#------------------------------------------------------------------------------ #$Date: 2020-10-06 09:57:52 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257279 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557902.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_1557902 loop_ _publ_author_name 'Okude, Ryo' 'Mori, Genki' 'Yagi, Akiko' 'Itami, Kenichiro' _publ_section_title ; Programmable synthesis of multiply arylated cubanes through C--H metalation and arylation ; _journal_issue 29 _journal_name_full 'Chemical Science' _journal_page_first 7672 _journal_page_last 7675 _journal_paper_doi 10.1039/D0SC01909G _journal_volume 11 _journal_year 2020 _chemical_absolute_configuration unk _chemical_formula_sum 'C68 H84 N4 O4' _chemical_formula_weight 1021.39 _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_method SHELXL-2016/6 _audit_update_record ; 2020-03-30 deposited with the CCDC. 2020-04-24 downloaded from the CCDC. ; _cell_angle_alpha 103.450(3) _cell_angle_beta 107.340(3) _cell_angle_gamma 103.234(3) _cell_formula_units_Z 2 _cell_length_a 13.5226(5) _cell_length_b 14.1690(5) _cell_length_c 17.1029(5) _cell_measurement_reflns_used 6543 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 26.0350 _cell_measurement_theta_min 2.5440 _cell_volume 2881.0(2) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution SIR97 _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_unetI/netI 0.1028 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 31848 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 24.998 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 2.347 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.76321 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.177 _exptl_crystal_description platelet _exptl_crystal_F_000 1104 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.545 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 701 _refine_ls_number_reflns 10091 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.1427 _refine_ls_R_factor_gt 0.0768 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+2.5830P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1775 _refine_ls_wR_factor_ref 0.2124 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5906 _reflns_number_total 10091 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01909g2.cif _cod_data_source_block 2e _cod_depositor_comments ;Adding full bibliography for 1557900--1557907.cif. Adding full bibliography for 1557900--1557907.cif. ; _cod_original_cell_volume 2880.96(18) _cod_database_code 1557902 _shelx_shelxl_version_number 2016/6 _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_min 0.989 _shelx_estimated_absorpt_t_max 0.999 _shelx_res_file ; TITL okude5 okude5.res created by SHELXL-2016/6 at 18:23:25 on 30-Oct-2018 REM Yadorkari-X generated CELL 0.71073 13.5226 14.1690 17.1029 103.4500 107.3400 103.2340 ZERR 2.0 0.0005 0.0005 0.0005 0.0030 0.0030 0.0030 LATT 1 REM SPGR P-1 triclinic SFAC C H N O UNIT 136 168 8 8 SIZE 0.15 0.05 0.02 TEMP -150.0 L.S. 10 FMAP 2 PLAN -25 ACTA CONF LIST 4 WPDB -1 BOND $H MERG 2 OMIT -10.000000 50.000000 WGHT 0.085600 2.583000 FVAR 0.29962 O1 4 0.334457 0.995763 0.102978 11.00000 0.03289 0.03266 = 0.03430 0.00891 0.00280 0.00771 C1 1 0.345794 1.087987 0.124230 11.00000 0.02287 0.03448 = 0.02621 0.00992 0.01052 0.00719 N1 3 0.424548 1.155805 0.198054 11.00000 0.02198 0.03533 = 0.02287 0.00998 -0.00058 0.00595 C2 1 0.501016 1.119302 0.256457 11.00000 0.02104 0.03950 = 0.03060 0.01282 0.00023 0.00892 AFIX 13 H10 2 0.551828 1.181297 0.306524 11.00000 -1.20000 AFIX 0 C3 1 0.443912 1.046515 0.294357 11.00000 0.03777 0.05555 = 0.03915 0.02577 0.00449 0.01308 AFIX 137 H11 2 0.402018 1.079284 0.323204 11.00000 -1.50000 H12 2 0.498729 1.030111 0.336450 11.00000 -1.50000 H13 2 0.394285 0.983366 0.247777 11.00000 -1.50000 AFIX 0 C4 1 0.571896 1.075480 0.214481 11.00000 0.03651 0.05314 = 0.04612 0.01638 0.00486 0.01986 AFIX 137 H14 2 0.526770 1.010416 0.168456 11.00000 -1.50000 H15 2 0.629481 1.063770 0.258073 11.00000 -1.50000 H16 2 0.605289 1.123907 0.189759 11.00000 -1.50000 AFIX 0 C5 1 0.437957 1.266263 0.224550 11.00000 0.02302 0.03091 = 0.02838 0.00791 0.00357 0.00707 AFIX 13 H17 2 0.385607 1.278538 0.175736 11.00000 -1.20000 AFIX 0 C6 1 0.407596 1.297474 0.302733 11.00000 0.03553 0.04780 = 0.02819 0.00484 0.00676 0.01341 AFIX 137 H18 2 0.331975 1.256820 0.289497 11.00000 -1.50000 H19 2 0.414364 1.370366 0.317593 11.00000 -1.50000 H20 2 0.456776 1.285460 0.351770 11.00000 -1.50000 AFIX 0 C7 1 0.552775 1.331849 0.239623 11.00000 0.02612 0.03971 = 0.03115 0.01019 0.00053 0.00112 AFIX 137 H21 2 0.605190 1.329555 0.292374 11.00000 -1.50000 H22 2 0.554426 1.402810 0.246043 11.00000 -1.50000 H23 2 0.572423 1.305287 0.190130 11.00000 -1.50000 AFIX 0 C8 1 0.271492 1.125190 0.062858 11.00000 0.02205 0.03041 = 0.02020 0.00664 0.00232 0.00291 C9 1 0.310760 1.186508 0.004279 11.00000 0.02055 0.02968 = 0.02377 0.00688 0.00603 0.00532 C10 1 0.234586 1.251790 0.016102 11.00000 0.02028 0.03026 = 0.02369 0.00701 0.00443 0.00716 AFIX 13 H24 2 0.256088 1.327865 0.029722 11.00000 -1.20000 AFIX 0 C11 1 0.196738 1.192640 0.074165 11.00000 0.02201 0.03853 = 0.02191 0.00975 0.00517 0.00864 AFIX 13 H25 2 0.190242 1.225130 0.130148 11.00000 -1.20000 AFIX 0 C12 1 0.100744 1.113507 -0.007734 11.00000 0.01693 0.03628 = 0.02530 0.01049 0.00464 0.00326 AFIX 13 H26 2 0.023371 1.087002 -0.012263 11.00000 -1.20000 AFIX 0 C13 1 0.175479 1.046663 -0.019311 11.00000 0.02212 0.03235 = 0.02359 0.00935 0.00334 0.00297 AFIX 13 H27 2 0.152948 0.970591 -0.032775 11.00000 -1.20000 AFIX 0 C14 1 0.213604 1.104900 -0.077425 11.00000 0.02103 0.03473 = 0.01776 0.00512 0.00303 0.00544 AFIX 13 H28 2 0.219540 1.071860 -0.133513 11.00000 -1.20000 AFIX 0 C15 1 0.139257 1.173195 -0.065986 11.00000 0.02059 0.03087 = 0.02214 0.00877 0.00572 0.00445 C16 1 0.424368 1.222752 0.008460 11.00000 0.02201 0.03155 = 0.01538 0.00706 0.00317 0.00684 C17 1 0.483804 1.155471 0.002658 11.00000 0.02091 0.03091 = 0.03153 0.00906 0.00730 0.00095 AFIX 43 H1 2 0.450692 1.085832 -0.003954 11.00000 -1.20000 AFIX 0 C18 1 0.590166 1.187187 0.006255 11.00000 0.02414 0.03350 = 0.03139 0.01004 0.01017 0.00875 AFIX 43 H2 2 0.629019 1.139342 0.002581 11.00000 -1.20000 AFIX 0 C19 1 0.641403 1.289469 0.015289 11.00000 0.02138 0.03256 = 0.01406 0.00931 0.00102 0.00447 C20 1 0.580822 1.355910 0.019600 11.00000 0.02805 0.02791 = 0.02007 0.00963 0.00558 0.00739 AFIX 43 H3 2 0.612779 1.425151 0.024481 11.00000 -1.20000 AFIX 0 C21 1 0.474742 1.323784 0.016961 11.00000 0.02634 0.03627 = 0.01811 0.01103 0.00433 0.01384 AFIX 43 H4 2 0.435838 1.371546 0.021024 11.00000 -1.20000 AFIX 0 C22 1 0.756447 1.323569 0.020710 11.00000 0.02332 0.03367 = 0.02140 0.01233 0.00596 0.00596 C23 1 0.801662 1.255050 -0.015589 11.00000 0.02984 0.03566 = 0.02838 0.01215 0.01173 0.00864 AFIX 43 H5 2 0.757864 1.185529 -0.045994 11.00000 -1.20000 AFIX 0 C24 1 0.910270 1.286604 -0.008145 11.00000 0.03337 0.04346 = 0.03505 0.01699 0.01865 0.01761 AFIX 43 H6 2 0.940207 1.238451 -0.032870 11.00000 -1.20000 AFIX 0 C25 1 0.974779 1.387584 0.035009 11.00000 0.02491 0.05346 = 0.03710 0.02828 0.01044 0.00950 AFIX 43 H7 2 1.049108 1.408992 0.040445 11.00000 -1.20000 AFIX 0 C26 1 0.930598 1.456809 0.070003 11.00000 0.02763 0.04280 = 0.03031 0.01748 0.00690 0.00140 AFIX 43 H8 2 0.974384 1.526577 0.098951 11.00000 -1.20000 AFIX 0 C27 1 0.822813 1.425839 0.063477 11.00000 0.03139 0.03432 = 0.02601 0.01261 0.01130 0.01139 AFIX 43 H9 2 0.793536 1.474554 0.088308 11.00000 -1.20000 AFIX 0 C28 1 0.071310 1.209063 -0.132934 11.00000 0.01879 0.03669 = 0.02221 0.00976 0.00863 0.00596 O2 4 0.090285 1.300932 -0.120861 11.00000 0.02361 0.03710 = 0.02786 0.01101 0.00458 0.00712 N2 3 -0.007864 1.136720 -0.205073 11.00000 0.02086 0.03444 = 0.02092 0.00860 0.00066 0.00601 C29 1 -0.029687 1.025861 -0.220307 11.00000 0.02561 0.03531 = 0.03049 0.00771 -0.00228 0.00505 AFIX 13 H29 2 0.022749 1.018176 -0.168728 11.00000 -1.20000 AFIX 0 C30 1 -0.005944 0.975653 -0.298609 11.00000 0.05380 0.04367 = 0.03458 0.00310 -0.00216 0.01610 AFIX 137 H30 2 -0.054515 0.983164 -0.350564 11.00000 -1.50000 H31 2 -0.018403 0.902704 -0.305843 11.00000 -1.50000 H32 2 0.070360 1.008788 -0.289797 11.00000 -1.50000 AFIX 0 C31 1 -0.144433 0.973354 -0.225824 11.00000 0.03431 0.05056 = 0.06101 0.02302 -0.00106 -0.00417 AFIX 137 H33 2 -0.157822 1.012112 -0.176754 11.00000 -1.50000 H34 2 -0.150987 0.903575 -0.224186 11.00000 -1.50000 H35 2 -0.198294 0.970603 -0.280082 11.00000 -1.50000 AFIX 0 C32 1 -0.077514 1.168032 -0.273134 11.00000 0.02848 0.03948 = 0.02223 0.01129 0.00140 0.01016 AFIX 13 H36 2 -0.128836 1.103478 -0.320195 11.00000 -1.20000 AFIX 0 C33 1 -0.147673 1.224043 -0.240466 11.00000 0.02824 0.05712 = 0.03448 0.01877 0.00391 0.01971 AFIX 137 H37 2 -0.193724 1.180189 -0.219571 11.00000 -1.50000 H38 2 -0.194187 1.240865 -0.287701 11.00000 -1.50000 H39 2 -0.100479 1.287297 -0.193001 11.00000 -1.50000 AFIX 0 C34 1 -0.010007 1.227492 -0.313546 11.00000 0.03770 0.05437 = 0.03034 0.01978 0.01026 0.01498 AFIX 137 H40 2 0.036727 1.294542 -0.271042 11.00000 -1.50000 H41 2 -0.059021 1.237026 -0.364165 11.00000 -1.50000 H42 2 0.035748 1.189199 -0.331458 11.00000 -1.50000 AFIX 0 O3 4 0.501682 0.405616 0.643484 11.00000 0.03765 0.05231 = 0.03461 0.01922 0.01487 0.01702 C35 1 0.419029 0.371114 0.657481 11.00000 0.03832 0.03412 = 0.02445 0.01214 0.00860 0.01575 N3 3 0.422441 0.339577 0.726970 11.00000 0.03000 0.03905 = 0.02123 0.01157 0.00541 0.01161 C36 1 0.528910 0.352068 0.792581 11.00000 0.03663 0.04951 = 0.02326 0.01533 0.00278 0.01957 AFIX 13 H52 2 0.511983 0.330865 0.840219 11.00000 -1.20000 AFIX 0 C37 1 0.585605 0.281233 0.758859 11.00000 0.06972 0.08702 = 0.04267 0.02396 0.01287 0.05504 AFIX 137 H53 2 0.534714 0.210974 0.732646 11.00000 -1.50000 H54 2 0.649147 0.284108 0.806783 11.00000 -1.50000 H55 2 0.609797 0.302586 0.715235 11.00000 -1.50000 AFIX 0 C38 1 0.602911 0.462539 0.833488 11.00000 0.03339 0.06092 = 0.03315 0.01345 0.00354 0.01062 AFIX 137 H56 2 0.630699 0.484122 0.791513 11.00000 -1.50000 H57 2 0.664455 0.468643 0.884501 11.00000 -1.50000 H58 2 0.561431 0.506284 0.850901 11.00000 -1.50000 AFIX 0 C39 1 0.323475 0.298966 0.744408 11.00000 0.03481 0.05048 = 0.02338 0.01817 0.00142 0.00453 AFIX 13 H59 2 0.259265 0.286817 0.691169 11.00000 -1.20000 AFIX 0 C40 1 0.315613 0.377349 0.817124 11.00000 0.03991 0.07263 = 0.03042 0.01801 0.01322 0.01278 AFIX 137 H60 2 0.378137 0.392581 0.870543 11.00000 -1.50000 H61 2 0.247535 0.350065 0.825588 11.00000 -1.50000 H62 2 0.316067 0.440253 0.802418 11.00000 -1.50000 AFIX 0 C41 1 0.315219 0.196407 0.759152 11.00000 0.06062 0.05438 = 0.03779 0.02325 -0.00411 -0.00662 AFIX 137 H63 2 0.327144 0.150545 0.712837 11.00000 -1.50000 H64 2 0.242361 0.165995 0.759036 11.00000 -1.50000 H65 2 0.370817 0.206419 0.815110 11.00000 -1.50000 AFIX 0 C42 1 0.309290 0.360024 0.592972 11.00000 0.03458 0.03394 = 0.02757 0.01273 0.00701 0.01137 C43 1 0.225939 0.252417 0.522460 11.00000 0.03657 0.03225 = 0.03452 0.01798 0.01126 0.01214 C44 1 0.223643 0.302700 0.450070 11.00000 0.03292 0.04006 = 0.02682 0.01552 0.01132 0.01294 AFIX 13 H66 2 0.230075 0.270660 0.393951 11.00000 -1.20000 AFIX 0 C45 1 0.302833 0.407191 0.518851 11.00000 0.03611 0.03699 = 0.03289 0.01782 0.00377 0.00313 AFIX 13 H67 2 0.366874 0.452459 0.512916 11.00000 -1.20000 AFIX 0 C46 1 0.202922 0.438379 0.528848 11.00000 0.05088 0.03246 = 0.03306 0.01027 -0.00099 0.01831 AFIX 13 H68 2 0.193841 0.506914 0.531018 11.00000 -1.20000 AFIX 0 C47 1 0.207400 0.390441 0.601470 11.00000 0.05443 0.05415 = 0.02643 0.01039 0.01286 0.03235 AFIX 13 H69 2 0.200782 0.422962 0.657393 11.00000 -1.20000 AFIX 0 C48 1 0.127506 0.285593 0.532580 11.00000 0.03265 0.05473 = 0.03118 0.02451 0.01364 0.01408 AFIX 13 H70 2 0.062495 0.241244 0.538056 11.00000 -1.20000 AFIX 0 C49 1 0.123306 0.334233 0.459136 11.00000 0.03217 0.03970 = 0.02774 0.01519 0.00814 0.01392 C50 1 0.242132 0.150996 0.517311 11.00000 0.03381 0.03616 = 0.02656 0.01252 0.00576 0.00696 C51 1 0.330831 0.130873 0.498932 11.00000 0.03632 0.04370 = 0.04448 0.02015 0.01773 0.01182 AFIX 43 H43 2 0.380880 0.182524 0.490074 11.00000 -1.20000 AFIX 0 C52 1 0.346528 0.037896 0.493532 11.00000 0.02927 0.03535 = 0.04502 0.02244 0.01009 0.00336 AFIX 43 H44 2 0.406634 0.025914 0.479835 11.00000 -1.20000 AFIX 0 C53 1 0.276372 -0.039986 0.507654 11.00000 0.02810 0.03859 = 0.02918 0.01047 0.00008 0.00588 C54 1 0.188931 -0.019178 0.525302 11.00000 0.03955 0.03757 = 0.03467 0.01619 0.01469 0.01215 AFIX 43 H45 2 0.139192 -0.070773 0.534473 11.00000 -1.20000 AFIX 0 C55 1 0.171009 0.073914 0.530135 11.00000 0.03368 0.04358 = 0.03217 0.01367 0.01394 0.01229 AFIX 43 H46 2 0.109723 0.085081 0.542289 11.00000 -1.20000 AFIX 0 C56 1 0.295679 -0.139800 0.503372 11.00000 0.02485 0.03050 = 0.01991 0.00760 0.00186 0.00442 C57 1 0.357244 -0.174871 0.458382 11.00000 0.03427 0.04670 = 0.03349 0.01144 0.00723 0.00704 AFIX 43 H47 2 0.385457 -0.135910 0.426975 11.00000 -1.20000 AFIX 0 C58 1 0.378139 -0.266754 0.458794 11.00000 0.03953 0.03921 = 0.03756 0.00574 0.00076 0.01471 AFIX 43 H48 2 0.421421 -0.289082 0.428400 11.00000 -1.20000 AFIX 0 C59 1 0.337795 -0.324133 0.501668 11.00000 0.03677 0.04144 = 0.03278 0.00849 0.00022 0.01104 AFIX 43 H49 2 0.352366 -0.386629 0.501600 11.00000 -1.20000 AFIX 0 C60 1 0.273964 -0.290763 0.546501 11.00000 0.05704 0.03193 = 0.03366 0.01077 0.01125 0.00568 AFIX 43 H50 2 0.244497 -0.330814 0.576679 11.00000 -1.20000 AFIX 0 C61 1 0.254339 -0.199765 0.546484 11.00000 0.03519 0.03488 = 0.03280 0.01089 0.00318 0.00445 AFIX 43 H51 2 0.211109 -0.177638 0.577020 11.00000 -1.20000 AFIX 0 C62 1 0.017826 0.309222 0.384852 11.00000 0.02923 0.05048 = 0.02809 0.01877 0.01101 0.01501 O4 4 -0.064562 0.244561 0.380086 11.00000 0.03760 0.08666 = 0.04576 0.03788 0.01153 0.00760 N4 3 0.018986 0.351044 0.321296 11.00000 0.02629 0.04412 = 0.02514 0.01675 0.00614 0.01355 C63 1 0.114119 0.428988 0.326287 11.00000 0.02739 0.06392 = 0.04613 0.03712 -0.00217 -0.00007 AFIX 13 H71 2 0.173168 0.443418 0.383359 11.00000 -1.20000 AFIX 0 C64 1 0.156772 0.391266 0.257352 11.00000 0.04115 0.17424 = 0.06405 0.07706 0.02583 0.04016 AFIX 137 H72 2 0.164385 0.324024 0.256907 11.00000 -1.50000 H73 2 0.228246 0.439832 0.269466 11.00000 -1.50000 H74 2 0.105479 0.385360 0.200764 11.00000 -1.50000 AFIX 0 C65 1 0.088636 0.528377 0.326591 11.00000 0.08649 0.05340 = 0.07003 0.03699 -0.02215 -0.00275 AFIX 137 H75 2 0.031262 0.517516 0.271289 11.00000 -1.50000 H76 2 0.154788 0.581877 0.334735 11.00000 -1.50000 H77 2 0.063466 0.549660 0.373945 11.00000 -1.50000 AFIX 0 C66 1 -0.081095 0.318090 0.241945 11.00000 0.02775 0.05959 = 0.02766 0.02047 0.00795 0.01846 AFIX 13 H78 2 -0.062030 0.355989 0.203130 11.00000 -1.20000 AFIX 0 C67 1 -0.114228 0.203626 0.192470 11.00000 0.06580 0.05349 = 0.03955 0.01499 -0.00466 0.00819 AFIX 137 H79 2 -0.052196 0.188527 0.180148 11.00000 -1.50000 H80 2 -0.175973 0.185778 0.137937 11.00000 -1.50000 H81 2 -0.135696 0.163399 0.227698 11.00000 -1.50000 AFIX 0 C68 1 -0.174456 0.345586 0.259304 11.00000 0.04732 0.12628 = 0.04283 0.03784 0.01541 0.04761 AFIX 137 H82 2 -0.198842 0.306649 0.294339 11.00000 -1.50000 H83 2 -0.234969 0.329059 0.204297 11.00000 -1.50000 H84 2 -0.150847 0.419100 0.290673 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM okude5 REM R1 = 0.0768 for 5906 Fo > 4sig(Fo) and 0.1427 for all 10091 data REM 701 parameters refined using 0 restraints END WGHT 0.0855 2.5716 REM Highest difference peak 0.545, deepest hole -0.287, 1-sigma level 0.059 Q1 1 -0.0570 0.3272 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5.67560 -17 4 -1 13.1205 6.39127 -17 4 -1 10.9390 5.98602 17 -4 1 16.5963 6.33558 -17 4 -2-5.34743 6.23123 -17 4 -2-4.56547 6.06787 17 -4 2-1.52144 5.96453 -17 4 -3 7.89265 6.54661 -17 4 -3 9.48924 6.24751 -17 4 -4 5.76174 6.46607 -17 3 13-3.09809 6.29421 -17 3 12-6.13948 6.60610 17 -3 -12 3.36519 6.29718 -17 3 11 1.32742 6.31005 17 -3 -11-7.00734 6.03169 -17 3 10 3.03648 6.25244 17 -3 -10 0.40453 5.77525 -17 3 9 0.42415 6.23642 17 -3 -9 1.19235 5.73604 -17 3 8-0.83345 5.98950 17 -3 -8 0.39239 5.63972 17 -3 -7 7.77857 5.78394 -17 3 7 10.6435 6.04595 -17 3 6 9.65005 5.96473 17 -3 -6 3.88868 5.71015 -17 3 5 13.9102 5.98111 17 -3 -5-1.54996 5.90415 -17 3 5 4.10915 5.13729 -17 3 4-1.97573 5.82043 17 -3 -4-3.49169 5.31426 -17 3 4-3.57054 5.20522 -17 3 3 9.03403 6.12544 17 -3 -3 2.70144 5.73250 -17 3 3 2.01395 5.15088 -17 3 2-2.37350 6.14115 17 -3 -2-2.68502 5.58039 -17 3 2 4.48607 5.22377 -17 3 1 11.9404 6.32205 17 -3 -1 12.9837 5.96604 -17 3 1 7.50031 5.57847 -17 3 0 5.62434 6.26773 -17 3 0 2.58199 5.55945 17 -3 0 8.18608 6.13837 -17 3 -1-5.98117 6.57060 -17 3 -1-4.59504 5.90331 17 -3 1 6.30053 6.23434 17 -3 2-0.39964 6.19845 -17 3 -2-3.97521 6.02664 -17 3 -3 7.42779 6.22537 -17 2 14 2.61038 6.40705 -17 2 13-4.29063 6.43632 -17 2 12 10.6233 6.30702 -17 2 11-15.3958 6.49927 17 -2 -11-5.85482 6.08730 -17 2 10 5.10758 6.00531 17 -2 -10 8.23875 6.38618 -17 2 9-0.83146 6.18702 17 -2 -9 6.91835 5.89241 17 -2 -8 6.45717 6.19452 -17 2 8 4.89972 5.90378 -17 2 8-0.91125 4.87164 -17 2 7 8.01365 5.79675 17 -2 -7 6.42301 5.90858 -17 2 7-0.31226 4.87800 -17 2 6 14.5510 6.12551 17 -2 -6 6.42913 5.76546 -17 2 6-0.64707 4.97962 -17 2 5-3.48816 6.03543 17 -2 -5 12.0079 5.98858 -17 2 5 2.67925 5.37796 -17 2 4 4.62843 5.78182 17 -2 -4-0.79598 5.49807 -17 2 4 1.38274 5.27248 -17 2 3 1.91589 5.84696 17 -2 -3 7.11315 5.83621 -17 2 3 7.79347 5.48525 -17 2 2 6.58526 5.23042 17 -2 -2 0.78673 5.67779 -17 2 1-1.54970 6.27845 -17 2 1 8.25590 5.80060 17 -2 -1 0.40141 5.98050 -17 2 0-1.17656 6.26960 -17 2 0 12.3832 5.95671 17 -2 0 0.40585 6.08086 -17 2 -1 5.20116 6.06541 17 -2 1 5.36469 6.41486 17 -2 2 6.26947 6.65267 -17 2 -2 3.31305 5.96747 17 -2 3 6.80213 7.02493 -17 1 14 12.8182 6.27561 17 -1 -13 1.32270 6.28623 -17 1 13 2.92311 5.96226 -17 1 12 7.83725 6.12371 -17 1 11 0.82865 6.01177 -17 1 11-1.58443 5.08940 17 -1 -10 2.11260 6.01445 -17 1 10 2.51002 6.12660 -17 1 10-2.85722 5.00867 -17 1 9-0.81815 6.09348 17 -1 -9 5.03453 6.09646 -17 1 9 0.95401 4.88566 -17 1 8 1.60194 5.89029 17 -1 -8-3.74681 6.02630 -17 1 8-4.85030 4.91539 -17 1 7 0.39312 5.77278 17 -1 -7-0.41720 6.09427 -17 1 7 2.97418 5.02754 -17 1 6 5.77768 5.78318 17 -1 -6 7.84686 6.23035 -17 1 6 3.09839 5.50938 -17 1 5 6.44428 5.69270 17 -1 -5 6.55743 5.98221 -17 1 5-2.12254 5.45084 -17 1 4-4.52231 5.60613 17 -1 -4 5.70262 5.98156 -17 1 4 2.55852 5.47180 -17 1 3 3.73850 5.81050 -17 1 3 7.85497 5.51377 17 -1 -3 7.29549 5.91768 -17 1 2 6.42573 6.15259 -17 1 2 1.54131 5.55646 17 -1 -2 1.23969 6.12585 -17 1 1-0.78927 5.92228 17 -1 -1-0.41811 6.33723 -17 1 0 0.81168 6.06976 17 -1 0-6.35458 6.62491 17 -1 1 1.29270 6.72306 -17 1 -1 4.17850 6.18610 -17 0 14 5.46242 6.08170 -17 0 13 1.63206 5.11075 17 0 -13-1.34874 6.42794 -17 0 13 6.18030 5.93172 -17 0 12 1.34419 5.18982 -17 0 12-12.1105 6.28225 -17 0 11 3.67466 5.88661 -17 0 11 1.69666 5.41041 -17 0 10 6.17697 6.05325 17 0 -10 13.4958 6.44602 -17 0 10 9.49932 5.46445 -17 0 9 1.61236 5.89026 17 0 -9-4.75423 6.15467 -17 0 9-4.75313 5.42551 -17 0 8-4.32610 5.86526 17 0 -8-9.48813 6.50352 -17 0 8-1.72318 5.20665 -17 0 7 3.08461 5.81699 17 0 -7 4.69001 6.03700 -17 0 7-0.35168 5.31256 -17 0 6 33.2035 6.84585 17 0 -6 32.5797 6.71588 -17 0 6 29.0213 6.47926 -17 0 5-3.33769 5.79209 17 0 -5-2.09663 5.86955 -17 0 5-0.37358 5.64946 -17 0 4 3.68158 5.85426 -17 0 4 1.54263 5.49731 17 0 -4-5.01212 6.31490 -17 0 3-5.83126 6.01313 -17 0 3-1.57964 5.84485 17 0 -3-7.66487 6.51675 -17 0 2 8.10085 5.99902 17 0 -2 15.4936 6.76690 -17 0 1 4.57296 6.18151 17 0 -1 3.92435 6.57345 -17 0 0 2.12554 6.48392 -17 -1 15-1.38189 5.28802 -17 -1 14-3.79172 5.48362 -17 -1 14-1.24057 6.06616 -17 -1 13 0.34820 5.43761 -17 -1 13-2.84278 6.29024 17 1 -12 7.31514 6.48491 -17 -1 12 10.6489 5.79203 -17 -1 12 12.3555 6.32750 -17 -1 11 2.38440 5.85306 -17 -1 11 8.32168 5.50806 -17 -1 10-5.19657 6.13352 -17 -1 10-5.06459 5.55909 -17 -1 9 3.17456 6.16137 17 1 -9 0.89105 6.26290 -17 -1 9 1.44645 5.20566 -17 -1 8 19.7272 6.41191 17 1 -8 18.9588 6.86840 -17 -1 8 18.6881 6.03616 -17 -1 7 10.5983 6.02441 17 1 -7 6.55139 6.15942 -17 -1 7 1.86585 5.45700 -17 -1 6 8.50509 5.94653 -17 -1 6 5.77210 5.62699 17 1 -6 13.4240 6.39200 -17 -1 5 7.26977 5.97060 -17 -1 5 8.70379 5.86238 -17 -1 4 3.67016 6.00152 17 1 -4 4.82600 6.23330 -17 -1 3 4.16445 6.15328 17 1 -3 4.87408 6.15364 -17 -1 2-1.70120 6.49421 -17 -2 16 4.78466 5.69474 -17 -2 15 1.83495 5.71841 -17 -2 14 7.34375 5.52134 -17 -2 14-0.81930 5.94772 -17 -2 13-1.85302 5.69955 -17 -2 13 4.00863 6.06847 -17 -2 12 4.57688 5.64438 -17 -2 12 4.71506 6.00600 -17 -2 11 4.71482 6.00160 17 2 -11 16.7854 6.99191 -17 -2 11 6.16115 5.80422 -17 -2 10 0.39437 5.95616 -17 -2 10-3.84970 5.83581 -17 -2 9 9.77633 6.09536 -17 -2 9 2.30713 5.56055 -17 -2 8-10.2699 6.20590 17 2 -8-0.90125 6.40963 -17 -2 8-0.38931 5.79534 -17 -2 7 14.8581 6.24360 -17 -2 7 11.4828 6.00266 17 2 -7 19.6547 6.62745 -17 -2 6 2.03902 5.91299 17 2 -6 4.92889 6.33732 -17 -2 5 7.95505 6.27121 -17 -2 4 5.58064 6.42725 -17 -3 14-2.33666 5.80199 -17 -3 13 7.15111 5.99260 -17 -3 13 6.75726 6.09154 -17 -3 12 8.09864 6.39797 -17 -3 12 16.3465 6.45812 -17 -3 11-2.71904 5.98139 -17 -3 11 16.3519 6.32329 -17 -3 10 14.4018 6.52584 -17 -3 10 6.94502 6.15030 -17 -3 9 6.16052 6.09208 -17 -3 9 8.57167 6.21122 -17 -3 8 7.84410 6.29935 -17 -3 7 13.4273 6.25780 -17 -3 6 2.15867 6.34909 -17 -4 13 15.3796 6.62797 -17 -4 12 11.5653 6.34014 -17 -4 11 4.99098 6.08558 18 -11 -5 2.88033 5.86060 18 -10 -6-2.22283 5.86634 18 -10 -5-1.08526 5.91737 18 -10 -4 3.89681 5.76883 18 -9 -7 4.57186 6.00390 18 -9 -6 5.58444 5.87065 18 -9 -5-2.18562 5.72251 18 -9 -4 0.35770 5.64337 18 -9 -3 6.35587 5.69721 18 -8 -8 4.69752 6.20388 18 -8 -7 11.8656 6.14483 18 -8 -6 1.49983 5.76006 18 -8 -5-3.31736 5.81893 18 -8 -4 4.72134 5.78262 18 -8 -3-4.68696 5.83557 18 -8 -2 12.2675 6.17517 18 -7 -9 5.63223 5.99435 18 -7 -8-2.36315 6.02239 18 -7 -7 9.64674 6.04839 -18 7 6 4.74911 6.80334 18 -7 -6 4.17519 5.73822 -18 7 5 1.88281 6.51077 18 -7 -5 8.60426 5.86548 18 -7 -4-1.85883 5.74157 -18 7 4-10.3870 6.93252 18 -7 -3 1.48563 5.76325 -18 7 3 10.9096 6.75183 18 -7 -2-0.37119 6.02646 18 -7 -1-2.57709 5.90845 18 -6 -9 8.51887 6.16376 -18 6 8-5.17219 6.72348 18 -6 -8 9.15581 5.95413 -18 6 7-5.11543 6.58454 18 -6 -7-0.39071 5.84324 -18 6 6-4.61854 6.77600 18 -6 -6-2.31187 6.13061 18 -6 -5 4.98013 5.78235 -18 6 5 2.28966 6.34796 18 -6 -4-4.59381 6.02846 -18 6 4-6.39470 6.79381 -18 6 3 5.07204 6.38749 18 -6 -3-3.83194 6.00433 -18 6 2 2.30021 6.69052 18 -6 -2 6.85547 5.99563 -18 6 1-3.69766 6.95189 18 -6 -1-10.5662 6.33116 18 -5 -10-6.68471 6.43846 -18 5 9 5.60782 6.61272 18 -5 -9 9.02255 6.25613 -18 5 8 15.1508 6.82558 18 -5 -8 15.2970 6.18965 -18 5 7 9.50850 6.41788 18 -5 -7 1.59350 6.00998 18 -5 -6 11.0526 5.77527 -18 5 6-1.79715 6.62270 -18 5 5 8.03129 6.43148 18 -5 -5-3.54976 5.91271 -18 5 4 0.88683 6.33750 18 -5 -4 9.03726 6.08688 -18 5 3 0.89218 6.56950 18 -5 -3-5.89670 6.15498 -18 5 2 13.4296 6.84165 18 -5 -2 1.95002 6.19079 -18 5 1 6.29687 6.81882 18 -5 -1-0.77147 6.23088 -18 5 0 3.15885 6.45860 18 -5 0 11.4753 6.11418 -18 4 10 6.98091 6.66527 18 -4 -10 6.35382 6.16006 -18 4 9 15.0901 6.93910 18 -4 -9 4.99301 5.83648 -18 4 8-3.14748 6.38434 18 -4 -8 6.98114 6.11789 18 -4 -7-4.08984 6.12432 -18 4 7 10.1698 6.38323 -18 4 6 5.25177 6.35942 18 -4 -6-1.62693 6.15031 -18 4 5-2.61169 6.33855 18 -4 -5-6.10443 6.34588 -18 4 4 6.48336 6.46717 18 -4 -4 6.88683 6.13910 -18 4 3-1.30411 6.40233 18 -4 -3-4.42487 6.09212 -18 4 2 7.41600 6.59769 18 -4 -2-1.19651 5.93492 -18 4 1 10.9565 7.02519 18 -4 -1 8.31443 6.30976 -18 4 0 8.35138 6.79377 18 -4 0 13.2974 6.68799 -18 4 -1 1.74126 6.74302 -18 3 10-5.01475 6.22211 18 -3 -10 2.58363 6.19778 -18 3 9-1.34491 6.34756 18 -3 -9 5.95715 6.30677 18 -3 -8 0.42182 6.03250 -18 3 8-7.04078 6.36206 -18 3 7 11.6788 6.36080 18 -3 -7-7.12819 6.32504 -18 3 6-7.70120 6.35079 18 -3 -6 1.25890 6.11629 -18 3 5 16.1383 6.63550 18 -3 -5 0.41750 6.47839 -18 3 4-1.68469 6.45471 18 -3 -4 4.97407 5.90970 -18 3 3 5.93854 6.51814 18 -3 -3 0.41104 6.09347 -18 3 2 2.55224 6.39762 18 -3 -2 10.6148 6.35965 -18 3 1-0.42704 6.67364 18 -3 -1 8.71997 6.48197 -18 3 0 17.8933 6.94100 18 -3 0 6.27735 6.48519 -18 2 11-1.83014 6.41331 -18 2 10 7.60803 6.50212 -18 2 9 7.91805 6.43389 18 -2 -9-8.76324 6.67365 -18 2 8 2.15920 6.49758 18 -2 -8 1.30274 6.00763 -18 2 7 5.08474 6.32955 18 -2 -7 10.3902 6.49875 -18 2 6-0.41776 6.31957 18 -2 -6 6.88405 6.26293 -18 2 5 6.64468 6.22820 18 -2 -5 0.42715 6.17659 -18 2 4 7.40570 6.39183 18 -2 -4 4.23321 6.27731 -18 2 4 0.37065 5.93174 -18 2 3 2.89765 6.16870 -18 2 3 9.15822 5.93461 18 -2 -3-2.10207 6.22498 -18 2 2 0.41479 6.65465 -18 2 2 1.17142 6.23699 -18 2 1 4.42356 6.19775 -18 1 11 2.25127 6.76674 -18 1 10 3.07905 6.41923 -18 1 9-3.88821 6.45522 -18 1 8 0.84868 6.32007 -18 1 8-2.10996 5.60457 -18 1 7 13.3041 6.50308 -18 1 7 5.80674 5.72943 -18 1 6 9.40980 6.31630 -18 1 6 5.58265 5.81677 -18 1 5 17.8713 6.74217 -18 1 5 8.82063 5.99586 -18 1 4-0.80393 6.45939 -18 1 4 7.43929 6.05382 -18 1 3-9.69547 6.60999 -18 1 3 3.21873 5.95662 -18 1 2 13.1851 6.42694 -18 0 11-3.99352 6.66350 -18 0 10-1.30150 6.46128 -18 0 10 1.43858 5.34953 -18 0 9 20.3927 6.80659 -18 0 9 22.5854 6.31930 -18 0 8 5.41870 6.49401 -18 0 8-2.22700 5.56349 -18 0 7 13.4608 6.61280 -18 0 7 11.9361 6.13947 -18 0 6 7.21652 6.34899 -18 0 6 7.49184 6.05218 -18 0 5 8.74092 6.66797 -18 0 5 31.1547 6.87391 -18 0 4-3.72061 6.46687 -18 -1 13 15.2865 6.50947 -18 -1 12 2.29354 6.07334 -18 -1 11 9.62488 6.58528 -18 -1 11 3.42564 6.03822 -18 -1 10 8.97924 6.71048 -18 -1 10-1.91047 6.01781 -18 -1 9 15.0447 6.62697 -18 -1 9 4.64499 5.88192 -18 -1 8-4.09448 6.36013 -18 -1 8 10.2402 6.00990 -18 -1 7 9.20160 6.52837 -18 -1 7 13.7671 6.52899 -18 -1 6 4.98713 6.08634 -18 -2 10 8.00846 6.69863 -18 -2 9 18.5157 6.72982 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 97675 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 0.3345(2) 0.9958(2) 0.10298(17) 0.0365(7) Uani 1 1 d . . . . . C1 C 0.3458(3) 1.0880(3) 0.1242(2) 0.0279(9) Uani 1 1 d . . . . . N1 N 0.4245(2) 1.1558(2) 0.19805(19) 0.0294(7) Uani 1 1 d . . . . . C2 C 0.5010(3) 1.1193(3) 0.2565(2) 0.0325(9) Uani 1 1 d . . . . . H10 H 0.551828 1.181297 0.306524 0.039 Uiso 1 1 calc R U . . . C3 C 0.4439(3) 1.0465(3) 0.2944(3) 0.0449(11) Uani 1 1 d . . . . . H11 H 0.402018 1.079284 0.323204 0.067 Uiso 1 1 calc R U . . . H12 H 0.498729 1.030111 0.336450 0.067 Uiso 1 1 calc R U . . . H13 H 0.394285 0.983366 0.247777 0.067 Uiso 1 1 calc R U . . . C4 C 0.5719(3) 1.0755(3) 0.2145(3) 0.0467(11) Uani 1 1 d . . . . . H14 H 0.526770 1.010416 0.168456 0.070 Uiso 1 1 calc R U . . . H15 H 0.629481 1.063770 0.258073 0.070 Uiso 1 1 calc R U . . . H16 H 0.605289 1.123907 0.189759 0.070 Uiso 1 1 calc R U . . . C5 C 0.4380(3) 1.2663(3) 0.2245(2) 0.0295(9) Uani 1 1 d . . . . . H17 H 0.385607 1.278538 0.175736 0.035 Uiso 1 1 calc R U . . . C6 C 0.4076(3) 1.2975(3) 0.3027(2) 0.0398(10) Uani 1 1 d . . . . . H18 H 0.331975 1.256820 0.289497 0.060 Uiso 1 1 calc R U . . . H19 H 0.414364 1.370366 0.317593 0.060 Uiso 1 1 calc R U . . . H20 H 0.456776 1.285460 0.351770 0.060 Uiso 1 1 calc R U . . . C7 C 0.5528(3) 1.3318(3) 0.2396(3) 0.0368(10) Uani 1 1 d . . . . . H21 H 0.605190 1.329555 0.292374 0.055 Uiso 1 1 calc R U . . . H22 H 0.554426 1.402810 0.246043 0.055 Uiso 1 1 calc R U . . . H23 H 0.572423 1.305287 0.190130 0.055 Uiso 1 1 calc R U . . . C8 C 0.2715(3) 1.1252(3) 0.0629(2) 0.0269(9) Uani 1 1 d . . . . . C9 C 0.3108(3) 1.1865(3) 0.0043(2) 0.0260(8) Uani 1 1 d . . . . . C10 C 0.2346(3) 1.2518(3) 0.0161(2) 0.0261(8) Uani 1 1 d . . . . . H24 H 0.256088 1.327865 0.029722 0.031 Uiso 1 1 calc R U . . . C11 C 0.1967(3) 1.1926(3) 0.0742(2) 0.0284(9) Uani 1 1 d . . . . . H25 H 0.190242 1.225130 0.130148 0.034 Uiso 1 1 calc R U . . . C12 C 0.1007(3) 1.1135(3) -0.0077(2) 0.0278(9) Uani 1 1 d . . . . . H26 H 0.023371 1.087002 -0.012263 0.033 Uiso 1 1 calc R U . . . C13 C 0.1755(3) 1.0467(3) -0.0193(2) 0.0283(9) Uani 1 1 d . . . . . H27 H 0.152948 0.970591 -0.032775 0.034 Uiso 1 1 calc R U . . . C14 C 0.2136(3) 1.1049(3) -0.0774(2) 0.0268(9) Uani 1 1 d . . . . . H28 H 0.219540 1.071860 -0.133513 0.032 Uiso 1 1 calc R U . . . C15 C 0.1393(3) 1.1732(3) -0.0660(2) 0.0257(8) Uani 1 1 d . . . . . C16 C 0.4244(3) 1.2228(3) 0.0085(2) 0.0243(8) Uani 1 1 d . . . . . C17 C 0.4838(3) 1.1555(3) 0.0027(2) 0.0299(9) Uani 1 1 d . . . . . H1 H 0.450692 1.085832 -0.003954 0.036 Uiso 1 1 calc R U . . . C18 C 0.5902(3) 1.1872(3) 0.0063(2) 0.0299(9) Uani 1 1 d . . . . . H2 H 0.629019 1.139342 0.002581 0.036 Uiso 1 1 calc R U . . . C19 C 0.6414(3) 1.2895(3) 0.0153(2) 0.0245(8) Uani 1 1 d . . . . . C20 C 0.5808(3) 1.3559(3) 0.0196(2) 0.0261(9) Uani 1 1 d . . . . . H3 H 0.612779 1.425151 0.024481 0.031 Uiso 1 1 calc R U . . . C21 C 0.4747(3) 1.3238(3) 0.0170(2) 0.0268(9) Uani 1 1 d . . . . . H4 H 0.435838 1.371546 0.021024 0.032 Uiso 1 1 calc R U . . . C22 C 0.7564(3) 1.3236(3) 0.0207(2) 0.0266(9) Uani 1 1 d . . . . . C23 C 0.8017(3) 1.2550(3) -0.0156(2) 0.0311(9) Uani 1 1 d . . . . . H5 H 0.757864 1.185529 -0.045994 0.037 Uiso 1 1 calc R U . . . C24 C 0.9103(3) 1.2866(3) -0.0081(2) 0.0341(10) Uani 1 1 d . . . . . H6 H 0.940207 1.238451 -0.032870 0.041 Uiso 1 1 calc R U . . . C25 C 0.9748(3) 1.3876(3) 0.0350(3) 0.0368(10) Uani 1 1 d . . . . . H7 H 1.049108 1.408992 0.040445 0.044 Uiso 1 1 calc R U . . . C26 C 0.9306(3) 1.4568(3) 0.0700(2) 0.0353(10) Uani 1 1 d . . . . . H8 H 0.974384 1.526577 0.098951 0.042 Uiso 1 1 calc R U . . . C27 C 0.8228(3) 1.4258(3) 0.0635(2) 0.0297(9) Uani 1 1 d . . . . . H9 H 0.793536 1.474554 0.088308 0.036 Uiso 1 1 calc R U . . . C28 C 0.0713(3) 1.2091(3) -0.1329(2) 0.0261(9) Uani 1 1 d . . . . . O2 O 0.09029(19) 1.3009(2) -0.12086(16) 0.0311(6) Uani 1 1 d . . . . . N2 N -0.0079(2) 1.1367(2) -0.20507(18) 0.0277(7) Uani 1 1 d . . . . . C29 C -0.0297(3) 1.0259(3) -0.2203(2) 0.0350(10) Uani 1 1 d . . . . . H29 H 0.022749 1.018176 -0.168728 0.042 Uiso 1 1 calc R U . . . C30 C -0.0059(4) 0.9757(3) -0.2986(3) 0.0502(12) Uani 1 1 d . . . . . H30 H -0.054515 0.983164 -0.350564 0.075 Uiso 1 1 calc R U . . . H31 H -0.018403 0.902704 -0.305843 0.075 Uiso 1 1 calc R U . . . H32 H 0.070360 1.008788 -0.289797 0.075 Uiso 1 1 calc R U . . . C31 C -0.1444(3) 0.9734(4) -0.2258(3) 0.0555(13) Uani 1 1 d . . . . . H33 H -0.157822 1.012112 -0.176754 0.083 Uiso 1 1 calc R U . . . H34 H -0.150987 0.903575 -0.224186 0.083 Uiso 1 1 calc R U . . . H35 H -0.198294 0.970603 -0.280082 0.083 Uiso 1 1 calc R U . . . C32 C -0.0775(3) 1.1680(3) -0.2731(2) 0.0319(9) Uani 1 1 d . . . . . H36 H -0.128836 1.103478 -0.320195 0.038 Uiso 1 1 calc R U . . . C33 C -0.1477(3) 1.2240(3) -0.2405(3) 0.0400(10) Uani 1 1 d . . . . . H37 H -0.193724 1.180189 -0.219571 0.060 Uiso 1 1 calc R U . . . H38 H -0.194187 1.240865 -0.287701 0.060 Uiso 1 1 calc R U . . . H39 H -0.100479 1.287297 -0.193001 0.060 Uiso 1 1 calc R U . . . C34 C -0.0100(3) 1.2275(3) -0.3135(3) 0.0402(10) Uani 1 1 d . . . . . H40 H 0.036727 1.294542 -0.271042 0.060 Uiso 1 1 calc R U . . . H41 H -0.059021 1.237026 -0.364165 0.060 Uiso 1 1 calc R U . . . H42 H 0.035748 1.189199 -0.331458 0.060 Uiso 1 1 calc R U . . . O3 O 0.5017(2) 0.4056(2) 0.64348(17) 0.0397(7) Uani 1 1 d . . . . . C35 C 0.4190(3) 0.3711(3) 0.6575(2) 0.0318(9) Uani 1 1 d . . . . . N3 N 0.4224(2) 0.3396(2) 0.72697(18) 0.0307(8) Uani 1 1 d . . . . . C36 C 0.5289(3) 0.3521(3) 0.7926(2) 0.0368(10) Uani 1 1 d . . . . . H52 H 0.511983 0.330865 0.840219 0.044 Uiso 1 1 calc R U . . . C37 C 0.5856(4) 0.2812(4) 0.7589(3) 0.0624(15) Uani 1 1 d . . . . . H53 H 0.534714 0.210974 0.732646 0.094 Uiso 1 1 calc R U . . . H54 H 0.649147 0.284108 0.806783 0.094 Uiso 1 1 calc R U . . . H55 H 0.609797 0.302586 0.715235 0.094 Uiso 1 1 calc R U . . . C38 C 0.6029(3) 0.4625(3) 0.8335(3) 0.0458(11) Uani 1 1 d . . . . . H56 H 0.630699 0.484122 0.791513 0.069 Uiso 1 1 calc R U . . . H57 H 0.664455 0.468643 0.884501 0.069 Uiso 1 1 calc R U . . . H58 H 0.561431 0.506284 0.850901 0.069 Uiso 1 1 calc R U . . . C39 C 0.3235(3) 0.2990(3) 0.7444(2) 0.0390(10) Uani 1 1 d . . . . . H59 H 0.259265 0.286817 0.691169 0.047 Uiso 1 1 calc R U . . . C40 C 0.3156(4) 0.3773(4) 0.8171(3) 0.0483(12) Uani 1 1 d . . . . . H60 H 0.378137 0.392581 0.870543 0.073 Uiso 1 1 calc R U . . . H61 H 0.247535 0.350065 0.825588 0.073 Uiso 1 1 calc R U . . . H62 H 0.316067 0.440253 0.802418 0.073 Uiso 1 1 calc R U . . . C41 C 0.3152(4) 0.1964(3) 0.7592(3) 0.0594(14) Uani 1 1 d . . . . . H63 H 0.327144 0.150545 0.712837 0.089 Uiso 1 1 calc R U . . . H64 H 0.242361 0.165995 0.759036 0.089 Uiso 1 1 calc R U . . . H65 H 0.370817 0.206419 0.815110 0.089 Uiso 1 1 calc R U . . . C42 C 0.3093(3) 0.3600(3) 0.5930(2) 0.0325(9) Uani 1 1 d . . . . . C43 C 0.2259(3) 0.2524(3) 0.5225(2) 0.0334(9) Uani 1 1 d . . . . . C44 C 0.2236(3) 0.3027(3) 0.4501(2) 0.0321(9) Uani 1 1 d . . . . . H66 H 0.230075 0.270660 0.393951 0.039 Uiso 1 1 calc R U . . . C45 C 0.3028(3) 0.4072(3) 0.5189(2) 0.0379(10) Uani 1 1 d . . . . . H67 H 0.366874 0.452459 0.512916 0.045 Uiso 1 1 calc R U . . . C46 C 0.2029(3) 0.4384(3) 0.5288(3) 0.0420(11) Uani 1 1 d . . . . . H68 H 0.193841 0.506914 0.531018 0.050 Uiso 1 1 calc R U . . . C47 C 0.2074(4) 0.3904(3) 0.6015(3) 0.0433(11) Uani 1 1 d . . . . . H69 H 0.200782 0.422962 0.657393 0.052 Uiso 1 1 calc R U . . . C48 C 0.1275(3) 0.2856(3) 0.5326(2) 0.0371(10) Uani 1 1 d . . . . . H70 H 0.062495 0.241244 0.538056 0.045 Uiso 1 1 calc R U . . . C49 C 0.1233(3) 0.3342(3) 0.4591(2) 0.0327(9) Uani 1 1 d . . . . . C50 C 0.2421(3) 0.1510(3) 0.5173(2) 0.0338(10) Uani 1 1 d . . . . . C51 C 0.3308(3) 0.1309(3) 0.4989(3) 0.0399(10) Uani 1 1 d . . . . . H43 H 0.380880 0.182524 0.490074 0.048 Uiso 1 1 calc R U . . . C52 C 0.3465(3) 0.0379(3) 0.4935(3) 0.0370(10) Uani 1 1 d . . . . . H44 H 0.406634 0.025914 0.479835 0.044 Uiso 1 1 calc R U . . . C53 C 0.2764(3) -0.0400(3) 0.5077(2) 0.0355(10) Uani 1 1 d . . . . . C54 C 0.1889(3) -0.0192(3) 0.5253(2) 0.0362(10) Uani 1 1 d . . . . . H45 H 0.139192 -0.070773 0.534473 0.043 Uiso 1 1 calc R U . . . C55 C 0.1710(3) 0.0739(3) 0.5301(2) 0.0358(10) Uani 1 1 d . . . . . H46 H 0.109723 0.085081 0.542289 0.043 Uiso 1 1 calc R U . . . C56 C 0.2957(3) -0.1398(3) 0.5034(2) 0.0276(9) Uani 1 1 d . . . . . C57 C 0.3572(3) -0.1749(3) 0.4584(3) 0.0408(11) Uani 1 1 d . . . . . H47 H 0.385457 -0.135910 0.426975 0.049 Uiso 1 1 calc R U . . . C58 C 0.3781(3) -0.2668(3) 0.4588(3) 0.0429(11) Uani 1 1 d . . . . . H48 H 0.421421 -0.289082 0.428400 0.052 Uiso 1 1 calc R U . . . C59 C 0.3378(3) -0.3241(3) 0.5017(3) 0.0410(11) Uani 1 1 d . . . . . H49 H 0.352366 -0.386629 0.501600 0.049 Uiso 1 1 calc R U . . . C60 C 0.2740(4) -0.2908(3) 0.5465(3) 0.0438(11) Uani 1 1 d . . . . . H50 H 0.244497 -0.330814 0.576679 0.053 Uiso 1 1 calc R U . . . C61 C 0.2543(3) -0.1998(3) 0.5465(3) 0.0378(10) Uani 1 1 d . . . . . H51 H 0.211109 -0.177638 0.577020 0.045 Uiso 1 1 calc R U . . . C62 C 0.0178(3) 0.3092(3) 0.3849(2) 0.0343(10) Uani 1 1 d . . . . . O4 O -0.0646(2) 0.2446(3) 0.38009(19) 0.0568(9) Uani 1 1 d . . . . . N4 N 0.0190(2) 0.3510(2) 0.32130(19) 0.0312(8) Uani 1 1 d . . . . . C63 C 0.1141(3) 0.4290(3) 0.3263(3) 0.0488(12) Uani 1 1 d . . . . . H71 H 0.173168 0.443418 0.383359 0.059 Uiso 1 1 calc R U . . . C64 C 0.1568(4) 0.3913(5) 0.2574(3) 0.083(2) Uani 1 1 d . . . . . H72 H 0.164385 0.324024 0.256907 0.125 Uiso 1 1 calc R U . . . H73 H 0.228246 0.439832 0.269466 0.125 Uiso 1 1 calc R U . . . H74 H 0.105479 0.385360 0.200764 0.125 Uiso 1 1 calc R U . . . C65 C 0.0886(5) 0.5284(4) 0.3266(4) 0.084(2) Uani 1 1 d . . . . . H75 H 0.031262 0.517516 0.271289 0.126 Uiso 1 1 calc R U . . . H76 H 0.154788 0.581877 0.334735 0.126 Uiso 1 1 calc R U . . . H77 H 0.063466 0.549660 0.373945 0.126 Uiso 1 1 calc R U . . . C66 C -0.0811(3) 0.3181(3) 0.2419(2) 0.0369(10) Uani 1 1 d . . . . . H78 H -0.062030 0.355989 0.203130 0.044 Uiso 1 1 calc R U . . . C67 C -0.1142(4) 0.2036(4) 0.1925(3) 0.0609(14) Uani 1 1 d . . . . . H79 H -0.052196 0.188527 0.180148 0.091 Uiso 1 1 calc R U . . . H80 H -0.175973 0.185778 0.137937 0.091 Uiso 1 1 calc R U . . . H81 H -0.135696 0.163399 0.227698 0.091 Uiso 1 1 calc R U . . . C68 C -0.1745(4) 0.3456(5) 0.2593(3) 0.0669(16) Uani 1 1 d . . . . . H82 H -0.198842 0.306649 0.294339 0.100 Uiso 1 1 calc R U . . . H83 H -0.234969 0.329059 0.204297 0.100 Uiso 1 1 calc R U . . . H84 H -0.150847 0.419100 0.290673 0.100 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0329(15) 0.0327(17) 0.0343(16) 0.0089(13) 0.0028(12) 0.0077(13) C1 0.023(2) 0.034(2) 0.026(2) 0.0099(19) 0.0105(17) 0.0072(19) N1 0.0220(16) 0.0353(19) 0.0229(17) 0.0100(15) -0.0006(14) 0.0060(15) C2 0.021(2) 0.039(2) 0.031(2) 0.0128(19) 0.0002(17) 0.0089(18) C3 0.038(2) 0.056(3) 0.039(2) 0.026(2) 0.004(2) 0.013(2) C4 0.037(2) 0.053(3) 0.046(3) 0.016(2) 0.005(2) 0.020(2) C5 0.023(2) 0.031(2) 0.028(2) 0.0079(18) 0.0036(17) 0.0071(18) C6 0.036(2) 0.048(3) 0.028(2) 0.005(2) 0.0068(19) 0.013(2) C7 0.026(2) 0.040(2) 0.031(2) 0.0102(19) 0.0005(18) 0.0011(19) C8 0.0221(19) 0.030(2) 0.0202(19) 0.0066(17) 0.0023(16) 0.0029(17) C9 0.0205(19) 0.030(2) 0.0238(19) 0.0069(17) 0.0060(16) 0.0053(17) C10 0.0203(19) 0.030(2) 0.0237(19) 0.0070(17) 0.0044(16) 0.0072(17) C11 0.022(2) 0.039(2) 0.0219(19) 0.0098(17) 0.0052(16) 0.0086(18) C12 0.0169(18) 0.036(2) 0.025(2) 0.0105(18) 0.0046(16) 0.0033(17) C13 0.0221(19) 0.032(2) 0.024(2) 0.0093(17) 0.0033(16) 0.0030(17) C14 0.0210(19) 0.035(2) 0.0178(18) 0.0051(17) 0.0030(15) 0.0054(17) C15 0.0206(19) 0.031(2) 0.0221(19) 0.0088(17) 0.0057(16) 0.0045(17) C16 0.0220(19) 0.032(2) 0.0154(18) 0.0071(16) 0.0032(15) 0.0068(18) C17 0.021(2) 0.031(2) 0.032(2) 0.0091(18) 0.0073(17) 0.0009(18) C18 0.024(2) 0.033(2) 0.031(2) 0.0100(18) 0.0102(17) 0.0087(18) C19 0.0214(19) 0.033(2) 0.0141(18) 0.0093(16) 0.0010(15) 0.0045(17) C20 0.028(2) 0.028(2) 0.0201(19) 0.0096(16) 0.0056(16) 0.0074(18) C21 0.026(2) 0.036(2) 0.0181(18) 0.0110(17) 0.0043(16) 0.0138(18) C22 0.0233(19) 0.034(2) 0.0214(19) 0.0123(17) 0.0060(16) 0.0060(18) C23 0.030(2) 0.036(2) 0.028(2) 0.0121(18) 0.0117(18) 0.0086(19) C24 0.033(2) 0.043(3) 0.035(2) 0.017(2) 0.0186(19) 0.018(2) C25 0.025(2) 0.053(3) 0.037(2) 0.028(2) 0.0104(19) 0.009(2) C26 0.028(2) 0.043(3) 0.030(2) 0.017(2) 0.0069(18) 0.001(2) C27 0.031(2) 0.034(2) 0.026(2) 0.0126(18) 0.0113(17) 0.0114(19) C28 0.0188(19) 0.037(2) 0.022(2) 0.0098(18) 0.0086(16) 0.0060(18) O2 0.0236(14) 0.0371(17) 0.0279(14) 0.0110(13) 0.0046(11) 0.0071(13) N2 0.0209(16) 0.0344(19) 0.0209(16) 0.0086(15) 0.0007(13) 0.0060(15) C29 0.026(2) 0.035(2) 0.030(2) 0.0077(19) -0.0023(18) 0.0050(19) C30 0.054(3) 0.044(3) 0.035(2) 0.003(2) -0.002(2) 0.016(2) C31 0.034(3) 0.051(3) 0.061(3) 0.023(3) -0.001(2) -0.004(2) C32 0.028(2) 0.039(2) 0.022(2) 0.0113(18) 0.0014(17) 0.0102(19) C33 0.028(2) 0.057(3) 0.034(2) 0.019(2) 0.0039(19) 0.020(2) C34 0.038(2) 0.054(3) 0.030(2) 0.020(2) 0.0103(19) 0.015(2) O3 0.0377(17) 0.0523(18) 0.0346(16) 0.0192(14) 0.0149(14) 0.0170(15) C35 0.038(2) 0.034(2) 0.024(2) 0.0121(18) 0.0086(19) 0.016(2) N3 0.0300(18) 0.0390(19) 0.0212(17) 0.0116(15) 0.0054(14) 0.0116(16) C36 0.037(2) 0.050(3) 0.023(2) 0.015(2) 0.0028(18) 0.020(2) C37 0.070(3) 0.087(4) 0.043(3) 0.024(3) 0.013(3) 0.055(3) C38 0.033(2) 0.061(3) 0.033(2) 0.013(2) 0.004(2) 0.011(2) C39 0.035(2) 0.050(3) 0.023(2) 0.018(2) 0.0014(18) 0.005(2) C40 0.040(3) 0.073(3) 0.030(2) 0.018(2) 0.013(2) 0.013(2) C41 0.061(3) 0.054(3) 0.038(3) 0.023(2) -0.004(2) -0.007(3) C42 0.035(2) 0.034(2) 0.028(2) 0.0127(18) 0.0070(18) 0.0114(19) C43 0.037(2) 0.032(2) 0.035(2) 0.0180(19) 0.0113(19) 0.0121(19) C44 0.033(2) 0.040(2) 0.027(2) 0.0155(19) 0.0113(18) 0.013(2) C45 0.036(2) 0.037(2) 0.033(2) 0.0178(19) 0.0038(19) 0.003(2) C46 0.051(3) 0.032(2) 0.033(2) 0.0103(19) -0.001(2) 0.018(2) C47 0.054(3) 0.054(3) 0.026(2) 0.010(2) 0.013(2) 0.032(2) C48 0.033(2) 0.055(3) 0.031(2) 0.025(2) 0.0136(19) 0.014(2) C49 0.032(2) 0.040(2) 0.028(2) 0.0152(19) 0.0081(18) 0.0139(19) C50 0.034(2) 0.036(2) 0.027(2) 0.0125(18) 0.0058(18) 0.007(2) C51 0.036(2) 0.044(3) 0.044(3) 0.020(2) 0.018(2) 0.012(2) C52 0.029(2) 0.035(2) 0.045(3) 0.022(2) 0.0101(19) 0.0034(19) C53 0.028(2) 0.039(2) 0.029(2) 0.0105(19) 0.0001(18) 0.006(2) C54 0.040(2) 0.038(2) 0.035(2) 0.016(2) 0.015(2) 0.012(2) C55 0.034(2) 0.044(3) 0.032(2) 0.014(2) 0.0139(19) 0.012(2) C56 0.025(2) 0.031(2) 0.0199(19) 0.0076(17) 0.0019(16) 0.0044(18) C57 0.034(2) 0.047(3) 0.033(2) 0.011(2) 0.007(2) 0.007(2) C58 0.040(3) 0.039(3) 0.038(2) 0.006(2) 0.001(2) 0.015(2) C59 0.037(2) 0.041(3) 0.033(2) 0.008(2) 0.000(2) 0.011(2) C60 0.057(3) 0.032(2) 0.034(2) 0.011(2) 0.011(2) 0.006(2) C61 0.035(2) 0.035(2) 0.033(2) 0.0109(19) 0.0032(19) 0.004(2) C62 0.029(2) 0.050(3) 0.028(2) 0.019(2) 0.0110(18) 0.015(2) O4 0.0376(18) 0.087(2) 0.0458(19) 0.0379(18) 0.0115(15) 0.0076(18) N4 0.0263(17) 0.044(2) 0.0251(17) 0.0168(16) 0.0061(14) 0.0136(16) C63 0.027(2) 0.064(3) 0.046(3) 0.037(2) -0.002(2) 0.000(2) C64 0.041(3) 0.174(6) 0.064(4) 0.077(4) 0.026(3) 0.040(4) C65 0.086(4) 0.053(3) 0.070(4) 0.037(3) -0.022(3) -0.003(3) C66 0.028(2) 0.060(3) 0.028(2) 0.020(2) 0.0080(18) 0.018(2) C67 0.066(3) 0.053(3) 0.040(3) 0.015(2) -0.005(2) 0.008(3) C68 0.047(3) 0.126(5) 0.043(3) 0.038(3) 0.015(2) 0.048(3) 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 O1 C1 N1 122.3(3) . . ? O1 C1 C8 117.9(3) . . ? N1 C1 C8 119.7(3) . . ? C1 N1 C5 122.7(3) . . ? C1 N1 C2 119.5(3) . . ? C5 N1 C2 117.8(3) . . ? N1 C2 C4 112.2(3) . . ? N1 C2 C3 113.0(3) . . ? C4 C2 C3 112.3(3) . . ? N1 C2 H10 106.2 . . ? C4 C2 H10 106.2 . . ? C3 C2 H10 106.2 . . ? C2 C3 H11 109.5 . . ? C2 C3 H12 109.5 . . ? H11 C3 H12 109.5 . . ? C2 C3 H13 109.5 . . ? H11 C3 H13 109.5 . . ? H12 C3 H13 109.5 . . ? C2 C4 H14 109.5 . . ? C2 C4 H15 109.5 . . ? H14 C4 H15 109.5 . . ? C2 C4 H16 109.5 . . ? H14 C4 H16 109.5 . . ? H15 C4 H16 109.5 . . ? N1 C5 C6 111.1(3) . . ? N1 C5 C7 112.0(3) . . ? C6 C5 C7 111.7(3) . . ? N1 C5 H17 107.3 . . ? C6 C5 H17 107.3 . . ? C7 C5 H17 107.3 . . ? C5 C6 H18 109.5 . . ? C5 C6 H19 109.5 . . ? H18 C6 H19 109.5 . . ? C5 C6 H20 109.5 . . ? H18 C6 H20 109.5 . . ? H19 C6 H20 109.5 . . ? C5 C7 H21 109.5 . . ? C5 C7 H22 109.5 . . ? H21 C7 H22 109.5 . . ? C5 C7 H23 109.5 . . ? H21 C7 H23 109.5 . . ? H22 C7 H23 109.5 . . ? C1 C8 C13 119.9(3) . . ? C1 C8 C11 133.2(3) . . ? C13 C8 C11 89.6(3) . . ? C1 C8 C9 123.1(3) . . ? C13 C8 C9 89.9(3) . . ? C11 C8 C9 89.2(3) . . ? C16 C9 C10 127.6(3) . . ? C16 C9 C14 123.9(3) . . ? C10 C9 C14 89.7(3) . . ? C16 C9 C8 125.6(3) . . ? C10 C9 C8 89.6(3) . . ? C14 C9 C8 88.7(2) . . ? C15 C10 C9 90.6(3) . . ? C15 C10 C11 90.7(3) . . ? C9 C10 C11 90.6(3) . . ? C15 C10 H24 124.8 . . ? C9 C10 H24 124.8 . . ? C11 C10 H24 124.8 . . ? C12 C11 C10 89.7(3) . . ? C12 C11 C8 90.2(3) . . ? C10 C11 C8 90.7(3) . . ? C12 C11 H25 125.1 . . ? C10 C11 H25 125.1 . . ? C8 C11 H25 125.1 . . ? C11 C12 C13 89.8(3) . . ? C11 C12 C15 90.1(3) . . ? C13 C12 C15 90.2(3) . . ? C11 C12 H26 125.2 . . ? C13 C12 H26 125.2 . . ? C15 C12 H26 125.2 . . ? C8 C13 C14 90.7(3) . . ? C8 C13 C12 90.4(3) . . ? C14 C13 C12 90.1(3) . . ? C8 C13 H27 125.0 . . ? C14 C13 H27 125.0 . . ? C12 C13 H27 125.0 . . ? C13 C14 C15 90.5(3) . . ? C13 C14 C9 90.7(3) . . ? C15 C14 C9 89.5(3) . . ? C13 C14 H28 125.1 . . ? C15 C14 H28 125.1 . . ? C9 C14 H28 125.1 . . ? C28 C15 C10 120.5(3) . . ? C28 C15 C14 128.1(3) . . ? C10 C15 C14 90.1(3) . . ? C28 C15 C12 127.9(3) . . ? C10 C15 C12 89.5(3) . . ? C14 C15 C12 89.2(3) . . ? C17 C16 C21 117.7(3) . . ? C17 C16 C9 120.4(3) . . ? C21 C16 C9 121.9(3) . . ? C18 C17 C16 121.6(4) . . ? C18 C17 H1 119.2 . . ? C16 C17 H1 119.2 . . ? C17 C18 C19 120.7(4) . . ? C17 C18 H2 119.6 . . ? C19 C18 H2 119.6 . . ? C20 C19 C18 117.3(3) . . ? C20 C19 C22 122.2(3) . . ? C18 C19 C22 120.5(3) . . ? C19 C20 C21 121.6(3) . . ? C19 C20 H3 119.2 . . ? C21 C20 H3 119.2 . . ? C20 C21 C16 121.0(3) . . ? C20 C21 H4 119.5 . . ? C16 C21 H4 119.5 . . ? C23 C22 C27 117.9(3) . . ? C23 C22 C19 121.1(3) . . ? C27 C22 C19 121.0(3) . . ? C22 C23 C24 120.9(4) . . ? C22 C23 H5 119.5 . . ? C24 C23 H5 119.5 . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H6 119.8 . . ? C23 C24 H6 119.8 . . ? C26 C25 C24 119.4(4) . . ? C26 C25 H7 120.3 . . ? C24 C25 H7 120.3 . . ? C25 C26 C27 120.6(4) . . ? C25 C26 H8 119.7 . . ? C27 C26 H8 119.7 . . ? C26 C27 C22 120.8(4) . . ? C26 C27 H9 119.6 . . ? C22 C27 H9 119.6 . . ? O2 C28 N2 122.9(3) . . ? O2 C28 C15 119.2(3) . . ? N2 C28 C15 117.8(3) . . ? C28 N2 C29 123.0(3) . . ? C28 N2 C32 120.0(3) . . ? C29 N2 C32 117.0(3) . . ? N2 C29 C30 111.2(3) . . ? N2 C29 C31 111.8(3) . . ? C30 C29 C31 112.8(4) . . ? N2 C29 H29 106.9 . . ? C30 C29 H29 106.9 . . ? C31 C29 H29 106.9 . . ? C29 C30 H30 109.5 . . ? C29 C30 H31 109.5 . . ? H30 C30 H31 109.5 . . ? C29 C30 H32 109.5 . . ? H30 C30 H32 109.5 . . ? H31 C30 H32 109.5 . . ? C29 C31 H33 109.5 . . ? C29 C31 H34 109.5 . . ? H33 C31 H34 109.5 . . ? C29 C31 H35 109.5 . . ? H33 C31 H35 109.5 . . ? H34 C31 H35 109.5 . . ? N2 C32 C33 112.1(3) . . ? N2 C32 C34 111.5(3) . . ? C33 C32 C34 112.9(3) . . ? N2 C32 H36 106.7 . . ? C33 C32 H36 106.7 . . ? C34 C32 H36 106.7 . . ? C32 C33 H37 109.5 . . ? C32 C33 H38 109.5 . . ? H37 C33 H38 109.5 . . ? C32 C33 H39 109.5 . . ? H37 C33 H39 109.5 . . ? H38 C33 H39 109.5 . . ? C32 C34 H40 109.5 . . ? C32 C34 H41 109.5 . . ? H40 C34 H41 109.5 . . ? C32 C34 H42 109.5 . . ? H40 C34 H42 109.5 . . ? H41 C34 H42 109.5 . . ? O3 C35 N3 122.5(3) . . ? O3 C35 C42 118.5(3) . . ? N3 C35 C42 118.9(4) . . ? C35 N3 C39 122.6(3) . . ? C35 N3 C36 120.2(3) . . ? C39 N3 C36 117.0(3) . . ? N3 C36 C37 112.5(3) . . ? N3 C36 C38 112.9(3) . . ? C37 C36 C38 112.3(4) . . ? N3 C36 H52 106.1 . . ? C37 C36 H52 106.1 . . ? C38 C36 H52 106.1 . . ? C36 C37 H53 109.5 . . ? C36 C37 H54 109.5 . . ? H53 C37 H54 109.5 . . ? C36 C37 H55 109.5 . . ? H53 C37 H55 109.5 . . ? H54 C37 H55 109.5 . . ? C36 C38 H56 109.5 . . ? C36 C38 H57 109.5 . . ? H56 C38 H57 109.5 . . ? C36 C38 H58 109.5 . . ? H56 C38 H58 109.5 . . ? H57 C38 H58 109.5 . . ? N3 C39 C40 110.9(3) . . ? N3 C39 C41 112.2(4) . . ? C40 C39 C41 112.9(4) . . ? N3 C39 H59 106.8 . . ? C40 C39 H59 106.8 . . ? C41 C39 H59 106.8 . . ? C39 C40 H60 109.5 . . ? C39 C40 H61 109.5 . . ? H60 C40 H61 109.5 . . ? C39 C40 H62 109.5 . . ? H60 C40 H62 109.5 . . ? H61 C40 H62 109.5 . . ? C39 C41 H63 109.5 . . ? C39 C41 H64 109.5 . . ? H63 C41 H64 109.5 . . ? C39 C41 H65 109.5 . . ? H63 C41 H65 109.5 . . ? H64 C41 H65 109.5 . . ? C35 C42 C45 120.3(3) . . ? C35 C42 C47 133.8(3) . . ? C45 C42 C47 89.3(3) . . ? C35 C42 C43 123.5(3) . . ? C45 C42 C43 89.3(3) . . ? C47 C42 C43 88.3(3) . . ? C50 C43 C48 128.0(3) . . ? C50 C43 C44 123.6(3) . . ? C48 C43 C44 90.0(3) . . ? C50 C43 C42 124.8(3) . . ? C48 C43 C42 90.1(3) . . ? C44 C43 C42 88.8(3) . . ? C49 C44 C45 90.2(3) . . ? C49 C44 C43 89.9(3) . . ? C45 C44 C43 90.9(3) . . ? C49 C44 H66 125.0 . . ? C45 C44 H66 125.0 . . ? C43 C44 H66 125.0 . . ? C42 C45 C46 90.2(3) . . ? C42 C45 C44 91.0(3) . . ? C46 C45 C44 89.9(3) . . ? C42 C45 H67 125.0 . . ? C46 C45 H67 125.0 . . ? C44 C45 H67 125.0 . . ? C47 C46 C45 90.3(3) . . ? C47 C46 C49 90.8(3) . . ? C45 C46 C49 90.2(3) . . ? C47 C46 H68 125.0 . . ? C45 C46 H68 125.0 . . ? C49 C46 H68 125.0 . . ? C46 C47 C48 89.9(3) . . ? C46 C47 C42 90.2(3) . . ? C48 C47 C42 91.1(3) . . ? C46 C47 H69 125.0 . . ? C48 C47 H69 125.0 . . ? C42 C47 H69 125.0 . . ? C43 C48 C49 90.3(3) . . ? C43 C48 C47 90.6(3) . . ? C49 C48 C47 90.0(3) . . ? C43 C48 H70 125.1 . . ? C49 C48 H70 125.1 . . ? C47 C48 H70 125.1 . . ? C62 C49 C48 120.8(3) . . ? C62 C49 C44 124.1(3) . . ? C48 C49 C44 89.8(3) . . ? C62 C49 C46 131.5(3) . . ? C48 C49 C46 89.3(3) . . ? C44 C49 C46 89.7(3) . . ? C55 C50 C51 117.9(4) . . ? C55 C50 C43 121.8(4) . . ? C51 C50 C43 120.3(4) . . ? C52 C51 C50 121.0(4) . . ? C52 C51 H43 119.5 . . ? C50 C51 H43 119.5 . . ? C51 C52 C53 121.7(4) . . ? C51 C52 H44 119.1 . . ? C53 C52 H44 119.1 . . ? C54 C53 C52 116.6(4) . . ? C54 C53 C56 122.2(4) . . ? C52 C53 C56 121.2(4) . . ? C53 C54 C55 122.5(4) . . ? C53 C54 H45 118.7 . . ? C55 C54 H45 118.7 . . ? C54 C55 C50 120.3(4) . . ? C54 C55 H46 119.9 . . ? C50 C55 H46 119.9 . . ? C61 C56 C57 117.8(4) . . ? C61 C56 C53 120.2(4) . . ? C57 C56 C53 122.0(3) . . ? C56 C57 C58 120.7(4) . . ? C56 C57 H47 119.7 . . ? C58 C57 H47 119.7 . . ? C59 C58 C57 120.9(4) . . ? C59 C58 H48 119.6 . . ? C57 C58 H48 119.6 . . ? C58 C59 C60 119.3(4) . . ? C58 C59 H49 120.3 . . ? C60 C59 H49 120.3 . . ? C61 C60 C59 119.6(4) . . ? C61 C60 H50 120.2 . . ? C59 C60 H50 120.2 . . ? C60 C61 C56 121.8(4) . . ? C60 C61 H51 119.1 . . ? C56 C61 H51 119.1 . . ? O4 C62 N4 122.4(3) . . ? O4 C62 C49 118.8(3) . . ? N4 C62 C49 118.6(3) . . ? C62 N4 C63 123.4(3) . . ? C62 N4 C66 119.7(3) . . ? C63 N4 C66 116.9(3) . . ? N4 C63 C64 111.8(4) . . ? N4 C63 C65 110.1(4) . . ? C64 C63 C65 113.7(4) . . ? N4 C63 H71 107.0 . . ? C64 C63 H71 107.0 . . ? C65 C63 H71 107.0 . . ? C63 C64 H72 109.5 . . ? C63 C64 H73 109.5 . . ? H72 C64 H73 109.5 . . ? C63 C64 H74 109.5 . . ? H72 C64 H74 109.5 . . ? H73 C64 H74 109.5 . . ? C63 C65 H75 109.5 . . ? C63 C65 H76 109.5 . . ? H75 C65 H76 109.5 . . ? C63 C65 H77 109.5 . . ? H75 C65 H77 109.5 . . ? H76 C65 H77 109.5 . . ? N4 C66 C68 113.2(3) . . ? N4 C66 C67 111.5(3) . . ? C68 C66 C67 111.4(4) . . ? N4 C66 H78 106.8 . . ? C68 C66 H78 106.8 . . ? C67 C66 H78 106.8 . . ? C66 C67 H79 109.5 . . ? C66 C67 H80 109.5 . . ? H79 C67 H80 109.5 . . ? C66 C67 H81 109.5 . . ? H79 C67 H81 109.5 . . ? H80 C67 H81 109.5 . . ? C66 C68 H82 109.5 . . ? C66 C68 H83 109.5 . . ? H82 C68 H83 109.5 . . ? C66 C68 H84 109.5 . . ? H82 C68 H84 109.5 . . ? H83 C68 H84 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.232(4) . ? C1 N1 1.348(5) . ? C1 C8 1.503(5) . ? N1 C5 1.476(5) . ? N1 C2 1.485(4) . ? C2 C4 1.515(6) . ? C2 C3 1.525(5) . ? C2 H10 1.0000 . ? C3 H11 0.9800 . ? C3 H12 0.9800 . ? C3 H13 0.9800 . ? C4 H14 0.9800 . ? C4 H15 0.9800 . ? C4 H16 0.9800 . ? C5 C6 1.512(5) . ? C5 C7 1.526(5) . ? C5 H17 1.0000 . ? C6 H18 0.9800 . ? C6 H19 0.9800 . ? C6 H20 0.9800 . ? C7 H21 0.9800 . ? C7 H22 0.9800 . ? C7 H23 0.9800 . ? C8 C13 1.556(5) . ? C8 C11 1.564(5) . ? C8 C9 1.597(5) . ? C9 C16 1.478(5) . ? C9 C10 1.559(5) . ? C9 C14 1.573(5) . ? C10 C15 1.552(5) . ? C10 C11 1.563(5) . ? C10 H24 1.0000 . ? C11 C12 1.557(5) . ? C11 H25 1.0000 . ? C12 C13 1.558(5) . ? C12 C15 1.574(5) . ? C12 H26 1.0000 . ? C13 C14 1.558(5) . ? C13 H27 1.0000 . ? C14 C15 1.568(5) . ? C14 H28 1.0000 . ? C15 C28 1.507(5) . ? C16 C17 1.385(5) . ? C16 C21 1.390(5) . ? C17 C18 1.383(5) . ? C17 H1 0.9500 . ? C18 C19 1.406(5) . ? C18 H2 0.9500 . ? C19 C20 1.386(5) . ? C19 C22 1.487(5) . ? C20 C21 1.386(5) . ? C20 H3 0.9500 . ? C21 H4 0.9500 . ? C22 C23 1.385(5) . ? C22 C27 1.400(5) . ? C23 C24 1.391(5) . ? C23 H5 0.9500 . ? C24 C25 1.381(6) . ? C24 H6 0.9500 . ? C25 C26 1.373(6) . ? C25 H7 0.9500 . ? C26 C27 1.385(5) . ? C26 H8 0.9500 . ? C27 H9 0.9500 . ? C28 O2 1.222(4) . ? C28 N2 1.357(4) . ? N2 C29 1.474(5) . ? N2 C32 1.489(4) . ? C29 C30 1.523(6) . ? C29 C31 1.524(6) . ? C29 H29 1.0000 . ? C30 H30 0.9800 . ? C30 H31 0.9800 . ? C30 H32 0.9800 . ? C31 H33 0.9800 . ? C31 H34 0.9800 . ? C31 H35 0.9800 . ? C32 C33 1.515(5) . ? C32 C34 1.522(5) . ? C32 H36 1.0000 . ? C33 H37 0.9800 . ? C33 H38 0.9800 . ? C33 H39 0.9800 . ? C34 H40 0.9800 . ? C34 H41 0.9800 . ? C34 H42 0.9800 . ? O3 C35 1.229(4) . ? C35 N3 1.356(5) . ? C35 C42 1.510(5) . ? N3 C39 1.475(5) . ? N3 C36 1.480(5) . ? C36 C37 1.508(6) . ? C36 C38 1.516(6) . ? C36 H52 1.0000 . ? C37 H53 0.9800 . ? C37 H54 0.9800 . ? C37 H55 0.9800 . ? C38 H56 0.9800 . ? C38 H57 0.9800 . ? C38 H58 0.9800 . ? C39 C40 1.511(6) . ? C39 C41 1.517(6) . ? C39 H59 1.0000 . ? C40 H60 0.9800 . ? C40 H61 0.9800 . ? C40 H62 0.9800 . ? C41 H63 0.9800 . ? C41 H64 0.9800 . ? C41 H65 0.9800 . ? C42 C45 1.554(5) . ? C42 C47 1.571(6) . ? C42 C43 1.612(5) . ? C43 C50 1.489(5) . ? C43 C48 1.552(5) . ? C43 C44 1.562(5) . ? C44 C49 1.561(5) . ? C44 C45 1.561(6) . ? C44 H66 1.0000 . ? C45 C46 1.557(6) . ? C45 H67 1.0000 . ? C46 C47 1.541(6) . ? C46 C49 1.564(6) . ? C46 H68 1.0000 . ? C47 C48 1.567(6) . ? C47 H69 1.0000 . ? C48 C49 1.560(5) . ? C48 H70 1.0000 . ? C49 C62 1.501(5) . ? C50 C55 1.386(5) . ? C50 C51 1.399(5) . ? C51 C52 1.368(6) . ? C51 H43 0.9500 . ? C52 C53 1.399(5) . ? C52 H44 0.9500 . ? C53 C54 1.381(5) . ? C53 C56 1.485(5) . ? C54 C55 1.383(5) . ? C54 H45 0.9500 . ? C55 H46 0.9500 . ? C56 C61 1.378(5) . ? C56 C57 1.388(5) . ? C57 C58 1.395(6) . ? C57 H47 0.9500 . ? C58 C59 1.345(6) . ? C58 H48 0.9500 . ? C59 C60 1.403(6) . ? C59 H49 0.9500 . ? C60 C61 1.375(6) . ? C60 H50 0.9500 . ? C61 H51 0.9500 . ? C62 O4 1.237(5) . ? C62 N4 1.356(5) . ? N4 C63 1.457(5) . ? N4 C66 1.487(5) . ? C63 C64 1.504(7) . ? C63 C65 1.524(7) . ? C63 H71 1.0000 . ? C64 H72 0.9800 . ? C64 H73 0.9800 . ? C64 H74 0.9800 . ? C65 H75 0.9800 . ? C65 H76 0.9800 . ? C65 H77 0.9800 . ? C66 C68 1.493(6) . ? C66 C67 1.533(6) . ? C66 H78 1.0000 . ? C67 H79 0.9800 . ? C67 H80 0.9800 . ? C67 H81 0.9800 . ? C68 H82 0.9800 . ? C68 H83 0.9800 . ? C68 H84 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 N1 C5 -179.3(3) . . . . ? C8 C1 N1 C5 3.5(5) . . . . ? O1 C1 N1 C2 0.1(5) . . . . ? C8 C1 N1 C2 -177.2(3) . . . . ? C1 N1 C2 C4 64.4(4) . . . . ? C5 N1 C2 C4 -116.3(4) . . . . ? C1 N1 C2 C3 -63.8(5) . . . . ? C5 N1 C2 C3 115.5(4) . . . . ? C1 N1 C5 C6 110.6(4) . . . . ? C2 N1 C5 C6 -68.7(4) . . . . ? C1 N1 C5 C7 -123.7(4) . . . . ? C2 N1 C5 C7 56.9(4) . . . . ? O1 C1 C8 C13 6.8(5) . . . . ? N1 C1 C8 C13 -175.8(3) . . . . ? O1 C1 C8 C11 128.8(4) . . . . ? N1 C1 C8 C11 -53.9(5) . . . . ? O1 C1 C8 C9 -105.1(4) . . . . ? N1 C1 C8 C9 72.2(5) . . . . ? C1 C8 C9 C16 -6.2(5) . . . . ? C13 C8 C9 C16 -132.7(4) . . . . ? C11 C8 C9 C16 137.8(3) . . . . ? C1 C8 C9 C10 -144.4(3) . . . . ? C13 C8 C9 C10 89.1(3) . . . . ? C11 C8 C9 C10 -0.5(2) . . . . ? C1 C8 C9 C14 125.9(3) . . . . ? C13 C8 C9 C14 -0.6(3) . . . . ? C11 C8 C9 C14 -90.2(3) . . . . ? C16 C9 C10 C15 133.0(4) . . . . ? C14 C9 C10 C15 -1.5(3) . . . . ? C8 C9 C10 C15 -90.2(3) . . . . ? C16 C9 C10 C11 -136.4(4) . . . . ? C14 C9 C10 C11 89.1(3) . . . . ? C8 C9 C10 C11 0.5(2) . . . . ? C15 C10 C11 C12 -0.1(3) . . . . ? C9 C10 C11 C12 -90.7(3) . . . . ? C15 C10 C11 C8 90.1(3) . . . . ? C9 C10 C11 C8 -0.5(3) . . . . ? C1 C8 C11 C12 -132.3(4) . . . . ? C13 C8 C11 C12 0.3(3) . . . . ? C9 C8 C11 C12 90.2(3) . . . . ? C1 C8 C11 C10 137.9(4) . . . . ? C13 C8 C11 C10 -89.4(3) . . . . ? C9 C8 C11 C10 0.5(2) . . . . ? C10 C11 C12 C13 90.3(3) . . . . ? C8 C11 C12 C13 -0.3(3) . . . . ? C10 C11 C12 C15 0.1(3) . . . . ? C8 C11 C12 C15 -90.6(3) . . . . ? C1 C8 C13 C14 -128.4(3) . . . . ? C11 C8 C13 C14 89.8(3) . . . . ? C9 C8 C13 C14 0.6(3) . . . . ? C1 C8 C13 C12 141.5(3) . . . . ? C11 C8 C13 C12 -0.3(3) . . . . ? C9 C8 C13 C12 -89.5(3) . . . . ? C11 C12 C13 C8 0.3(3) . . . . ? C15 C12 C13 C8 90.4(3) . . . . ? C11 C12 C13 C14 -90.4(3) . . . . ? C15 C12 C13 C14 -0.3(3) . . . . ? C8 C13 C14 C15 -90.2(3) . . . . ? C12 C13 C14 C15 0.3(3) . . . . ? C8 C13 C14 C9 -0.6(3) . . . . ? C12 C13 C14 C9 89.8(3) . . . . ? C16 C9 C14 C13 134.0(3) . . . . ? C10 C9 C14 C13 -89.0(3) . . . . ? C8 C9 C14 C13 0.6(3) . . . . ? C16 C9 C14 C15 -135.6(3) . . . . ? C10 C9 C14 C15 1.5(3) . . . . ? C8 C9 C14 C15 91.1(3) . . . . ? C9 C10 C15 C28 -134.3(3) . . . . ? C11 C10 C15 C28 135.1(3) . . . . ? C9 C10 C15 C14 1.5(3) . . . . ? C11 C10 C15 C14 -89.1(3) . . . . ? C9 C10 C15 C12 90.7(3) . . . . ? C11 C10 C15 C12 0.1(3) . . . . ? C13 C14 C15 C28 -140.5(4) . . . . ? C9 C14 C15 C28 128.7(4) . . . . ? C13 C14 C15 C10 89.2(3) . . . . ? C9 C14 C15 C10 -1.5(3) . . . . ? C13 C14 C15 C12 -0.3(3) . . . . ? C9 C14 C15 C12 -91.0(3) . . . . ? C11 C12 C15 C28 -129.6(4) . . . . ? C13 C12 C15 C28 140.6(4) . . . . ? C11 C12 C15 C10 -0.1(3) . . . . ? C13 C12 C15 C10 -89.9(3) . . . . ? C11 C12 C15 C14 90.1(3) . . . . ? C13 C12 C15 C14 0.3(3) . . . . ? C10 C9 C16 C17 175.3(3) . . . . ? C14 C9 C16 C17 -64.0(5) . . . . ? C8 C9 C16 C17 52.6(5) . . . . ? C10 C9 C16 C21 -5.6(5) . . . . ? C14 C9 C16 C21 115.1(4) . . . . ? C8 C9 C16 C21 -128.4(4) . . . . ? C21 C16 C17 C18 0.8(5) . . . . ? C9 C16 C17 C18 179.9(3) . . . . ? C16 C17 C18 C19 -0.5(6) . . . . ? C17 C18 C19 C20 -0.5(5) . . . . ? C17 C18 C19 C22 178.9(3) . . . . ? C18 C19 C20 C21 1.3(5) . . . . ? C22 C19 C20 C21 -178.1(3) . . . . ? C19 C20 C21 C16 -1.0(5) . . . . ? C17 C16 C21 C20 -0.1(5) . . . . ? C9 C16 C21 C20 -179.1(3) . . . . ? C20 C19 C22 C23 -154.8(3) . . . . ? C18 C19 C22 C23 25.8(5) . . . . ? C20 C19 C22 C27 25.8(5) . . . . ? C18 C19 C22 C27 -153.6(3) . . . . ? C27 C22 C23 C24 1.3(5) . . . . ? C19 C22 C23 C24 -178.1(3) . . . . ? C22 C23 C24 C25 -0.7(6) . . . . ? C23 C24 C25 C26 -0.5(6) . . . . ? C24 C25 C26 C27 1.0(6) . . . . ? C25 C26 C27 C22 -0.4(5) . . . . ? C23 C22 C27 C26 -0.8(5) . . . . ? C19 C22 C27 C26 178.6(3) . . . . ? C10 C15 C28 O2 -1.8(5) . . . . ? C14 C15 C28 O2 -119.5(4) . . . . ? C12 C15 C28 O2 114.6(4) . . . . ? C10 C15 C28 N2 177.2(3) . . . . ? C14 C15 C28 N2 59.6(5) . . . . ? C12 C15 C28 N2 -66.3(5) . . . . ? O2 C28 N2 C29 179.0(3) . . . . ? C15 C28 N2 C29 0.0(5) . . . . ? O2 C28 N2 C32 -1.1(5) . . . . ? C15 C28 N2 C32 179.8(3) . . . . ? C28 N2 C29 C30 -115.6(4) . . . . ? C32 N2 C29 C30 64.5(4) . . . . ? C28 N2 C29 C31 117.3(4) . . . . ? C32 N2 C29 C31 -62.5(4) . . . . ? C28 N2 C32 C33 -64.5(4) . . . . ? C29 N2 C32 C33 115.4(4) . . . . ? C28 N2 C32 C34 63.1(4) . . . . ? C29 N2 C32 C34 -117.0(4) . . . . ? O3 C35 N3 C39 179.4(4) . . . . ? C42 C35 N3 C39 -2.8(5) . . . . ? O3 C35 N3 C36 3.9(5) . . . . ? C42 C35 N3 C36 -178.3(3) . . . . ? C35 N3 C36 C37 -70.2(5) . . . . ? C39 N3 C36 C37 114.0(4) . . . . ? C35 N3 C36 C38 58.2(5) . . . . ? C39 N3 C36 C38 -117.6(4) . . . . ? C35 N3 C39 C40 -104.5(4) . . . . ? C36 N3 C39 C40 71.2(4) . . . . ? C35 N3 C39 C41 128.2(4) . . . . ? C36 N3 C39 C41 -56.1(4) . . . . ? O3 C35 C42 C45 -9.6(5) . . . . ? N3 C35 C42 C45 172.6(3) . . . . ? O3 C35 C42 C47 -132.1(4) . . . . ? N3 C35 C42 C47 50.0(6) . . . . ? O3 C35 C42 C43 102.1(4) . . . . ? N3 C35 C42 C43 -75.7(5) . . . . ? C35 C42 C43 C50 5.6(6) . . . . ? C45 C42 C43 C50 132.2(4) . . . . ? C47 C42 C43 C50 -138.5(4) . . . . ? C35 C42 C43 C48 144.3(4) . . . . ? C45 C42 C43 C48 -89.1(3) . . . . ? C47 C42 C43 C48 0.2(3) . . . . ? C35 C42 C43 C44 -125.7(4) . . . . ? C45 C42 C43 C44 0.9(3) . . . . ? C47 C42 C43 C44 90.2(3) . . . . ? C50 C43 C44 C49 136.7(4) . . . . ? C48 C43 C44 C49 -1.0(3) . . . . ? C42 C43 C44 C49 -91.1(3) . . . . ? C50 C43 C44 C45 -133.1(4) . . . . ? C48 C43 C44 C45 89.2(3) . . . . ? C42 C43 C44 C45 -0.9(3) . . . . ? C35 C42 C45 C46 -141.7(4) . . . . ? C47 C42 C45 C46 0.8(3) . . . . ? C43 C42 C45 C46 89.1(3) . . . . ? C35 C42 C45 C44 128.3(3) . . . . ? C47 C42 C45 C44 -89.2(3) . . . . ? C43 C42 C45 C44 -0.9(3) . . . . ? C49 C44 C45 C42 90.8(3) . . . . ? C43 C44 C45 C42 0.9(3) . . . . ? C49 C44 C45 C46 0.6(3) . . . . ? C43 C44 C45 C46 -89.3(3) . . . . ? C42 C45 C46 C47 -0.8(3) . . . . ? C44 C45 C46 C47 90.2(3) . . . . ? C42 C45 C46 C49 -91.6(3) . . . . ? C44 C45 C46 C49 -0.6(3) . . . . ? C45 C46 C47 C48 -90.3(3) . . . . ? C49 C46 C47 C48 -0.1(3) . . . . ? C45 C46 C47 C42 0.8(3) . . . . ? C49 C46 C47 C42 91.0(3) . . . . ? C35 C42 C47 C46 132.5(4) . . . . ? C45 C42 C47 C46 -0.8(3) . . . . ? C43 C42 C47 C46 -90.1(3) . . . . ? C35 C42 C47 C48 -137.6(4) . . . . ? C45 C42 C47 C48 89.1(3) . . . . ? C43 C42 C47 C48 -0.2(3) . . . . ? C50 C43 C48 C49 -133.6(4) . . . . ? C44 C43 C48 C49 1.0(3) . . . . ? C42 C43 C48 C49 89.8(3) . . . . ? C50 C43 C48 C47 136.4(4) . . . . ? C44 C43 C48 C47 -89.0(3) . . . . ? C42 C43 C48 C47 -0.2(3) . . . . ? C46 C47 C48 C43 90.4(3) . . . . ? C42 C47 C48 C43 0.2(3) . . . . ? C46 C47 C48 C49 0.1(3) . . . . ? C42 C47 C48 C49 -90.1(3) . . . . ? C43 C48 C49 C62 129.5(4) . . . . ? C47 C48 C49 C62 -139.9(4) . . . . ? C43 C48 C49 C44 -1.0(3) . . . . ? C47 C48 C49 C44 89.6(3) . . . . ? C43 C48 C49 C46 -90.7(3) . . . . ? C47 C48 C49 C46 -0.1(3) . . . . ? C45 C44 C49 C62 142.1(4) . . . . ? C43 C44 C49 C62 -126.9(4) . . . . ? C45 C44 C49 C48 -89.9(3) . . . . ? C43 C44 C49 C48 1.0(3) . . . . ? C45 C44 C49 C46 -0.6(3) . . . . ? C43 C44 C49 C46 90.3(3) . . . . ? C47 C46 C49 C62 132.3(4) . . . . ? C45 C46 C49 C62 -137.4(4) . . . . ? C47 C46 C49 C48 0.1(3) . . . . ? C45 C46 C49 C48 90.4(3) . . . . ? C47 C46 C49 C44 -89.6(3) . . . . ? C45 C46 C49 C44 0.6(3) . . . . ? C48 C43 C50 C55 -6.7(6) . . . . ? C44 C43 C50 C55 -128.0(4) . . . . ? C42 C43 C50 C55 116.4(4) . . . . ? C48 C43 C50 C51 173.2(4) . . . . ? C44 C43 C50 C51 51.9(5) . . . . ? C42 C43 C50 C51 -63.7(5) . . . . ? C55 C50 C51 C52 0.2(6) . . . . ? C43 C50 C51 C52 -179.7(4) . . . . ? C50 C51 C52 C53 -1.2(6) . . . . ? C51 C52 C53 C54 1.5(6) . . . . ? C51 C52 C53 C56 -178.7(4) . . . . ? C52 C53 C54 C55 -0.8(6) . . . . ? C56 C53 C54 C55 179.4(3) . . . . ? C53 C54 C55 C50 -0.2(6) . . . . ? C51 C50 C55 C54 0.5(6) . . . . ? C43 C50 C55 C54 -179.7(4) . . . . ? C54 C53 C56 C61 -24.0(5) . . . . ? C52 C53 C56 C61 156.2(4) . . . . ? C54 C53 C56 C57 157.6(4) . . . . ? C52 C53 C56 C57 -22.2(5) . . . . ? C61 C56 C57 C58 -1.4(5) . . . . ? C53 C56 C57 C58 177.1(4) . . . . ? C56 C57 C58 C59 1.0(6) . . . . ? C57 C58 C59 C60 0.0(6) . . . . ? C58 C59 C60 C61 -0.5(6) . . . . ? C59 C60 C61 C56 0.1(6) . . . . ? C57 C56 C61 C60 0.9(6) . . . . ? C53 C56 C61 C60 -177.6(4) . . . . ? C48 C49 C62 O4 -4.3(6) . . . . ? C44 C49 C62 O4 109.1(4) . . . . ? C46 C49 C62 O4 -124.8(5) . . . . ? C48 C49 C62 N4 -178.1(3) . . . . ? C44 C49 C62 N4 -64.7(5) . . . . ? C46 C49 C62 N4 61.4(6) . . . . ? O4 C62 N4 C63 178.5(4) . . . . ? C49 C62 N4 C63 -7.9(6) . . . . ? O4 C62 N4 C66 -0.8(6) . . . . ? C49 C62 N4 C66 172.7(3) . . . . ? C62 N4 C63 C64 116.3(4) . . . . ? C66 N4 C63 C64 -64.4(5) . . . . ? C62 N4 C63 C65 -116.3(4) . . . . ? C66 N4 C63 C65 63.0(5) . . . . ? C62 N4 C66 C68 64.8(5) . . . . ? C63 N4 C66 C68 -114.6(4) . . . . ? C62 N4 C66 C67 -61.8(5) . . . . ? C63 N4 C66 C67 118.8(4) . . . . ?