# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Xin Zhao' 'Xi-Kui Jiang' 'Zhan-Ting Li' 'Yun-Xiang Xu' _publ_contact_author_name 'Xin Zhao' _publ_contact_author_email XZHAO@MAIL.SIOC.AC.CN data_XYX _database_code_depnum_ccdc_archive 'CCDC 715335' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H96 N6 O9' _chemical_formula_weight 1045.43 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.1075(8) _cell_length_b 20.1933(11) _cell_length_c 23.5204(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.509(2) _cell_angle_gamma 90.00 _cell_volume 6698.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.475 _exptl_crystal_size_mid 0.314 _exptl_crystal_size_min 0.265 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.037 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.693712 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75209 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.01 _reflns_number_total 11753 _reflns_number_gt 7743 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+9.6703P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11753 _refine_ls_number_parameters 703 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.2335 _refine_ls_wR_factor_gt 0.1812 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2176(2) 0.84329(15) 0.19995(13) 0.0358(7) Uani 1 1 d . . . C2 C 0.1833(2) 0.84853(15) 0.25413(13) 0.0353(7) Uani 1 1 d . . . H2A H 0.1168 0.8496 0.2596 0.042 Uiso 1 1 calc R . . C3 C 0.2455(2) 0.85221(14) 0.30063(13) 0.0324(7) Uani 1 1 d . . . C4 C 0.3424(2) 0.85252(14) 0.29275(13) 0.0328(7) Uani 1 1 d . . . H4A H 0.3851 0.8553 0.3246 0.039 Uiso 1 1 calc R . . C5 C 0.3772(2) 0.84867(14) 0.23775(13) 0.0330(7) Uani 1 1 d . . . C6 C 0.3152(2) 0.84345(15) 0.19179(13) 0.0359(7) Uani 1 1 d . . . H6A H 0.3389 0.8400 0.1545 0.043 Uiso 1 1 calc R . . C7 C 0.4818(2) 0.85570(16) 0.23032(14) 0.0391(7) Uani 1 1 d . . . C8 C 0.6214(2) 0.8227(2) 0.17445(17) 0.0568(11) Uani 1 1 d . . . C9 C 0.6481(3) 0.8931(2) 0.1589(2) 0.0759(13) Uani 1 1 d . . . H9A H 0.6413 0.9219 0.1921 0.114 Uiso 1 1 calc R . . H9B H 0.6062 0.9087 0.1278 0.114 Uiso 1 1 calc R . . H9C H 0.7140 0.8941 0.1467 0.114 Uiso 1 1 calc R . . C10 C 0.6312(3) 0.7779(3) 0.1226(2) 0.105(2) Uani 1 1 d . . . H10A H 0.6139 0.7324 0.1327 0.157 Uiso 1 1 calc R . . H10B H 0.6970 0.7788 0.1102 0.157 Uiso 1 1 calc R . . H10C H 0.5890 0.7936 0.0917 0.157 Uiso 1 1 calc R . . C11 C 0.6819(3) 0.7979(3) 0.2234(2) 0.0762(13) Uani 1 1 d . . . H11A H 0.6750 0.8274 0.2561 0.114 Uiso 1 1 calc R . . H11B H 0.7485 0.7971 0.2124 0.114 Uiso 1 1 calc R . . H11C H 0.6619 0.7531 0.2336 0.114 Uiso 1 1 calc R . . C12 C 0.2030(2) 0.85912(15) 0.35805(13) 0.0355(7) Uani 1 1 d . . . C13 C 0.2217(2) 0.83569(17) 0.46192(14) 0.0436(8) Uani 1 1 d . . . C14 C 0.1318(3) 0.7949(2) 0.46795(16) 0.0594(10) Uani 1 1 d . . . H14A H 0.1435 0.7493 0.4556 0.089 Uiso 1 1 calc R . . H14B H 0.0807 0.8142 0.4443 0.089 Uiso 1 1 calc R . . H14C H 0.1133 0.7948 0.5078 0.089 Uiso 1 1 calc R . . C15 C 0.3024(3) 0.8049(2) 0.49710(15) 0.0597(10) Uani 1 1 d . . . H15A H 0.3117 0.7590 0.4851 0.090 Uiso 1 1 calc R . . H15B H 0.2867 0.8059 0.5374 0.090 Uiso 1 1 calc R . . H15C H 0.3608 0.8301 0.4915 0.090 Uiso 1 1 calc R . . C16 C 0.2071(3) 0.9073(2) 0.48058(17) 0.0593(10) Uani 1 1 d . . . H16A H 0.2662 0.9321 0.4765 0.089 Uiso 1 1 calc R . . H16B H 0.1886 0.9082 0.5205 0.089 Uiso 1 1 calc R . . H16C H 0.1569 0.9276 0.4568 0.089 Uiso 1 1 calc R . . C17 C 0.0620(2) 0.8374(2) 0.15796(15) 0.0525(9) Uani 1 1 d . . . H17A H 0.0403 0.8803 0.1733 0.063 Uiso 1 1 calc R . . H17B H 0.0443 0.8019 0.1847 0.063 Uiso 1 1 calc R . . C18 C 0.0161(3) 0.8252(2) 0.10080(17) 0.0612(11) Uani 1 1 d . . . H18A H 0.0397 0.8592 0.0737 0.073 Uiso 1 1 calc R . . C19 C -0.0901(3) 0.8332(4) 0.1051(2) 0.108(2) Uani 1 1 d . . . H19A H -0.1044 0.8778 0.1189 0.162 Uiso 1 1 calc R . . H19B H -0.1144 0.8003 0.1317 0.162 Uiso 1 1 calc R . . H19C H -0.1203 0.8266 0.0675 0.162 Uiso 1 1 calc R . . C20 C 0.0421(3) 0.7571(2) 0.07852(19) 0.0773(13) Uani 1 1 d . . . H20A H 0.1112 0.7536 0.0763 0.116 Uiso 1 1 calc R . . H20B H 0.0131 0.7508 0.0406 0.116 Uiso 1 1 calc R . . H20C H 0.0188 0.7231 0.1043 0.116 Uiso 1 1 calc R . . C21 C 0.1875(2) 0.68046(16) 0.26252(14) 0.0409(8) Uani 1 1 d . . . C22 C 0.2205(2) 0.67749(15) 0.20728(14) 0.0378(7) Uani 1 1 d . . . H22A H 0.1768 0.6750 0.1760 0.045 Uiso 1 1 calc R . . C23 C 0.3165(2) 0.67815(15) 0.19799(13) 0.0354(7) Uani 1 1 d . . . C24 C 0.3807(2) 0.68143(15) 0.24422(13) 0.0368(7) Uani 1 1 d . . . H24A H 0.4470 0.6817 0.2380 0.044 Uiso 1 1 calc R . . C25 C 0.3476(2) 0.68432(15) 0.29886(13) 0.0379(7) Uani 1 1 d . . . C26 C 0.2503(2) 0.68423(15) 0.30814(14) 0.0408(8) Uani 1 1 d . . . H26A H 0.2275 0.6868 0.3457 0.049 Uiso 1 1 calc R . . C27 C 0.4131(2) 0.69309(17) 0.34923(14) 0.0440(8) Uani 1 1 d . . . C28 C 0.5734(3) 0.6643(2) 0.38993(16) 0.0647(12) Uani 1 1 d . . . C29 C 0.6036(4) 0.7359(3) 0.3995(2) 0.0955(17) Uani 1 1 d . . . H29A H 0.6241 0.7550 0.3635 0.143 Uiso 1 1 calc R . . H29B H 0.6562 0.7375 0.4275 0.143 Uiso 1 1 calc R . . H29C H 0.5500 0.7614 0.4136 0.143 Uiso 1 1 calc R . . C30 C 0.5402(4) 0.6317(3) 0.4447(2) 0.0948(18) Uani 1 1 d . . . H30A H 0.4881 0.6575 0.4602 0.142 Uiso 1 1 calc R . . H30B H 0.5930 0.6300 0.4726 0.142 Uiso 1 1 calc R . . H30C H 0.5183 0.5866 0.4363 0.142 Uiso 1 1 calc R . . C31 C 0.6552(3) 0.6249(3) 0.3657(2) 0.0893(17) Uani 1 1 d . . . H31A H 0.6763 0.6462 0.3308 0.134 Uiso 1 1 calc R . . H31B H 0.6340 0.5797 0.3571 0.134 Uiso 1 1 calc R . . H31C H 0.7079 0.6235 0.3937 0.134 Uiso 1 1 calc R . . C32 C 0.3553(2) 0.67943(16) 0.13926(14) 0.0387(7) Uani 1 1 d . . . C33 C 0.3289(3) 0.64655(19) 0.03781(14) 0.0492(9) Uani 1 1 d . . . C34 C 0.3432(3) 0.7157(2) 0.01450(17) 0.0703(12) Uani 1 1 d . . . H34A H 0.3969 0.7367 0.0346 0.105 Uiso 1 1 calc R . . H34B H 0.2858 0.7420 0.0200 0.105 Uiso 1 1 calc R . . H34C H 0.3560 0.7131 -0.0262 0.105 Uiso 1 1 calc R . . C35 C 0.2447(3) 0.6143(2) 0.00631(16) 0.0634(11) Uani 1 1 d . . . H35A H 0.2353 0.5694 0.0209 0.095 Uiso 1 1 calc R . . H35B H 0.2573 0.6123 -0.0344 0.095 Uiso 1 1 calc R . . H35C H 0.1874 0.6407 0.0122 0.095 Uiso 1 1 calc R . . C36 C 0.4175(3) 0.6048(2) 0.03196(18) 0.0674(12) Uani 1 1 d . . . H36A H 0.4062 0.5604 0.0472 0.101 Uiso 1 1 calc R . . H36B H 0.4702 0.6255 0.0532 0.101 Uiso 1 1 calc R . . H36C H 0.4332 0.6015 -0.0083 0.101 Uiso 1 1 calc R . . C37 C 0.0515(3) 0.6865(3) 0.3207(2) 0.0855(16) Uani 1 1 d D . . H37A H 0.0844 0.7207 0.3440 0.103 Uiso 1 1 calc R A 1 H37B H 0.0528 0.6438 0.3414 0.103 Uiso 1 1 calc R A 1 C38 C -0.0577(5) 0.7089(5) 0.3028(4) 0.089(3) Uani 0.60 1 d PDU B 1 H38A H -0.0614 0.7459 0.2746 0.107 Uiso 0.60 1 calc PR B 1 C39 C -0.1017(8) 0.7249(6) 0.3592(4) 0.145(4) Uani 0.70 1 d PDU B 1 H39A H -0.1666 0.7409 0.3525 0.217 Uiso 0.70 1 calc PR B 1 H39B H -0.0642 0.7592 0.3788 0.217 Uiso 0.70 1 calc PR B 1 H39C H -0.1029 0.6849 0.3828 0.217 Uiso 0.70 1 calc PR B 1 C40 C -0.0983(8) 0.6430(5) 0.2803(5) 0.111(3) Uani 0.60 1 d PDU B 1 H40A H -0.1643 0.6495 0.2674 0.167 Uiso 0.60 1 calc PR B 1 H40B H -0.0959 0.6099 0.3108 0.167 Uiso 0.60 1 calc PR B 1 H40C H -0.0607 0.6276 0.2485 0.167 Uiso 0.60 1 calc PR B 1 C38' C -0.0513(6) 0.6750(4) 0.3218(4) 0.042(2) Uani 0.40 1 d PDU B 2 H38B H -0.0878 0.7129 0.3048 0.051 Uiso 0.40 1 calc PR B 2 C39' C -0.071(3) 0.667(2) 0.3847(7) 0.225(16) Uani 0.30 1 d PDU B 2 H39D H -0.0495 0.7064 0.4054 0.337 Uiso 0.30 1 calc PR B 2 H39E H -0.0362 0.6280 0.3996 0.337 Uiso 0.30 1 calc PR B 2 H39F H -0.1388 0.6604 0.3898 0.337 Uiso 0.30 1 calc PR B 2 C40' C -0.0856(8) 0.6085(5) 0.2976(5) 0.071(3) Uani 0.40 1 d PDU B 2 H40D H -0.0775 0.6080 0.2563 0.107 Uiso 0.40 1 calc PR B 2 H40E H -0.1527 0.6024 0.3058 0.107 Uiso 0.40 1 calc PR B 2 H40F H -0.0484 0.5725 0.3151 0.107 Uiso 0.40 1 calc PR B 2 C41 C 0.2102(2) 0.51177(16) 0.31561(13) 0.0414(8) Uani 1 1 d . . . C42 C 0.3071(2) 0.51229(16) 0.30863(14) 0.0411(8) Uani 1 1 d . . . H42A H 0.3491 0.5116 0.3409 0.049 Uiso 1 1 calc R . . C43 C 0.3427(2) 0.51383(15) 0.25413(14) 0.0372(7) Uani 1 1 d . . . C44 C 0.2821(2) 0.51662(14) 0.20717(13) 0.0333(7) Uani 1 1 d . . . H44A H 0.3069 0.5182 0.1700 0.040 Uiso 1 1 calc R . . C45 C 0.1841(2) 0.51706(14) 0.21445(13) 0.0334(7) Uani 1 1 d . . . C46 C 0.1484(2) 0.51388(15) 0.26874(13) 0.0380(7) Uani 1 1 d . . . H46A H 0.0819 0.5131 0.2738 0.046 Uiso 1 1 calc R . . C47 C 0.1221(2) 0.52372(15) 0.16197(13) 0.0354(7) Uani 1 1 d . . . C48 C -0.0342(2) 0.49790(18) 0.11543(14) 0.0440(8) Uani 1 1 d . . . C49 C -0.0519(3) 0.5676(2) 0.09422(18) 0.0633(11) Uani 1 1 d . . . H49A H -0.0752 0.5949 0.1253 0.095 Uiso 1 1 calc R . . H49B H -0.0994 0.5667 0.0631 0.095 Uiso 1 1 calc R . . H49C H 0.0073 0.5864 0.0805 0.095 Uiso 1 1 calc R . . C50 C -0.1263(2) 0.4696(3) 0.13834(17) 0.0695(13) Uani 1 1 d . . . H50A H -0.1495 0.4986 0.1683 0.104 Uiso 1 1 calc R . . H50B H -0.1143 0.4253 0.1540 0.104 Uiso 1 1 calc R . . H50C H -0.1740 0.4667 0.1074 0.104 Uiso 1 1 calc R . . C51 C 0.0016(3) 0.4531(2) 0.06874(16) 0.0602(10) Uani 1 1 d . . . H51A H 0.0604 0.4714 0.0539 0.090 Uiso 1 1 calc R . . H51B H -0.0463 0.4503 0.0379 0.090 Uiso 1 1 calc R . . H51C H 0.0139 0.4088 0.0842 0.090 Uiso 1 1 calc R . . C52 C 0.4484(2) 0.51432(16) 0.24837(14) 0.0404(8) Uani 1 1 d . . . C53 C 0.5827(2) 0.48586(19) 0.18580(16) 0.0508(9) Uani 1 1 d . . . C54 C 0.5846(3) 0.4543(3) 0.12741(19) 0.0793(14) Uani 1 1 d . . . H54A H 0.5479 0.4816 0.1003 0.119 Uiso 1 1 calc R . . H54B H 0.5568 0.4099 0.1290 0.119 Uiso 1 1 calc R . . H54C H 0.6503 0.4512 0.1152 0.119 Uiso 1 1 calc R . . C55 C 0.6200(3) 0.5563(2) 0.1819(2) 0.0727(12) Uani 1 1 d . . . H55A H 0.5820 0.5810 0.1536 0.109 Uiso 1 1 calc R . . H55B H 0.6863 0.5554 0.1705 0.109 Uiso 1 1 calc R . . H55C H 0.6157 0.5779 0.2191 0.109 Uiso 1 1 calc R . . C56 C 0.6396(3) 0.4454(2) 0.2289(2) 0.0690(12) Uani 1 1 d . . . H56A H 0.6140 0.4004 0.2303 0.104 Uiso 1 1 calc R . . H56B H 0.6356 0.4660 0.2665 0.104 Uiso 1 1 calc R . . H56C H 0.7061 0.4438 0.2178 0.104 Uiso 1 1 calc R . . C57 C 0.2268(4) 0.5039(3) 0.41685(17) 0.0832(15) Uani 1 1 d . . . H57A H 0.2695 0.5427 0.4199 0.100 Uiso 1 1 calc R . . H57B H 0.2662 0.4635 0.4148 0.100 Uiso 1 1 calc R . . C58 C 0.1649(6) 0.5008(5) 0.4678(2) 0.130(3) Uani 1 1 d . . . H58A H 0.1182 0.5380 0.4686 0.156 Uiso 1 1 calc R . . C59 C 0.2244(8) 0.4970(7) 0.5208(3) 0.251(7) Uani 1 1 d . . . H59A H 0.2583 0.5389 0.5265 0.376 Uiso 1 1 calc R . . H59B H 0.2702 0.4608 0.5176 0.376 Uiso 1 1 calc R . . H59C H 0.1838 0.4888 0.5532 0.376 Uiso 1 1 calc R . . C60 C 0.1158(9) 0.4315(7) 0.4654(4) 0.235(6) Uani 1 1 d . . . H60A H 0.0734 0.4270 0.4975 0.353 Uiso 1 1 calc R . . H60B H 0.1641 0.3966 0.4675 0.353 Uiso 1 1 calc R . . H60C H 0.0789 0.4273 0.4297 0.353 Uiso 1 1 calc R . . O1 O 0.52712(15) 0.89476(12) 0.26067(10) 0.0508(6) Uani 1 1 d . . . O2 O 0.12624(16) 0.88817(12) 0.36280(10) 0.0486(6) Uani 1 1 d . . . O3 O 0.16260(15) 0.83842(12) 0.15172(9) 0.0470(6) Uani 1 1 d . . . O4 O 0.39171(19) 0.72973(13) 0.38882(10) 0.0595(7) Uani 1 1 d . . . O5 O 0.43057(16) 0.70868(12) 0.13063(10) 0.0500(6) Uani 1 1 d . . . O6 O 0.09100(17) 0.68057(14) 0.26613(11) 0.0589(7) Uani 1 1 d . B . O7 O 0.15260(16) 0.55304(12) 0.11986(9) 0.0467(6) Uani 1 1 d . . . O8 O 0.49989(17) 0.53964(13) 0.28557(12) 0.0595(7) Uani 1 1 d . . . O9 O 0.16750(19) 0.50934(15) 0.36698(10) 0.0620(7) Uani 1 1 d . . . N1 N 0.25172(18) 0.83335(13) 0.40208(11) 0.0384(6) Uani 1 1 d . . . H1A H 0.3057 0.8135 0.3951 0.046 Uiso 1 1 calc R . . N2 N 0.52025(18) 0.81981(15) 0.18907(12) 0.0477(7) Uani 1 1 d . . . H2B H 0.4830 0.7928 0.1694 0.057 Uiso 1 1 calc R . . N3 N 0.30312(19) 0.64947(13) 0.09830(11) 0.0410(6) Uani 1 1 d . . . H3A H 0.2500 0.6302 0.1081 0.049 Uiso 1 1 calc R . . N4 N 0.4960(2) 0.66132(15) 0.34688(12) 0.0497(8) Uani 1 1 d . . . H4B H 0.5050 0.6363 0.3169 0.060 Uiso 1 1 calc R . . N5 N 0.48149(18) 0.48695(14) 0.20131(12) 0.0458(7) Uani 1 1 d . . . H5A H 0.4402 0.4681 0.1777 0.055 Uiso 1 1 calc R . . N6 N 0.03489(17) 0.49787(13) 0.16381(11) 0.0379(6) Uani 1 1 d . . . H6B H 0.0175 0.4797 0.1959 0.045 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 C1 0.0403(17) 0.0313(17) 0.0358(18) -0.0032(13) 0.0006(13) -0.0024(13) C2 0.0347(16) 0.0304(16) 0.0412(18) 0.0001(13) 0.0065(13) 0.0014(12) C3 0.0369(16) 0.0266(15) 0.0341(17) 0.0027(12) 0.0074(13) 0.0030(12) C4 0.0358(16) 0.0274(16) 0.0355(17) -0.0004(13) 0.0045(13) -0.0003(12) C5 0.0353(16) 0.0264(15) 0.0377(17) -0.0062(13) 0.0081(13) -0.0025(12) C6 0.0416(17) 0.0305(16) 0.0360(17) -0.0043(13) 0.0088(13) -0.0025(13) C7 0.0364(16) 0.0405(18) 0.0408(18) -0.0102(15) 0.0055(14) -0.0033(14) C8 0.0375(18) 0.077(3) 0.057(2) -0.032(2) 0.0181(17) -0.0139(18) C9 0.053(2) 0.099(4) 0.076(3) -0.009(3) 0.025(2) -0.026(2) C10 0.053(3) 0.148(5) 0.114(4) -0.088(4) 0.041(3) -0.032(3) C11 0.044(2) 0.089(3) 0.096(4) -0.017(3) 0.011(2) 0.006(2) C12 0.0345(16) 0.0351(17) 0.0371(18) 0.0045(13) 0.0082(13) 0.0022(13) C13 0.0506(19) 0.049(2) 0.0319(18) 0.0007(15) 0.0087(14) 0.0061(16) C14 0.062(2) 0.070(3) 0.047(2) 0.0113(19) 0.0147(18) -0.001(2) C15 0.069(3) 0.072(3) 0.038(2) 0.0006(18) 0.0001(18) 0.018(2) C16 0.068(2) 0.061(3) 0.049(2) -0.0107(19) 0.0072(18) 0.012(2) C17 0.0411(19) 0.071(3) 0.045(2) -0.0060(18) 0.0027(15) -0.0002(17) C18 0.046(2) 0.090(3) 0.047(2) -0.001(2) -0.0030(17) -0.004(2) C19 0.049(3) 0.195(7) 0.080(4) -0.034(4) -0.009(2) 0.009(3) C20 0.081(3) 0.088(3) 0.062(3) -0.017(2) -0.008(2) -0.014(3) C21 0.0415(18) 0.0343(18) 0.047(2) -0.0076(14) 0.0077(15) 0.0010(14) C22 0.0415(17) 0.0296(17) 0.0422(19) -0.0045(13) -0.0005(14) -0.0009(13) C23 0.0426(17) 0.0288(16) 0.0349(17) -0.0024(13) 0.0021(13) -0.0046(13) C24 0.0411(17) 0.0300(16) 0.0395(18) -0.0036(13) 0.0036(14) 0.0000(13) C25 0.0469(18) 0.0284(16) 0.0385(18) -0.0063(13) 0.0030(14) 0.0051(13) C26 0.053(2) 0.0329(17) 0.0366(18) -0.0060(14) 0.0078(15) 0.0032(14) C27 0.055(2) 0.042(2) 0.0347(18) -0.0073(15) 0.0024(15) 0.0084(16) C28 0.061(2) 0.090(3) 0.042(2) -0.022(2) -0.0109(18) 0.017(2) C29 0.082(3) 0.113(4) 0.090(4) -0.041(3) -0.027(3) -0.006(3) C30 0.094(4) 0.136(5) 0.053(3) 0.002(3) -0.007(2) 0.044(3) C31 0.056(3) 0.139(5) 0.072(3) -0.040(3) -0.017(2) 0.031(3) C32 0.0436(18) 0.0344(17) 0.0380(18) -0.0029(14) 0.0001(14) -0.0068(14) C33 0.053(2) 0.060(2) 0.0344(19) -0.0006(16) 0.0023(15) -0.0177(17) C34 0.084(3) 0.083(3) 0.044(2) 0.018(2) -0.001(2) -0.031(2) C35 0.068(3) 0.085(3) 0.037(2) -0.006(2) 0.0001(18) -0.026(2) C36 0.063(2) 0.086(3) 0.053(2) -0.018(2) 0.0119(19) -0.008(2) C37 0.053(2) 0.124(4) 0.081(3) -0.045(3) 0.026(2) -0.009(3) C38 0.088(3) 0.094(3) 0.087(3) -0.0048(19) 0.0133(19) -0.0090(19) C39 0.142(4) 0.147(4) 0.146(4) -0.005(2) 0.007(2) 0.000(2) C40 0.108(4) 0.114(4) 0.112(4) -0.001(2) 0.007(2) -0.001(2) C38' 0.040(2) 0.045(3) 0.043(3) -0.0026(19) 0.0072(18) 0.0036(18) C39' 0.225(17) 0.225(17) 0.225(17) 0.000(2) 0.006(2) 0.000(2) C40' 0.068(3) 0.073(3) 0.074(3) 0.000(2) 0.006(2) 0.000(2) C41 0.0515(19) 0.0386(18) 0.0343(18) -0.0029(14) 0.0029(14) 0.0032(15) C42 0.0490(19) 0.0348(18) 0.0392(19) -0.0072(14) -0.0062(15) 0.0060(14) C43 0.0396(17) 0.0280(16) 0.0437(19) -0.0048(14) -0.0033(14) 0.0014(13) C44 0.0353(15) 0.0281(16) 0.0366(17) -0.0005(13) 0.0024(13) -0.0031(12) C45 0.0367(16) 0.0283(16) 0.0353(17) 0.0012(13) 0.0002(13) -0.0039(12) C46 0.0387(16) 0.0340(17) 0.0415(18) -0.0019(14) 0.0033(14) -0.0013(13) C47 0.0347(16) 0.0353(17) 0.0364(17) 0.0034(14) 0.0023(13) -0.0031(13) C48 0.0342(16) 0.059(2) 0.0382(18) 0.0110(16) -0.0023(13) -0.0057(15) C49 0.059(2) 0.069(3) 0.061(3) 0.018(2) -0.0122(19) 0.007(2) C50 0.0352(19) 0.116(4) 0.057(2) 0.023(2) -0.0056(17) -0.018(2) C51 0.059(2) 0.073(3) 0.049(2) 0.000(2) -0.0069(18) -0.010(2) C52 0.0371(16) 0.0343(18) 0.049(2) -0.0089(15) -0.0085(15) 0.0038(14) C53 0.0331(17) 0.060(2) 0.059(2) -0.0103(18) 0.0019(15) -0.0039(16) C54 0.045(2) 0.117(4) 0.077(3) -0.032(3) 0.017(2) -0.010(2) C55 0.053(2) 0.070(3) 0.096(3) 0.001(2) 0.007(2) -0.011(2) C56 0.048(2) 0.074(3) 0.086(3) 0.003(2) 0.005(2) 0.017(2) C57 0.094(3) 0.114(4) 0.041(2) -0.006(2) 0.002(2) 0.028(3) C58 0.142(6) 0.207(8) 0.041(3) 0.003(4) 0.003(3) 0.050(6) C59 0.281(13) 0.410(19) 0.062(5) 0.003(7) -0.010(6) 0.146(13) C60 0.258(14) 0.326(18) 0.127(8) 0.033(10) 0.089(8) -0.011(13) O1 0.0389(12) 0.0582(15) 0.0557(15) -0.0256(12) 0.0077(11) -0.0062(11) O2 0.0440(13) 0.0599(15) 0.0426(13) 0.0132(11) 0.0118(10) 0.0178(11) O3 0.0384(12) 0.0648(16) 0.0377(13) -0.0077(11) 0.0028(10) -0.0024(11) O4 0.0732(17) 0.0654(17) 0.0395(14) -0.0175(12) -0.0064(12) 0.0277(14) O5 0.0473(13) 0.0573(15) 0.0456(14) -0.0093(11) 0.0059(11) -0.0231(12) O6 0.0413(13) 0.0717(18) 0.0643(17) -0.0182(14) 0.0122(12) 0.0032(12) O7 0.0435(12) 0.0560(15) 0.0406(13) 0.0129(11) 0.0005(10) -0.0164(11) O8 0.0426(13) 0.0641(17) 0.0710(18) -0.0307(14) -0.0157(12) 0.0098(12) O9 0.0640(16) 0.089(2) 0.0331(14) -0.0030(13) 0.0048(12) 0.0079(14) N1 0.0371(14) 0.0419(15) 0.0363(15) 0.0018(12) 0.0048(11) 0.0079(11) N2 0.0344(14) 0.0591(19) 0.0502(18) -0.0253(14) 0.0125(12) -0.0124(13) N3 0.0417(15) 0.0476(16) 0.0336(15) -0.0008(12) 0.0026(11) -0.0141(12) N4 0.0514(17) 0.0608(19) 0.0368(16) -0.0184(14) -0.0034(13) 0.0121(14) N5 0.0325(14) 0.0545(18) 0.0503(17) -0.0115(14) -0.0016(12) -0.0035(12) N6 0.0319(13) 0.0477(16) 0.0340(14) 0.0097(12) 0.0011(11) -0.0041(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O3 1.361(4) . ? C1 C2 1.379(4) . ? C1 C6 1.395(4) . ? C2 C3 1.387(4) . ? C2 H2A 0.9500 . ? C3 C4 1.384(4) . ? C3 C12 1.498(4) . ? C4 C5 1.397(4) . ? C4 H4A 0.9500 . ? C5 C6 1.376(4) . ? C5 C7 1.498(4) . ? C6 H6A 0.9500 . ? C7 O1 1.232(4) . ? C7 N2 1.338(4) . ? C8 N2 1.478(4) . ? C8 C11 1.501(6) . ? C8 C9 1.517(6) . ? C8 C10 1.528(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 O2 1.240(4) . ? C12 N1 1.333(4) . ? C13 N1 1.481(4) . ? C13 C15 1.522(5) . ? C13 C14 1.523(5) . ? C13 C16 1.527(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O3 1.431(4) . ? C17 C18 1.497(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.514(6) . ? C18 C20 1.519(6) . ? C18 H18A 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 O6 1.366(4) . ? C21 C26 1.375(5) . ? C21 C22 1.393(5) . ? C22 C23 1.378(4) . ? C22 H22A 0.9500 . ? C23 C24 1.398(4) . ? C23 C32 1.499(4) . ? C24 C25 1.380(4) . ? C24 H24A 0.9500 . ? C25 C26 1.397(5) . ? C25 C27 1.494(5) . ? C26 H26A 0.9500 . ? C27 O4 1.233(4) 1 ? C27 O4 1.233(4) . ? C27 N4 1.335(4) . ? C28 N4 1.471(5) . ? C28 C29 1.522(7) . ? C28 C31 1.525(6) . ? C28 C30 1.531(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 O5 1.237(4) 1 ? C32 O5 1.237(4) . ? C32 N3 1.341(4) . ? C33 N3 1.479(4) . ? C33 C34 1.515(5) . ? C33 C36 1.517(6) . ? C33 C35 1.529(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 O6 1.417(5) . ? C37 C38' 1.470(9) . ? C37 C38 1.649(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.513(8) . ? C38 C40 1.537(8) . ? C38 H38A 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C38' C39' 1.522(10) . ? C38' C40' 1.531(9) . ? C38' H38B 1.0000 . ? C39' H39D 0.9800 . ? C39' H39E 0.9800 . ? C39' H39F 0.9800 . ? C40' H40D 0.9800 . ? C40' H40E 0.9800 . ? C40' H40F 0.9800 . ? C41 O9 1.365(4) . ? C41 C42 1.381(5) . ? C41 C46 1.388(4) . ? C42 C43 1.389(5) . ? C42 H42A 0.9500 . ? C43 C44 1.380(4) . ? C43 C52 1.501(4) . ? C44 C45 1.398(4) . ? C44 H44A 0.9500 . ? C45 C46 1.386(4) . ? C45 C47 1.500(4) . ? C46 H46A 0.9500 . ? C47 O7 1.241(4) 1 ? C47 O7 1.241(4) . ? C47 N6 1.338(4) . ? C48 N6 1.478(4) . ? C48 C49 1.513(5) . ? C48 C51 1.519(5) . ? C48 C50 1.531(5) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O8 1.233(4) 1 ? C52 O8 1.233(4) . ? C52 N5 1.333(4) . ? C53 N5 1.484(4) . ? C53 C54 1.515(5) . ? C53 C56 1.516(5) . ? C53 C55 1.520(6) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 O9 1.427(5) . ? C57 C58 1.502(8) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.486(10) . ? C58 C60 1.563(13) . ? C58 H58A 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O4 O4 0.000(7) 1 ? O5 O5 0.000(5) 1 ? O7 O7 0.000(6) 1 ? O8 O8 0.000(7) 1 ? N1 H1A 0.8800 . ? N2 H2B 0.8800 . ? N3 H3A 0.8800 . ? N4 H4B 0.8800 . ? N5 H5A 0.8800 . ? N6 H6B 0.8800 . ? 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 O3 C1 C2 124.7(3) . . ? O3 C1 C6 115.4(3) . . ? C2 C1 C6 119.9(3) . . ? C1 C2 C3 120.2(3) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 C12 122.7(3) . . ? C2 C3 C12 117.1(3) . . ? C3 C4 C5 119.7(3) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C6 C5 C4 120.0(3) . . ? C6 C5 C7 121.6(3) . . ? C4 C5 C7 118.3(3) . . ? C5 C6 C1 120.1(3) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? O1 C7 N2 123.6(3) . . ? O1 C7 C5 119.4(3) . . ? N2 C7 C5 117.0(3) . . ? N2 C8 C11 110.0(3) . . ? N2 C8 C9 109.9(3) . . ? C11 C8 C9 111.0(3) . . ? N2 C8 C10 105.7(3) . . ? C11 C8 C10 110.6(4) . . ? C9 C8 C10 109.5(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C12 N1 123.2(3) . . ? O2 C12 C3 119.8(3) . . ? N1 C12 C3 117.0(3) . . ? N1 C13 C15 106.0(3) . . ? N1 C13 C14 109.3(3) . . ? C15 C13 C14 110.0(3) . . ? N1 C13 C16 110.3(3) . . ? C15 C13 C16 109.6(3) . . ? C14 C13 C16 111.5(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C18 108.4(3) . . ? O3 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? O3 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? C17 C18 C19 109.1(3) . . ? C17 C18 C20 110.9(4) . . ? C19 C18 C20 111.6(4) . . ? C17 C18 H18A 108.4 . . ? C19 C18 H18A 108.4 . . ? C20 C18 H18A 108.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O6 C21 C26 125.0(3) . . ? O6 C21 C22 114.6(3) . . ? C26 C21 C22 120.4(3) . . ? C23 C22 C21 120.1(3) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C22 C23 C24 119.8(3) . . ? C22 C23 C32 122.0(3) . . ? C24 C23 C32 118.1(3) . . ? C25 C24 C23 119.9(3) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 120.2(3) . . ? C24 C25 C27 121.8(3) . . ? C26 C25 C27 117.8(3) . . ? C21 C26 C25 119.6(3) . . ? C21 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? O4 C27 O4 0.0(3) 1 . ? O4 C27 N4 123.5(3) 1 . ? O4 C27 N4 123.5(3) . . ? O4 C27 C25 120.7(3) 1 . ? O4 C27 C25 120.7(3) . . ? N4 C27 C25 115.7(3) . . ? N4 C28 C29 109.9(4) . . ? N4 C28 C31 106.1(3) . . ? C29 C28 C31 109.8(4) . . ? N4 C28 C30 108.9(4) . . ? C29 C28 C30 112.0(4) . . ? C31 C28 C30 109.9(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O5 C32 O5 0.0(3) 1 . ? O5 C32 N3 123.7(3) 1 . ? O5 C32 N3 123.7(3) . . ? O5 C32 C23 119.7(3) 1 . ? O5 C32 C23 119.7(3) . . ? N3 C32 C23 116.6(3) . . ? N3 C33 C34 110.5(3) . . ? N3 C33 C36 109.5(3) . . ? C34 C33 C36 111.2(3) . . ? N3 C33 C35 106.0(3) . . ? C34 C33 C35 109.0(3) . . ? C36 C33 C35 110.6(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O6 C37 C38' 114.5(5) . . ? O6 C37 C38 100.4(4) . . ? C38' C37 C38 29.8(4) . . ? O6 C37 H37A 111.7 . . ? C38' C37 H37A 123.3 . . ? C38 C37 H37A 111.7 . . ? O6 C37 H37B 111.7 . . ? C38' C37 H37B 81.9 . . ? C38 C37 H37B 111.7 . . ? H37A C37 H37B 109.5 . . ? C39 C38 C40 109.2(8) . . ? C39 C38 C37 103.8(7) . . ? C40 C38 C37 100.8(7) . . ? C39 C38 H38A 114.0 . . ? C40 C38 H38A 114.0 . . ? C37 C38 H38A 114.0 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C37 C38' C39' 103.7(17) . . ? C37 C38' C40' 115.7(7) . . ? C39' C38' C40' 101.7(17) . . ? C37 C38' H38B 111.7 . . ? C39' C38' H38B 111.7 . . ? C40' C38' H38B 111.7 . . ? C38' C39' H39D 109.5 . . ? C38' C39' H39E 109.5 . . ? H39D C39' H39E 109.5 . . ? C38' C39' H39F 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? C38' C40' H40D 109.5 . . ? C38' C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C38' C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? O9 C41 C42 124.5(3) . . ? O9 C41 C46 114.9(3) . . ? C42 C41 C46 120.5(3) . . ? C41 C42 C43 119.5(3) . . ? C41 C42 H42A 120.2 . . ? C43 C42 H42A 120.2 . . ? C44 C43 C42 120.5(3) . . ? C44 C43 C52 121.6(3) . . ? C42 C43 C52 117.9(3) . . ? C43 C44 C45 119.7(3) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C46 C45 C44 119.8(3) . . ? C46 C45 C47 123.0(3) . . ? C44 C45 C47 117.2(3) . . ? C45 C46 C41 119.8(3) . . ? C45 C46 H46A 120.1 . . ? C41 C46 H46A 120.1 . . ? O7 C47 O7 0.0(2) 1 . ? O7 C47 N6 123.4(3) 1 . ? O7 C47 N6 123.4(3) . . ? O7 C47 C45 119.5(3) 1 . ? O7 C47 C45 119.5(3) . . ? N6 C47 C45 117.1(3) . . ? N6 C48 C49 110.8(3) . . ? N6 C48 C51 109.4(3) . . ? C49 C48 C51 111.8(3) . . ? N6 C48 C50 106.1(3) . . ? C49 C48 C50 109.2(3) . . ? C51 C48 C50 109.5(3) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O8 C52 O8 0.0(3) 1 . ? O8 C52 N5 123.3(3) 1 . ? O8 C52 N5 123.3(3) . . ? O8 C52 C43 120.4(3) 1 . ? O8 C52 C43 120.4(3) . . ? N5 C52 C43 116.3(3) . . ? N5 C53 C54 105.6(3) . . ? N5 C53 C56 109.9(3) . . ? C54 C53 C56 111.0(4) . . ? N5 C53 C55 109.8(3) . . ? C54 C53 C55 108.9(4) . . ? C56 C53 C55 111.5(3) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O9 C57 C58 108.6(4) . . ? O9 C57 H57A 110.0 . . ? C58 C57 H57A 110.0 . . ? O9 C57 H57B 110.0 . . ? C58 C57 H57B 110.0 . . ? H57A C57 H57B 108.4 . . ? C59 C58 C57 110.2(7) . . ? C59 C58 C60 102.9(9) . . ? C57 C58 C60 106.0(6) . . ? C59 C58 H58A 112.4 . . ? C57 C58 H58A 112.4 . . ? C60 C58 H58A 112.4 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C1 O3 C17 117.4(2) . . ? O4 O4 C27 0(10) 1 . ? O5 O5 C32 0(10) 1 . ? C21 O6 C37 118.2(3) . . ? O7 O7 C47 0(10) 1 . ? O8 O8 C52 0(10) 1 . ? C41 O9 C57 117.9(3) . . ? C12 N1 C13 124.9(3) . . ? C12 N1 H1A 117.6 . . ? C13 N1 H1A 117.6 . . ? C7 N2 C8 124.0(3) . . ? C7 N2 H2B 118.0 . . ? C8 N2 H2B 118.0 . . ? C32 N3 C33 124.4(3) . . ? C32 N3 H3A 117.8 . . ? C33 N3 H3A 117.8 . . ? C27 N4 C28 125.9(3) . . ? C27 N4 H4B 117.0 . . ? C28 N4 H4B 117.0 . . ? C52 N5 C53 124.8(3) . . ? C52 N5 H5A 117.6 . . ? C53 N5 H5A 117.6 . . ? C47 N6 C48 124.2(3) . . ? C47 N6 H6B 117.9 . . ? C48 N6 H6B 117.9 . . ? 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 O3 C1 C2 C3 179.0(3) . . . . ? C6 C1 C2 C3 -1.7(4) . . . . ? C1 C2 C3 C4 1.8(4) . . . . ? C1 C2 C3 C12 178.9(3) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? C12 C3 C4 C5 -177.3(3) . . . . ? C3 C4 C5 C6 -1.1(4) . . . . ? C3 C4 C5 C7 174.2(3) . . . . ? C4 C5 C6 C1 1.2(4) . . . . ? C7 C5 C6 C1 -173.9(3) . . . . ? O3 C1 C6 C5 179.5(3) . . . . ? C2 C1 C6 C5 0.2(5) . . . . ? C6 C5 C7 O1 138.6(3) . . . . ? C4 C5 C7 O1 -36.7(4) . . . . ? C6 C5 C7 N2 -39.4(4) . . . . ? C4 C5 C7 N2 145.4(3) . . . . ? C4 C3 C12 O2 146.7(3) . . . . ? C2 C3 C12 O2 -30.3(4) . . . . ? C4 C3 C12 N1 -32.9(4) . . . . ? C2 C3 C12 N1 150.1(3) . . . . ? O3 C17 C18 C19 -172.4(4) . . . . ? O3 C17 C18 C20 64.3(4) . . . . ? O6 C21 C22 C23 179.0(3) . . . . ? C26 C21 C22 C23 0.2(5) . . . . ? C21 C22 C23 C24 0.4(5) . . . . ? C21 C22 C23 C32 -176.0(3) . . . . ? C22 C23 C24 C25 -0.3(5) . . . . ? C32 C23 C24 C25 176.2(3) . . . . ? C23 C24 C25 C26 -0.2(5) . . . . ? C23 C24 C25 C27 -175.2(3) . . . . ? O6 C21 C26 C25 -179.4(3) . . . . ? C22 C21 C26 C25 -0.7(5) . . . . ? C24 C25 C26 C21 0.8(5) . . . . ? C27 C25 C26 C21 175.9(3) . . . . ? C24 C25 C27 O4 139.4(4) . . . 1 ? C26 C25 C27 O4 -35.7(5) . . . 1 ? C24 C25 C27 O4 139.4(4) . . . . ? C26 C25 C27 O4 -35.7(5) . . . . ? C24 C25 C27 N4 -37.8(5) . . . . ? C26 C25 C27 N4 147.0(3) . . . . ? C22 C23 C32 O5 147.4(3) . . . 1 ? C24 C23 C32 O5 -29.0(4) . . . 1 ? C22 C23 C32 O5 147.4(3) . . . . ? C24 C23 C32 O5 -29.0(4) . . . . ? C22 C23 C32 N3 -30.9(4) . . . . ? C24 C23 C32 N3 152.7(3) . . . . ? O6 C37 C38 C39 -173.0(7) . . . . ? C38' C37 C38 C39 65.1(10) . . . . ? O6 C37 C38 C40 74.0(7) . . . . ? C38' C37 C38 C40 -47.9(9) . . . . ? O6 C37 C38' C39' 166.1(17) . . . . ? C38 C37 C38' C39' -127.4(19) . . . . ? O6 C37 C38' C40' 55.7(10) . . . . ? C38 C37 C38' C40' 122.2(13) . . . . ? O9 C41 C42 C43 179.0(3) . . . . ? C46 C41 C42 C43 -1.1(5) . . . . ? C41 C42 C43 C44 1.7(5) . . . . ? C41 C42 C43 C52 -180.0(3) . . . . ? C42 C43 C44 C45 -0.8(4) . . . . ? C52 C43 C44 C45 -179.0(3) . . . . ? C43 C44 C45 C46 -0.8(4) . . . . ? C43 C44 C45 C47 176.9(3) . . . . ? C44 C45 C46 C41 1.4(5) . . . . ? C47 C45 C46 C41 -176.1(3) . . . . ? O9 C41 C46 C45 179.4(3) . . . . ? C42 C41 C46 C45 -0.5(5) . . . . ? C46 C45 C47 O7 149.9(3) . . . 1 ? C44 C45 C47 O7 -27.7(4) . . . 1 ? C46 C45 C47 O7 149.9(3) . . . . ? C44 C45 C47 O7 -27.7(4) . . . . ? C46 C45 C47 N6 -29.2(4) . . . . ? C44 C45 C47 N6 153.2(3) . . . . ? C44 C43 C52 O8 148.5(3) . . . 1 ? C42 C43 C52 O8 -29.7(5) . . . 1 ? C44 C43 C52 O8 148.5(3) . . . . ? C42 C43 C52 O8 -29.7(5) . . . . ? C44 C43 C52 N5 -30.7(4) . . . . ? C42 C43 C52 N5 151.0(3) . . . . ? O9 C57 C58 C59 -178.5(8) . . . . ? O9 C57 C58 C60 70.8(8) . . . . ? C2 C1 O3 C17 -1.2(5) . . . . ? C6 C1 O3 C17 179.4(3) . . . . ? C18 C17 O3 C1 -174.5(3) . . . . ? N4 C27 O4 O4 0.0(3) . . . 1 ? C25 C27 O4 O4 0.00(18) . . . 1 ? N3 C32 O5 O5 0.00(6) . . . 1 ? C23 C32 O5 O5 0.00(10) . . . 1 ? C26 C21 O6 C37 1.5(5) . . . . ? C22 C21 O6 C37 -177.2(4) . . . . ? C38' C37 O6 C21 -170.2(5) . . . . ? C38 C37 O6 C21 162.2(4) . . . . ? N6 C47 O7 O7 0.00(3) . . . 1 ? C45 C47 O7 O7 0.00(16) . . . 1 ? N5 C52 O8 O8 0.00(19) . . . 1 ? C43 C52 O8 O8 0.00(6) . . . 1 ? C42 C41 O9 C57 -3.0(5) . . . . ? C46 C41 O9 C57 177.1(4) . . . . ? C58 C57 O9 C41 -178.9(5) . . . . ? O2 C12 N1 C13 -0.1(5) . . . . ? C3 C12 N1 C13 179.5(3) . . . . ? C15 C13 N1 C12 -175.8(3) . . . . ? C14 C13 N1 C12 65.7(4) . . . . ? C16 C13 N1 C12 -57.3(4) . . . . ? O1 C7 N2 C8 -0.4(6) . . . . ? C5 C7 N2 C8 177.5(3) . . . . ? C11 C8 N2 C7 64.7(5) . . . . ? C9 C8 N2 C7 -57.8(5) . . . . ? C10 C8 N2 C7 -175.9(4) . . . . ? O5 C32 N3 C33 0.8(5) 1 . . . ? O5 C32 N3 C33 0.8(5) . . . . ? C23 C32 N3 C33 179.0(3) . . . . ? C34 C33 N3 C32 -56.3(5) . . . . ? C36 C33 N3 C32 66.5(4) . . . . ? C35 C33 N3 C32 -174.2(3) . . . . ? O4 C27 N4 C28 0.2(6) 1 . . . ? O4 C27 N4 C28 0.2(6) . . . . ? C25 C27 N4 C28 177.4(4) . . . . ? C29 C28 N4 C27 -56.5(5) . . . . ? C31 C28 N4 C27 -175.2(4) . . . . ? C30 C28 N4 C27 66.6(5) . . . . ? O8 C52 N5 C53 -3.1(6) 1 . . . ? O8 C52 N5 C53 -3.1(6) . . . . ? C43 C52 N5 C53 176.2(3) . . . . ? C54 C53 N5 C52 -175.9(4) . . . . ? C56 C53 N5 C52 64.2(5) . . . . ? C55 C53 N5 C52 -58.7(5) . . . . ? O7 C47 N6 C48 3.2(5) 1 . . . ? O7 C47 N6 C48 3.2(5) . . . . ? C45 C47 N6 C48 -177.8(3) . . . . ? C49 C48 N6 C47 -56.3(4) . . . . ? C51 C48 N6 C47 67.3(4) . . . . ? C50 C48 N6 C47 -174.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O4 0.88 2.09 2.900(3) 152.8 1 N2 H2B O5 0.88 2.06 2.904(3) 161.4 1 N3 H3A O7 0.88 2.10 2.935(3) 157.8 1 N4 H4B O8 0.88 2.09 2.850(4) 144.6 1 N5 H5A O2 0.88 2.08 2.905(4) 154.8 2_545 N6 H6B O1 0.88 2.10 2.888(3) 148.4 2_545 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.063 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.053