.9642(3) 0.6225(3) -0.10025(13) 0.0685(8) Uani 1 1 d . . . . . H25 H 0.9967 0.5571 -0.1233 0.082 Uiso 1 1 calc R . . . . C26 C 0.8439(3) 0.9072(3) 0.70820(13) 0.0649(7) Uani 1 1 d . . . . . H26 H 0.8659 0.9611 0.7544 0.078 Uiso 1 1 calc R . . . . C27 C 0.8159(3) 0.9563(2) 0.65264(14) 0.0615(7) Uani 1 1 d . . . . . H27 H 0.8174 1.0435 0.6612 0.074 Uiso 1 1 calc R . . . . C28 C 0.7855(2) 0.8770(2) 0.58439(12) 0.0494(6) Uani 1 1 d . . . . . H28 H 0.7663 0.9113 0.5471 0.059 Uiso 1 1 calc R . . . . C29 C 0.7830(2) 0.7473(2) 0.57018(11) 0.0379(5) Uani 1 1 d . . . . . C30 C 0.74587(19) 0.66251(19) 0.49482(10) 0.0349(5) Uani 1 1 d . . . . . C31 C 0.5872(2) 0.60222(19) 0.39798(10) 0.0344(4) Uani 1 1 d . . . . . C32 C 0.4656(2) 0.6272(2) 0.36875(11) 0.0384(5) Uani 1 1 d . . . . . C33 C 0.4185(2) 0.7199(2) 0.40945(13) 0.0526(6) Uani 1 1 d . . . . . H33 H 0.4656 0.7698 0.4540 0.063 Uiso 1 1 calc R . . . . C34 C 0.3030(3) 0.7389(3) 0.38482(16) 0.0683(7) Uani 1 1 d . . . . . H34 H 0.2714 0.8001 0.4133 0.082 Uiso 1 1 calc R . . . . C35 C 0.2337(3) 0.6688(3) 0.31879(17) 0.0701(8) Uani 1 1 d . . . . . H35 H 0.1559 0.6825 0.3021 0.084 Uiso 1 1 calc R . . . . C36 C 0.8147(2) 0.73201(19) 0.43992(11) 0.0377(5) Uani 1 1 d . . . . . C37 C 0.3953(2) 0.5571(2) 0.30236(12) 0.0534(6) Uani 1 1 d . . . . . H37 H 0.4255 0.4949 0.2739 0.064 Uiso 1 1 calc R . . . . C38 C 0.2802(3) 0.5788(3) 0.27778(14) 0.0656(7) Uani 1 1 d . . . . . H38 H 0.2340 0.5313 0.2327 0.079 Uiso 1 1 calc R . . . . C39 C 0.5879(2) 0.46145(19) 0.37293(11) 0.0401(5) Uani 1 1 d . . . . . H39A H 0.5816 0.4378 0.3214 0.048 Uiso 1 1 calc R . . . . H39B H 0.5075 0.3993 0.3866 0.048 Uiso 1 1 calc R . . . . C40 C 0.7191(2) 0.44797(19) 0.40455(11) 0.0394(5) Uani 1 1 d . . . . . H40 H 0.7942 0.4889 0.3784 0.047 Uiso 1 1 calc R . . . . C41 C 0.7602(2) 0.52563(19) 0.48309(11) 0.0390(5) Uani 1 1 d . . . . . H41A H 0.7017 0.4746 0.5123 0.047 Uiso 1 1 calc R . . . . H41B H 0.8550 0.5373 0.4976 0.047 Uiso 1 1 calc R . . . . C42 C 0.7096(2) 0.3046(2) 0.39708(11) 0.0418(5) Uani 1 1 d . . . . . C43 C 0.5880(3) 0.2033(2) 0.39905(16) 0.0698(8) Uani 1 1 d . . . . . H43 H 0.5071 0.2217 0.4030 0.084 Uiso 1 1 calc R . . . . C44 C 0.5841(3) 0.0750(3) 0.39519(17) 0.0822(9) Uani 1 1 d . . . . . H44 H 0.5012 0.0082 0.3971 0.099 Uiso 1 1 calc R . . . . C45 C 0.7014(3) 0.0457(3) 0.38857(13) 0.0664(7) Uani 1 1 d . . . . . H45 H 0.6987 -0.0407 0.3862 0.080 Uiso 1 1 calc R . . . . C46 C 0.8220(3) 0.1435(3) 0.38553(14) 0.0654(7) Uani 1 1 d . . . . . H46 H 0.9020 0.1239 0.3805 0.078 Uiso 1 1 calc R . . . . C47 C 0.8261(2) 0.2715(2) 0.38985(13) 0.0562(6) Uani 1 1 d . . . . . H47 H 0.9096 0.3375 0.3879 0.067 Uiso 1 1 calc R . . . . C48 C 0.9615(2) 0.8066(3) 0.44052(14) 0.0603(7) Uani 1 1 d . . . . . H48A H 1.0027 0.7493 0.4127 0.090 Uiso 1 1 calc GR . . . . H48B H 1.0063 0.8377 0.4886 0.090 Uiso 1 1 calc GR . . . . H48C H 0.9720 0.8816 0.4207 0.090 Uiso 1 1 calc GR . . . . C49 C 0.8101(2) 0.6986(2) 0.62689(12) 0.0500(6) Uani 1 1 d . . . . . H49 H 0.8086 0.6115 0.6189 0.060 Uiso 1 1 calc R . . . . C50 C 0.8393(3) 0.7787(3) 0.69510(13) 0.0659(7) Uani 1 1 d . . . . . H50 H 0.8560 0.7445 0.7328 0.079 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 O1 0.0308(7) 0.0404(8) 0.0318(7) 0.0077(6) 0.0027(6) 0.0152(6) O2 0.0306(8) 0.0524(9) 0.0480(9) 0.0104(7) -0.0057(6) 0.0062(7) O3 0.0315(7) 0.0406(8) 0.0357(8) 0.0133(6) 0.0083(6) 0.0127(6) O4 0.0619(10) 0.0647(10) 0.0418(9) 0.0282(8) 0.0173(7) 0.0219(8) O5 0.0548(12) 0.1122(16) 0.0769(14) 0.0404(12) 0.0052(9) 0.0352(11) N1 0.0344(10) 0.0331(9) 0.0350(9) 0.0090(7) -0.0001(7) 0.0089(8) N2 0.0403(10) 0.0381(10) 0.0409(10) 0.0180(8) 0.0139(8) 0.0140(8) C1 0.0537(16) 0.113(2) 0.0491(15) 0.0329(16) 0.0188(12) 0.0338(16) C2 0.0508(15) 0.0748(18) 0.0532(15) 0.0307(13) 0.0094(12) 0.0121(13) C3 0.0452(13) 0.0531(14) 0.0439(13) 0.0151(11) 0.0075(10) 0.0150(11) C4 0.0290(11) 0.0465(12) 0.0348(11) 0.0096(9) 0.0017(9) 0.0122(9) C5 0.0275(10) 0.0357(11) 0.0336(11) 0.0060(8) 0.0000(8) 0.0119(9) C6 0.0373(11) 0.0342(10) 0.0315(10) 0.0084(8) 0.0079(9) 0.0159(9) C7 0.0323(11) 0.0322(11) 0.0460(12) 0.0081(9) 0.0048(9) 0.0132(9) C8 0.0554(15) 0.0576(14) 0.0503(14) 0.0170(11) 0.0084(11) 0.0319(12) C9 0.0764(19) 0.0735(18) 0.0659(17) 0.0172(14) -0.0044(15) 0.0467(16) C10 0.0471(15) 0.0561(16) 0.103(2) 0.0114(15) -0.0055(15) 0.0287(13) C11 0.0375(11) 0.0372(11) 0.0381(11) 0.0088(9) 0.0038(9) 0.0171(9) C12 0.0384(11) 0.0347(11) 0.0347(11) 0.0082(9) 0.0013(9) 0.0141(9) C13 0.0374(11) 0.0373(11) 0.0400(12) 0.0120(9) 0.0081(9) 0.0147(9) C14 0.0616(16) 0.0729(17) 0.0785(18) 0.0397(14) 0.0319(14) 0.0409(14) C15 0.0520(16) 0.0741(19) 0.119(3) 0.0416(18) 0.0382(16) 0.0392(15) C16 0.0398(12) 0.0323(10) 0.0358(11) 0.0096(9) 0.0036(9) 0.0153(9) C17 0.0652(16) 0.0486(14) 0.0462(13) -0.0014(11) 0.0009(11) 0.0265(12) C18 0.0513(13) 0.0394(12) 0.0315(11) 0.0109(9) 0.0092(9) 0.0213(11) C19 0.0556(15) 0.0392(12) 0.0498(13) 0.0133(10) 0.0029(11) 0.0137(11) C20 0.0702(17) 0.0432(14) 0.0681(17) 0.0208(12) 0.0119(14) 0.0132(13) C21 0.094(2) 0.0499(15) 0.0754(19) 0.0323(14) 0.0310(16) 0.0344(16) C22 0.087(2) 0.0687(17) 0.0628(16) 0.0324(14) 0.0230(14) 0.0533(17) C23 0.0563(15) 0.0555(14) 0.0533(14) 0.0220(11) 0.0149(11) 0.0303(12) C24 0.0522(14) 0.0660(15) 0.0477(14) 0.0160(12) 0.0126(11) 0.0323(13) C25 0.0647(17) 0.106(2) 0.0534(16) 0.0200(15) 0.0219(13) 0.0521(17) C26 0.0698(18) 0.0599(17) 0.0446(15) -0.0004(13) 0.0058(12) 0.0063(14) C27 0.0716(17) 0.0437(14) 0.0576(16) 0.0041(12) 0.0116(13) 0.0112(12) C28 0.0575(15) 0.0411(13) 0.0457(13) 0.0104(10) 0.0058(11) 0.0130(11) C29 0.0312(11) 0.0383(12) 0.0404(12) 0.0112(9) 0.0077(9) 0.0063(9) C30 0.0283(11) 0.0376(11) 0.0388(11) 0.0124(9) 0.0066(9) 0.0098(9) C31 0.0353(11) 0.0373(11) 0.0331(11) 0.0136(9) 0.0087(8) 0.0125(9) C32 0.0363(11) 0.0409(12) 0.0428(12) 0.0205(10) 0.0076(9) 0.0131(10) C33 0.0532(15) 0.0491(13) 0.0604(15) 0.0137(11) 0.0021(12) 0.0251(12) C34 0.0619(17) 0.0717(18) 0.087(2) 0.0249(16) 0.0066(15) 0.0407(15) C35 0.0497(16) 0.085(2) 0.094(2) 0.0456(18) 0.0059(15) 0.0332(15) C36 0.0344(11) 0.0355(11) 0.0422(12) 0.0122(9) 0.0087(10) 0.0092(9) C37 0.0529(15) 0.0671(16) 0.0448(14) 0.0175(12) 0.0053(11) 0.0251(13) C38 0.0556(16) 0.084(2) 0.0580(16) 0.0288(15) -0.0073(13) 0.0204(15) C39 0.0398(12) 0.0365(11) 0.0435(12) 0.0113(9) 0.0059(9) 0.0122(10) C40 0.0396(12) 0.0360(11) 0.0442(12) 0.0125(9) 0.0112(9) 0.0133(9) C41 0.0347(11) 0.0400(12) 0.0446(12) 0.0149(10) 0.0043(9) 0.0135(9) C42 0.0505(13) 0.0392(12) 0.0387(12) 0.0092(9) 0.0065(10) 0.0202(11) C43 0.0616(17) 0.0469(15) 0.112(2) 0.0286(15) 0.0355(16) 0.0251(13) C44 0.082(2) 0.0457(16) 0.126(3) 0.0296(16) 0.0397(19) 0.0232(15) C45 0.102(2) 0.0470(15) 0.0610(16) 0.0111(12) 0.0120(15) 0.0410(17) C46 0.0691(18) 0.0601(17) 0.0756(18) 0.0089(14) -0.0015(14) 0.0401(15) C47 0.0470(14) 0.0500(14) 0.0721(17) 0.0101(12) -0.0017(12) 0.0220(12) C48 0.0394(13) 0.0645(16) 0.0653(16) 0.0174(13) 0.0092(12) 0.0028(12) C49 0.0554(14) 0.0488(13) 0.0431(13) 0.0128(11) 0.0049(11) 0.0147(11) C50 0.0758(19) 0.0726(19) 0.0417(15) 0.0168(13) -0.0014(12) 0.0166(15) 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 O1 C6 104.62(14) . . ? C31 O3 C30 104.80(14) . . ? H5A O5 H5B 104.5 . . ? O2 N1 C5 120.79(15) . . ? C16 N1 O2 128.73(17) . . ? C16 N1 C5 109.92(16) . . ? O4 N2 C31 120.52(16) . . ? C36 N2 O4 129.29(17) . . ? C36 N2 C31 109.68(16) . . ? C2 C1 H1 120.0 . . ? C25 C1 H1 120.0 . . ? C25 C1 C2 120.0(2) . . ? C1 C2 H2 120.3 . . ? C1 C2 C3 119.3(2) . . ? C3 C2 H2 120.3 . . ? C2 C3 H3 119.4 . . ? C2 C3 C4 121.3(2) . . ? C4 C3 H3 119.4 . . ? C3 C4 C5 119.08(18) . . ? C24 C4 C3 118.7(2) . . ? C24 C4 C5 122.18(19) . . ? O1 C5 N1 100.36(14) . . ? O1 C5 C4 109.58(15) . . ? O1 C5 C11 109.09(15) . . ? N1 C5 C11 107.57(16) . . ? C4 C5 N1 111.21(16) . . ? C4 C5 C11 117.62(16) . . ? O1 C6 C7 109.12(15) . . ? O1 C6 C13 106.37(15) . . ? O1 C6 C16 100.51(15) . . ? C7 C6 C13 113.42(16) . . ? C7 C6 C16 116.42(17) . . ? C16 C6 C13 109.76(16) . . ? C8 C7 C6 121.17(18) . . ? C8 C7 C14 117.7(2) . . ? C14 C7 C6 121.10(19) . . ? C7 C8 H8 119.6 . . ? C7 C8 C9 120.7(2) . . ? C9 C8 H8 119.6 . . ? C8 C9 H9 119.6 . . ? C10 C9 C8 120.8(3) . . ? C10 C9 H9 119.6 . . ? C9 C10 H10 120.5 . . ? C15 C10 C9 119.1(2) . . ? C15 C10 H10 120.5 . . ? C5 C11 H11A 109.3 . . ? C5 C11 H11B 109.3 . . ? C5 C11 C12 111.56(15) . . ? H11A C11 H11B 108.0 . . ? C12 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? C11 C12 H12 106.6 . . ? C13 C12 C11 110.97(16) . . ? C13 C12 H12 106.6 . . ? C18 C12 C11 111.57(16) . . ? C18 C12 H12 106.6 . . ? C18 C12 C13 114.01(17) . . ? C6 C13 H13A 109.4 . . ? C6 C13 H13B 109.4 . . ? C12 C13 C6 111.31(16) . . ? C12 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C7 C14 H14 119.4 . . ? C7 C14 C15 121.2(2) . . ? C15 C14 H14 119.4 . . ? C10 C15 C14 120.5(2) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? N1 C16 C6 107.78(17) . . ? N1 C16 C17 123.37(19) . . ? C17 C16 C6 128.10(18) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C12 123.37(19) . . ? C19 C18 C23 118.2(2) . . ? C23 C18 C12 118.4(2) . . ? C18 C19 H19 119.5 . . ? C20 C19 C18 121.0(2) . . ? C20 C19 H19 119.5 . . ? C19 C20 H20 119.7 . . ? C21 C20 C19 120.6(3) . . ? C21 C20 H20 119.7 . . ? C20 C21 H21 120.3 . . ? C20 C21 C22 119.4(2) . . ? C22 C21 H21 120.3 . . ? C21 C22 H22 119.7 . . ? C21 C22 C23 120.7(2) . . ? C23 C22 H22 119.7 . . ? C18 C23 H23 120.0 . . ? C22 C23 C18 120.1(2) . . ? C22 C23 H23 120.0 . . ? C4 C24 H24 120.0 . . ? C25 C24 C4 120.0(2) . . ? C25 C24 H24 120.0 . . ? C1 C25 C24 120.6(2) . . ? C1 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 H26 120.3 . . ? C50 C26 H26 120.3 . . ? C50 C26 C27 119.3(2) . . ? C26 C27 H27 119.9 . . ? C26 C27 C28 120.2(2) . . ? C28 C27 H27 119.9 . . ? C27 C28 H28 119.4 . . ? C27 C28 C29 121.1(2) . . ? C29 C28 H28 119.4 . . ? C28 C29 C30 119.48(18) . . ? C28 C29 C49 118.1(2) . . ? C49 C29 C30 122.42(19) . . ? O3 C30 C29 107.86(15) . . ? O3 C30 C36 100.88(15) . . ? O3 C30 C41 106.60(15) . . ? C29 C30 C36 114.79(17) . . ? C29 C30 C41 115.72(17) . . ? C36 C30 C41 109.59(16) . . ? O3 C31 N2 100.27(15) . . ? O3 C31 C32 109.97(15) . . ? O3 C31 C39 108.90(15) . . ? C32 C31 N2 112.63(16) . . ? C32 C31 C39 116.36(17) . . ? C39 C31 N2 107.47(16) . . ? C33 C32 C31 120.1(2) . . ? C37 C32 C31 121.67(19) . . ? C37 C32 C33 118.2(2) . . ? C32 C33 H33 119.6 . . ? C34 C33 C32 120.7(2) . . ? C34 C33 H33 119.6 . . ? C33 C34 H34 119.7 . . ? C35 C34 C33 120.7(3) . . ? C35 C34 H34 119.7 . . ? C34 C35 H35 120.4 . . ? C38 C35 C34 119.2(2) . . ? C38 C35 H35 120.4 . . ? N2 C36 C30 107.90(17) . . ? N2 C36 C48 123.30(19) . . ? C48 C36 C30 128.05(19) . . ? C32 C37 H37 119.8 . . ? C32 C37 C38 120.4(2) . . ? C38 C37 H37 119.8 . . ? C35 C38 C37 120.8(3) . . ? C35 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C31 C39 H39A 109.2 . . ? C31 C39 H39B 109.2 . . ? C31 C39 C40 112.01(17) . . ? H39A C39 H39B 107.9 . . ? C40 C39 H39A 109.2 . . ? C40 C39 H39B 109.2 . . ? C39 C40 H40 107.1 . . ? C41 C40 C39 111.33(16) . . ? C41 C40 H40 107.1 . . ? C42 C40 C39 114.11(17) . . ? C42 C40 H40 107.1 . . ? C42 C40 C41 109.65(16) . . ? C30 C41 C40 111.15(16) . . ? C30 C41 H41A 109.4 . . ? C30 C41 H41B 109.4 . . ? C40 C41 H41A 109.4 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C43 C42 C40 122.6(2) . . ? C43 C42 C47 117.1(2) . . ? C47 C42 C40 120.3(2) . . ? C42 C43 H43 119.5 . . ? C42 C43 C44 121.1(2) . . ? C44 C43 H43 119.5 . . ? C43 C44 H44 119.8 . . ? C45 C44 C43 120.4(3) . . ? C45 C44 H44 119.8 . . ? C44 C45 H45 120.2 . . ? C46 C45 C44 119.5(2) . . ? C46 C45 H45 120.2 . . ? C45 C46 H46 119.9 . . ? C45 C46 C47 120.2(2) . . ? C47 C46 H46 119.9 . . ? C42 C47 H47 119.1 . . ? C46 C47 C42 121.7(2) . . ? C46 C47 H47 119.1 . . ? C36 C48 H48A 109.5 . . ? C36 C48 H48B 109.5 . . ? C36 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C29 C49 H49 119.9 . . ? C50 C49 C29 120.3(2) . . ? C50 C49 H49 119.9 . . ? C26 C50 C49 121.1(2) . . ? C26 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? 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 O1 C5 1.417(2) . ? O1 C6 1.449(2) . ? O2 N1 1.303(2) . ? O3 C30 1.454(2) . ? O3 C31 1.412(2) . ? O4 N2 1.298(2) . ? O5 H5A 0.8501 . ? O5 H5B 0.8499 . ? N1 C5 1.509(3) . ? N1 C16 1.292(3) . ? N2 C31 1.523(3) . ? N2 C36 1.295(3) . ? C1 H1 0.9300 . ? C1 C2 1.377(4) . ? C1 C25 1.372(4) . ? C2 H2 0.9300 . ? C2 C3 1.378(3) . ? C3 H3 0.9300 . ? C3 C4 1.385(3) . ? C4 C5 1.508(3) . ? C4 C24 1.381(3) . ? C5 C11 1.521(3) . ? C6 C7 1.511(3) . ? C6 C13 1.533(3) . ? C6 C16 1.514(3) . ? C7 C8 1.375(3) . ? C7 C14 1.380(3) . ? C8 H8 0.9300 . ? C8 C9 1.385(3) . ? C9 H9 0.9300 . ? C9 C10 1.365(4) . ? C10 H10 0.9300 . ? C10 C15 1.361(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.542(3) . ? C12 H12 0.9800 . ? C12 C13 1.526(3) . ? C12 C18 1.523(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14 0.9300 . ? C14 C15 1.381(3) . ? C15 H15 0.9300 . ? C16 C17 1.465(3) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.382(3) . ? C18 C23 1.390(3) . ? C19 H19 0.9300 . ? C19 C20 1.382(3) . ? C20 H20 0.9300 . ? C20 C21 1.361(4) . ? C21 H21 0.9300 . ? C21 C22 1.378(4) . ? C22 H22 0.9300 . ? C22 C23 1.388(3) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C24 C25 1.381(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C26 C27 1.371(4) . ? C26 C50 1.361(4) . ? C27 H27 0.9300 . ? C27 C28 1.374(3) . ? C28 H28 0.9300 . ? C28 C29 1.382(3) . ? C29 C30 1.507(3) . ? C29 C49 1.384(3) . ? C30 C36 1.509(3) . ? C30 C41 1.529(3) . ? C31 C32 1.498(3) . ? C31 C39 1.518(3) . ? C32 C33 1.384(3) . ? C32 C37 1.377(3) . ? C33 H33 0.9300 . ? C33 C34 1.372(3) . ? C34 H34 0.9300 . ? C34 C35 1.368(4) . ? C35 H35 0.9300 . ? C35 C38 1.361(4) . ? C36 C48 1.462(3) . ? C37 H37 0.9300 . ? C37 C38 1.383(3) . ? C38 H38 0.9300 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 C40 1.539(3) . ? C40 H40 0.9800 . ? C40 C41 1.538(3) . ? C40 C42 1.518(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.379(3) . ? C42 C47 1.380(3) . ? C43 H43 0.9300 . ? C43 C44 1.382(4) . ? C44 H44 0.9300 . ? C44 C45 1.365(4) . ? C45 H45 0.9300 . ? C45 C46 1.358(4) . ? C46 H46 0.9300 . ? C46 C47 1.376(3) . ? C47 H47 0.9300 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49 0.9300 . ? C49 C50 1.377(3) . ? C50 H50 0.9300 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C5 C11 C12 -57.0(2) . . . . ? O1 C6 C7 C8 -20.5(3) . . . . ? O1 C6 C7 C14 157.5(2) . . . . ? O1 C6 C13 C12 61.0(2) . . . . ? O1 C6 C16 N1 -23.66(19) . . . . ? O1 C6 C16 C17 166.18(19) . . . . ? O2 N1 C5 O1 -163.36(14) . . . . ? O2 N1 C5 C4 -47.5(2) . . . . ? O2 N1 C5 C11 82.64(19) . . . . ? O2 N1 C16 C6 -171.52(16) . . . . ? O2 N1 C16 C17 -0.8(3) . . . . ? O3 C30 C36 N2 -23.22(19) . . . . ? O3 C30 C36 C48 166.6(2) . . . . ? O3 C30 C41 C40 59.8(2) . . . . ? O3 C31 C32 C33 23.9(3) . . . . ? O3 C31 C32 C37 -154.20(19) . . . . ? O3 C31 C39 C40 -56.7(2) . . . . ? O4 N2 C31 O3 -163.03(15) . . . . ? O4 N2 C31 C32 -46.2(2) . . . . ? O4 N2 C31 C39 83.3(2) . . . . ? O4 N2 C36 C30 -172.02(18) . . . . ? O4 N2 C36 C48 -1.2(3) . . . . ? N1 C5 C11 C12 51.1(2) . . . . ? N2 C31 C32 C33 -87.0(2) . . . . ? N2 C31 C32 C37 94.9(2) . . . . ? N2 C31 C39 C40 51.1(2) . . . . ? C1 C2 C3 C4 0.3(3) . . . . ? C2 C1 C25 C24 -0.6(4) . . . . ? C2 C3 C4 C5 -179.6(2) . . . . ? C2 C3 C4 C24 -0.7(3) . . . . ? C3 C4 C5 O1 59.5(2) . . . . ? C3 C4 C5 N1 -50.5(2) . . . . ? C3 C4 C5 C11 -175.15(18) . . . . ? C3 C4 C24 C25 0.4(3) . . . . ? C4 C5 C11 C12 177.50(16) . . . . ? C4 C24 C25 C1 0.2(4) . . . . ? C5 O1 C6 C7 162.15(15) . . . . ? C5 O1 C6 C13 -75.15(17) . . . . ? C5 O1 C6 C16 39.24(17) . . . . ? C5 N1 C16 C6 -0.2(2) . . . . ? C5 N1 C16 C17 170.57(18) . . . . ? C5 C4 C24 C25 179.3(2) . . . . ? C5 C11 C12 C13 41.5(2) . . . . ? C5 C11 C12 C18 169.79(16) . . . . ? C6 O1 C5 N1 -39.04(16) . . . . ? C6 O1 C5 C4 -156.13(15) . . . . ? C6 O1 C5 C11 73.79(17) . . . . ? C6 C7 C8 C9 176.0(2) . . . . ? C6 C7 C14 C15 -175.9(2) . . . . ? C7 C6 C13 C12 -179.04(16) . . . . ? C7 C6 C16 N1 -141.32(17) . . . . ? C7 C6 C16 C17 48.5(3) . . . . ? C7 C8 C9 C10 0.3(4) . . . . ? C7 C14 C15 C10 -0.4(4) . . . . ? C8 C7 C14 C15 2.1(4) . . . . ? C8 C9 C10 C15 1.4(4) . . . . ? C9 C10 C15 C14 -1.4(4) . . . . ? C11 C12 C13 C6 -44.2(2) . . . . ? C11 C12 C18 C19 -108.8(2) . . . . ? C11 C12 C18 C23 71.7(2) . . . . ? C12 C18 C19 C20 179.9(2) . . . . ? C12 C18 C23 C22 -179.69(19) . . . . ? C13 C6 C7 C8 -138.8(2) . . . . ? C13 C6 C7 C14 39.1(3) . . . . ? C13 C6 C16 N1 88.14(19) . . . . ? C13 C6 C16 C17 -82.0(2) . . . . ? C13 C12 C18 C19 17.8(3) . . . . ? C13 C12 C18 C23 -161.65(18) . . . . ? C14 C7 C8 C9 -2.1(3) . . . . ? C16 N1 C5 O1 24.48(19) . . . . ? C16 N1 C5 C4 140.36(17) . . . . ? C16 N1 C5 C11 -89.51(18) . . . . ? C16 C6 C7 C8 92.4(2) . . . . ? C16 C6 C7 C14 -89.7(2) . . . . ? C16 C6 C13 C12 -46.9(2) . . . . ? C18 C12 C13 C6 -171.17(16) . . . . ? C18 C19 C20 C21 0.2(4) . . . . ? C19 C18 C23 C22 0.8(3) . . . . ? C19 C20 C21 C22 0.0(4) . . . . ? C20 C21 C22 C23 0.2(4) . . . . ? C21 C22 C23 C18 -0.6(4) . . . . ? C23 C18 C19 C20 -0.6(3) . . . . ? C24 C4 C5 O1 -119.3(2) . . . . ? C24 C4 C5 N1 130.6(2) . . . . ? C24 C4 C5 C11 6.0(3) . . . . ? C25 C1 C2 C3 0.4(4) . . . . ? C26 C27 C28 C29 -0.2(4) . . . . ? C27 C26 C50 C49 1.6(4) . . . . ? C27 C28 C29 C30 178.6(2) . . . . ? C27 C28 C29 C49 0.9(3) . . . . ? C28 C29 C30 O3 -66.8(2) . . . . ? C28 C29 C30 C36 44.7(3) . . . . ? C28 C29 C30 C41 173.96(18) . . . . ? C28 C29 C49 C50 -0.4(3) . . . . ? C29 C30 C36 N2 -138.87(18) . . . . ? C29 C30 C36 C48 50.9(3) . . . . ? C29 C30 C41 C40 179.77(16) . . . . ? C29 C49 C50 C26 -0.9(4) . . . . ? C30 O3 C31 N2 -38.60(16) . . . . ? C30 O3 C31 C32 -157.40(15) . . . . ? C30 O3 C31 C39 74.01(18) . . . . ? C30 C29 C49 C50 -177.9(2) . . . . ? C31 O3 C30 C29 159.68(15) . . . . ? C31 O3 C30 C36 38.98(17) . . . . ? C31 O3 C30 C41 -75.45(17) . . . . ? C31 N2 C36 C30 -0.3(2) . . . . ? C31 N2 C36 C48 170.47(19) . . . . ? C31 C32 C33 C34 -176.7(2) . . . . ? C31 C32 C37 C38 177.6(2) . . . . ? C31 C39 C40 C41 40.4(2) . . . . ? C31 C39 C40 C42 165.14(16) . . . . ? C32 C31 C39 C40 178.42(16) . . . . ? C32 C33 C34 C35 -1.5(4) . . . . ? C32 C37 C38 C35 -0.4(4) . . . . ? C33 C32 C37 C38 -0.5(3) . . . . ? C33 C34 C35 C38 0.5(4) . . . . ? C34 C35 C38 C37 0.5(4) . . . . ? C36 N2 C31 O3 24.41(19) . . . . ? C36 N2 C31 C32 141.25(18) . . . . ? C36 N2 C31 C39 -89.30(19) . . . . ? C36 C30 C41 C40 -48.5(2) . . . . ? C37 C32 C33 C34 1.5(3) . . . . ? C39 C31 C32 C33 148.3(2) . . . . ? C39 C31 C32 C37 -29.8(3) . . . . ? C39 C40 C41 C30 -42.7(2) . . . . ? C39 C40 C42 C43 -33.0(3) . . . . ? C39 C40 C42 C47 148.7(2) . . . . ? C40 C42 C43 C44 -177.2(2) . . . . ? C40 C42 C47 C46 177.6(2) . . . . ? C41 C30 C36 N2 88.9(2) . . . . ? C41 C30 C36 C48 -81.3(3) . . . . ? C41 C40 C42 C43 92.6(3) . . . . ? C41 C40 C42 C47 -85.6(2) . . . . ? C42 C40 C41 C30 -169.89(16) . . . . ? C42 C43 C44 C45 -0.7(5) . . . . ? C43 C42 C47 C46 -0.7(4) . . . . ? C43 C44 C45 C46 -0.3(5) . . . . ? C44 C45 C46 C47 0.7(4) . . . . ? C45 C46 C47 C42 -0.2(4) . . . . ? C47 C42 C43 C44 1.1(4) . . . . ? C49 C29 C30 O3 110.7(2) . . . . ? C49 C29 C30 C36 -137.7(2) . . . . ? C49 C29 C30 C41 -8.5(3) . . . . ? C50 C26 C27 C28 -1.0(4) . . . . ?