# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Yu Liu' _publ_contact_author_address ; Department of Chemistry Nankai University Tianjin 300071 CHINA ; _publ_contact_author_email YULIU@NANKAI.EDU.CN _publ_section_title ; Unique conformation and packing structure of p-sulfonatocalix[5]arene induced by 1,2-bis(pyridinium)ethane compounds ; loop_ _publ_author_name 'Yu Liu' 'Dong-Sheng Guo' 'Chun-Ju Li' 'Heng-Yi Zhang' data_051101b _database_code_depnum_ccdc_archive 'CCDC 600932' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H72.50 N4 O32.25 S5' _chemical_formula_weight 1489.99 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4122(13) _cell_length_b 15.3616(15) _cell_length_c 19.3740(18) _cell_angle_alpha 68.031(2) _cell_angle_beta 85.944(2) _cell_angle_gamma 65.8540(10) _cell_volume 3361.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 6032 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 26.33 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1561 _exptl_absorpt_coefficient_mu 0.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.763682 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17187 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.01 _reflns_number_total 11749 _reflns_number_gt 8017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1399P)^2^+6.8888P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11749 _refine_ls_number_parameters 933 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.2545 _refine_ls_wR_factor_gt 0.2122 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.004 _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 S1 S 0.40356(13) 0.78148(14) 1.00337(10) 0.0636(5) Uani 1 1 d . . . S2 S 1.11785(11) 0.37495(10) 0.85248(7) 0.0414(3) Uani 1 1 d . . . S3 S 1.16391(10) 0.84571(11) 0.62372(7) 0.0408(3) Uani 1 1 d . . . S4 S 0.69764(10) 0.88889(10) 0.36842(7) 0.0393(3) Uani 1 1 d . . . S5 S 0.67265(15) 0.44292(13) 0.62859(10) 0.0617(5) Uani 1 1 d . . . O1 O 0.6926(3) 0.4441(3) 0.90953(19) 0.0392(8) Uani 1 1 d . . . H1 H 0.7299 0.3942 0.9462 0.059 Uiso 1 1 calc R . . O2 O 0.3022(3) 0.8361(3) 0.9562(3) 0.0656(12) Uani 1 1 d . . . O3 O 0.3850(6) 0.7291(6) 1.0794(3) 0.155(3) Uani 1 1 d U . . O4 O 0.4596(6) 0.8422(6) 0.9988(6) 0.152(3) Uani 1 1 d U . . O5 O 0.7952(3) 0.6936(3) 0.9512(2) 0.0450(9) Uani 1 1 d . . . H5 H 0.7946 0.6706 0.9968 0.068 Uiso 1 1 calc R . . O6 O 1.2160(3) 0.3374(3) 0.9011(2) 0.0559(11) Uani 1 1 d . . . O7 O 1.1319(3) 0.4276(3) 0.7751(2) 0.0582(11) Uani 1 1 d . . . O8 O 1.0797(4) 0.2965(3) 0.8612(3) 0.0671(12) Uani 1 1 d . . . O9 O 0.7537(3) 0.8547(3) 0.75960(18) 0.0407(8) Uani 1 1 d . . . H9 H 0.7024 0.8755 0.7285 0.061 Uiso 1 1 calc R . . O10 O 1.2339(4) 0.7374(4) 0.6400(3) 0.0716(13) Uani 1 1 d . . . O11 O 1.1364(4) 0.9030(5) 0.5444(2) 0.0873(18) Uani 1 1 d . . . O12 O 1.2088(3) 0.8887(3) 0.6607(3) 0.0618(11) Uani 1 1 d . . . O13 O 0.5818(3) 0.8992(3) 0.66588(18) 0.0414(8) Uani 1 1 d . . . H13 H 0.5167 0.9114 0.6705 0.062 Uiso 1 1 calc R . . O14 O 0.8124(3) 0.8662(3) 0.3645(2) 0.0525(10) Uani 1 1 d . . . O15 O 0.6296(3) 0.9941(3) 0.31719(19) 0.0519(10) Uani 1 1 d . . . O16 O 0.6676(4) 0.8140(4) 0.3582(2) 0.0674(12) Uani 1 1 d . . . O17 O 0.4062(3) 0.7564(3) 0.75057(19) 0.0441(9) Uani 1 1 d . . . H17 H 0.3490 0.7954 0.7232 0.066 Uiso 1 1 calc R . . O18 O 0.7510(4) 0.4761(4) 0.5835(3) 0.0819(15) Uani 1 1 d . . . O19 O 0.5938(5) 0.4454(6) 0.5813(5) 0.127(3) Uani 1 1 d . . . O20 O 0.7261(6) 0.3459(4) 0.6896(3) 0.106(2) Uani 1 1 d . . . C1 C 0.4687(4) 0.5516(4) 0.8462(3) 0.0398(11) Uani 1 1 d . . . H1A H 0.4892 0.4778 0.8664 0.048 Uiso 1 1 calc R . . H1B H 0.3893 0.5855 0.8424 0.048 Uiso 1 1 calc R . . C2 C 0.5152(4) 0.5777(4) 0.9014(3) 0.0343(11) Uani 1 1 d . . . C3 C 0.4473(4) 0.6570(4) 0.9237(3) 0.0389(11) Uani 1 1 d . . . H3 H 0.3738 0.6938 0.9049 0.047 Uiso 1 1 calc R . . C4 C 0.4891(4) 0.6815(4) 0.9742(3) 0.0388(11) Uani 1 1 d . . . C5 C 0.5984(4) 0.6274(4) 1.0028(3) 0.0377(11) Uani 1 1 d . . . H5A H 0.6250 0.6445 1.0366 0.045 Uiso 1 1 calc R . . C6 C 0.6687(4) 0.5480(4) 0.9815(3) 0.0341(11) Uani 1 1 d . . . C7 C 0.6242(4) 0.5234(3) 0.9317(2) 0.0322(10) Uani 1 1 d . . . C8 C 0.7887(4) 0.4916(4) 1.0119(3) 0.0368(11) Uani 1 1 d . . . H8A H 0.7976 0.5069 1.0547 0.044 Uiso 1 1 calc R . . H8B H 0.8091 0.4180 1.0293 0.044 Uiso 1 1 calc R . . C9 C 0.8667(4) 0.5185(4) 0.9560(3) 0.0326(10) Uani 1 1 d . . . C10 C 0.9433(4) 0.4450(4) 0.9314(3) 0.0352(11) Uani 1 1 d . . . H10 H 0.9468 0.3784 0.9499 0.042 Uiso 1 1 calc R . . C11 C 1.0148(4) 0.4695(4) 0.8797(3) 0.0338(10) Uani 1 1 d . . . C12 C 1.0102(4) 0.5687(4) 0.8524(2) 0.0327(10) Uani 1 1 d . . . H12 H 1.0563 0.5854 0.8167 0.039 Uiso 1 1 calc R . . C13 C 0.9383(4) 0.6431(4) 0.8775(2) 0.0306(10) Uani 1 1 d . . . C14 C 0.8670(4) 0.6170(4) 0.9292(2) 0.0310(10) Uani 1 1 d . . . C15 C 0.9429(4) 0.7470(4) 0.8538(2) 0.0336(10) Uani 1 1 d . . . H15A H 1.0081 0.7380 0.8793 0.040 Uiso 1 1 calc R . . H15B H 0.8797 0.7919 0.8700 0.040 Uiso 1 1 calc R . . C16 C 0.9445(4) 0.7996(3) 0.7701(2) 0.0303(10) Uani 1 1 d . . . C17 C 1.0411(4) 0.7971(4) 0.7383(3) 0.0322(10) Uani 1 1 d . . . H17A H 1.1075 0.7600 0.7682 0.039 Uiso 1 1 calc R . . C18 C 1.0392(4) 0.8495(4) 0.6623(3) 0.0306(10) Uani 1 1 d . . . C19 C 0.9403(4) 0.9055(3) 0.6174(3) 0.0302(10) Uani 1 1 d . . . H19 H 0.9398 0.9404 0.5664 0.036 Uiso 1 1 calc R . . C20 C 0.8417(4) 0.9103(3) 0.6478(2) 0.0281(9) Uani 1 1 d . . . C21 C 0.8454(4) 0.8553(3) 0.7241(2) 0.0286(9) Uani 1 1 d . . . C22 C 0.7341(4) 0.9800(4) 0.5979(3) 0.0326(10) Uani 1 1 d . . . H22A H 0.6797 1.0112 0.6271 0.039 Uiso 1 1 calc R . . H22B H 0.7452 1.0353 0.5577 0.039 Uiso 1 1 calc R . . C23 C 0.6870(3) 0.9292(3) 0.5633(2) 0.0289(10) Uani 1 1 d . . . C24 C 0.7177(4) 0.9226(4) 0.4947(3) 0.0326(10) Uani 1 1 d . . . H24 H 0.7728 0.9424 0.4725 0.039 Uiso 1 1 calc R . . C25 C 0.6661(4) 0.8863(4) 0.4594(3) 0.0339(10) Uani 1 1 d . . . C26 C 0.5835(4) 0.8565(4) 0.4919(3) 0.0337(10) Uani 1 1 d . . . H26 H 0.5486 0.8339 0.4669 0.040 Uiso 1 1 calc R . . C27 C 0.5525(4) 0.8601(3) 0.5611(2) 0.0317(10) Uani 1 1 d . . . C28 C 0.6054(3) 0.8962(3) 0.5958(2) 0.0292(10) Uani 1 1 d . . . C29 C 0.4621(4) 0.8274(4) 0.5964(3) 0.0339(10) Uani 1 1 d . . . H29A H 0.4218 0.8700 0.6241 0.041 Uiso 1 1 calc R . . H29B H 0.4112 0.8403 0.5569 0.041 Uiso 1 1 calc R . . C30 C 0.5024(4) 0.7154(4) 0.6485(3) 0.0312(10) Uani 1 1 d . . . C31 C 0.5664(4) 0.6392(4) 0.6231(3) 0.0370(11) Uani 1 1 d . . . H31 H 0.5881 0.6575 0.5750 0.044 Uiso 1 1 calc R . . C32 C 0.5991(4) 0.5362(4) 0.6676(3) 0.0401(12) Uani 1 1 d . . . C33 C 0.5681(4) 0.5081(4) 0.7402(3) 0.0388(11) Uani 1 1 d . . . H33 H 0.5900 0.4386 0.7701 0.047 Uiso 1 1 calc R . . C34 C 0.5055(4) 0.5818(4) 0.7684(2) 0.0311(10) Uani 1 1 d . . . C35 C 0.4707(4) 0.6857(3) 0.7213(2) 0.0304(10) Uani 1 1 d . . . N1 N -0.2130(4) 0.5171(4) 0.7845(3) 0.0519(12) Uani 1 1 d . . . H1C H -0.2435 0.4941 0.8236 0.062 Uiso 1 1 calc R . . N2 N 0.0248(4) 0.7133(3) 0.4694(2) 0.0387(10) Uani 1 1 d . . . N3 N 0.0854(4) 0.9111(3) 0.3096(3) 0.0443(11) Uani 1 1 d . . . N4 N 0.2911(7) 1.0833(5) -0.0292(4) 0.090(2) Uani 1 1 d . . . H4 H 0.3145 1.1065 -0.0717 0.108 Uiso 1 1 calc R . . C36 C -0.2328(5) 0.6157(5) 0.7575(3) 0.0528(14) Uani 1 1 d . . . H36 H -0.2793 0.6589 0.7802 0.063 Uiso 1 1 calc R . . C37 C -0.1844(4) 0.6545(4) 0.6956(3) 0.0442(12) Uani 1 1 d . . . H37 H -0.1967 0.7237 0.6765 0.053 Uiso 1 1 calc R . . C38 C -0.1162(4) 0.5880(4) 0.6619(3) 0.0366(11) Uani 1 1 d . . . C39 C -0.0986(5) 0.4852(4) 0.6915(3) 0.0479(13) Uani 1 1 d . . . H39 H -0.0543 0.4401 0.6695 0.057 Uiso 1 1 calc R . . C40 C -0.1482(5) 0.4514(5) 0.7543(3) 0.0550(15) Uani 1 1 d . . . H40 H -0.1364 0.3823 0.7758 0.066 Uiso 1 1 calc R . . C41 C -0.0654(4) 0.6296(4) 0.5942(3) 0.0361(11) Uani 1 1 d . . . C42 C 0.0004(5) 0.6788(5) 0.5970(3) 0.0512(14) Uani 1 1 d . . . H42 H 0.0137 0.6843 0.6414 0.061 Uiso 1 1 calc R . . C43 C 0.0460(5) 0.7194(5) 0.5333(3) 0.0526(14) Uani 1 1 d . . . H43 H 0.0915 0.7510 0.5351 0.063 Uiso 1 1 calc R . . C44 C -0.0359(4) 0.6652(4) 0.4654(3) 0.0422(12) Uani 1 1 d . . . H44 H -0.0475 0.6604 0.4204 0.051 Uiso 1 1 calc R . . C45 C -0.0820(5) 0.6222(4) 0.5276(3) 0.0440(12) Uani 1 1 d . . . H45 H -0.1243 0.5882 0.5245 0.053 Uiso 1 1 calc R . . C46 C 0.0743(5) 0.7581(4) 0.4008(3) 0.0484(14) Uani 1 1 d . . . H46A H 0.0497 0.7490 0.3591 0.058 Uiso 1 1 calc R . . H46B H 0.1536 0.7218 0.4090 0.058 Uiso 1 1 calc R . . C47 C 0.0418(5) 0.8717(4) 0.3817(3) 0.0495(14) Uani 1 1 d . . . H47A H -0.0374 0.9082 0.3772 0.059 Uiso 1 1 calc R . . H47B H 0.0727 0.8815 0.4206 0.059 Uiso 1 1 calc R . . C48 C 0.1937(5) 0.8889(4) 0.3087(3) 0.0476(13) Uani 1 1 d . . . H48 H 0.2394 0.8512 0.3532 0.057 Uiso 1 1 calc R . . C49 C 0.2366(5) 0.9216(4) 0.2425(3) 0.0489(13) Uani 1 1 d . . . H49 H 0.3113 0.9060 0.2420 0.059 Uiso 1 1 calc R . . C50 C 0.1678(5) 0.9784(4) 0.1757(3) 0.0471(13) Uani 1 1 d . . . C51 C 0.0574(5) 1.0009(4) 0.1792(3) 0.0542(15) Uani 1 1 d . . . H51 H 0.0097 1.0395 0.1357 0.065 Uiso 1 1 calc R . . C52 C 0.0175(5) 0.9668(5) 0.2465(4) 0.0543(15) Uani 1 1 d . . . H52 H -0.0571 0.9824 0.2483 0.065 Uiso 1 1 calc R . . C53 C 0.2131(5) 1.0149(4) 0.1028(3) 0.0532(15) Uani 1 1 d . . . C54 C 0.2976(6) 1.0444(6) 0.0992(4) 0.0699(19) Uani 1 1 d . . . H54 H 0.3285 1.0404 0.1424 0.084 Uiso 1 1 calc R . . C55 C 0.3371(8) 1.0803(6) 0.0307(5) 0.086(3) Uani 1 1 d . . . H55 H 0.3937 1.1015 0.0269 0.103 Uiso 1 1 calc R . . C56 C 0.2117(9) 1.0530(6) -0.0276(4) 0.089(3) Uani 1 1 d . . . H56 H 0.1840 1.0551 -0.0711 0.107 Uiso 1 1 calc R . . C57 C 0.1712(7) 1.0186(5) 0.0383(4) 0.0705(19) Uani 1 1 d . . . H57 H 0.1150 0.9975 0.0401 0.085 Uiso 1 1 calc R . . O21 O 0.8282(5) 0.6265(4) 0.3523(3) 0.0851(15) Uani 1 1 d U . . O22 O 0.2266(5) 0.9843(5) 0.8086(3) 0.104(2) Uani 1 1 d U . . O23 O 0.0580(5) 0.2172(6) 0.7537(4) 0.117(2) Uani 1 1 d U . . O24 O 0.3044(6) 0.7362(6) 0.4834(4) 0.123(2) Uani 1 1 d U . . O25 O 0.8459(9) 0.2497(9) 0.0161(6) 0.184(4) Uani 1 1 d U . . O26 O 0.2136(8) 0.7611(6) 0.1617(5) 0.147(3) Uani 1 1 d U . . O27 O 0.7454(9) 0.4994(8) 0.4374(5) 0.168(3) Uani 1 1 d U . . O28 O 0.9611(8) 0.1674(8) 0.9239(7) 0.190(4) Uani 1 1 d U . . O29 O 0.3690(10) 0.1545(8) 0.8406(5) 0.194(4) Uani 1 1 d U . . O30 O 0.7133(12) 0.4788(13) 0.2534(9) 0.128(5) Uani 0.50 1 d PU . . O31 O 0.5399(12) 0.7019(12) 0.1967(8) 0.118(4) Uani 0.50 1 d PU . . O32 O 0.5660(12) 0.8151(12) 0.8276(7) 0.123(5) Uani 0.50 1 d PU . . O33 O 0.4882(11) 0.9482(13) 0.2344(8) 0.115(4) Uani 0.50 1 d PU . . O34 O 0.4832(15) 0.7744(18) 0.3228(12) 0.182(7) Uani 0.50 1 d PU . . O36 O 0.676(2) 0.4469(19) 0.3489(16) 0.110(8) Uani 0.25 1 d PU . . O37 O 0.6455(17) 0.5831(17) 0.2086(12) 0.077(5) Uani 0.25 1 d PU . . O38 O 0.5108(17) 1.0173(17) 0.1869(12) 0.076(5) Uani 0.25 1 d PU . . 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 S1 0.0477(9) 0.0662(10) 0.0657(10) -0.0414(9) -0.0013(7) 0.0029(8) S2 0.0372(7) 0.0461(7) 0.0435(7) -0.0248(6) 0.0086(5) -0.0132(6) S3 0.0277(6) 0.0513(8) 0.0374(7) -0.0088(6) 0.0056(5) -0.0183(6) S4 0.0383(7) 0.0433(7) 0.0310(6) -0.0149(5) 0.0063(5) -0.0118(6) S5 0.0721(11) 0.0507(9) 0.0640(10) -0.0361(8) 0.0179(8) -0.0159(8) O1 0.0375(19) 0.0364(19) 0.0360(18) -0.0124(15) 0.0076(15) -0.0099(15) O2 0.053(3) 0.057(3) 0.064(3) -0.022(2) 0.000(2) 0.000(2) O3 0.143(5) 0.150(5) 0.055(3) -0.038(3) 0.025(3) 0.044(4) O4 0.092(4) 0.135(5) 0.288(8) -0.158(6) 0.003(5) -0.030(4) O5 0.049(2) 0.0371(19) 0.039(2) -0.0126(16) 0.0155(17) -0.0119(17) O6 0.036(2) 0.064(3) 0.055(2) -0.032(2) 0.0005(17) 0.0006(18) O7 0.060(3) 0.071(3) 0.041(2) -0.029(2) 0.0177(19) -0.020(2) O8 0.066(3) 0.061(3) 0.094(3) -0.049(3) 0.025(2) -0.030(2) O9 0.0294(17) 0.057(2) 0.0305(18) -0.0113(16) 0.0058(14) -0.0185(17) O10 0.048(2) 0.067(3) 0.095(4) -0.039(3) 0.024(2) -0.014(2) O11 0.045(2) 0.141(5) 0.038(2) 0.008(3) 0.0070(19) -0.042(3) O12 0.038(2) 0.069(3) 0.090(3) -0.034(2) 0.009(2) -0.030(2) O13 0.0303(18) 0.064(2) 0.0296(18) -0.0179(16) 0.0072(14) -0.0196(18) O14 0.037(2) 0.065(3) 0.041(2) -0.0204(19) 0.0096(16) -0.0086(18) O15 0.044(2) 0.057(2) 0.0302(19) -0.0087(17) 0.0037(16) -0.0043(18) O16 0.092(3) 0.081(3) 0.056(3) -0.040(2) 0.026(2) -0.051(3) O17 0.046(2) 0.038(2) 0.0313(18) -0.0137(16) 0.0011(15) -0.0014(16) O18 0.095(4) 0.079(3) 0.077(3) -0.046(3) 0.051(3) -0.032(3) O19 0.102(5) 0.163(7) 0.179(7) -0.141(6) 0.020(5) -0.046(5) O20 0.152(6) 0.041(3) 0.087(4) -0.026(3) 0.052(4) -0.011(3) C1 0.040(3) 0.041(3) 0.035(3) -0.009(2) 0.006(2) -0.019(2) C2 0.035(3) 0.035(3) 0.025(2) -0.0022(19) 0.0051(19) -0.016(2) C3 0.030(2) 0.039(3) 0.035(3) -0.008(2) 0.002(2) -0.007(2) C4 0.035(3) 0.040(3) 0.033(3) -0.012(2) 0.008(2) -0.010(2) C5 0.038(3) 0.044(3) 0.029(2) -0.011(2) 0.007(2) -0.018(2) C6 0.033(2) 0.036(3) 0.028(2) -0.006(2) 0.0086(19) -0.015(2) C7 0.035(2) 0.030(2) 0.028(2) -0.0053(19) 0.0118(19) -0.016(2) C8 0.036(3) 0.037(3) 0.029(2) -0.004(2) 0.005(2) -0.014(2) C9 0.026(2) 0.038(3) 0.027(2) -0.008(2) 0.0012(18) -0.010(2) C10 0.033(2) 0.035(3) 0.034(3) -0.008(2) -0.001(2) -0.013(2) C11 0.029(2) 0.036(3) 0.032(2) -0.013(2) 0.0026(19) -0.009(2) C12 0.029(2) 0.043(3) 0.025(2) -0.009(2) 0.0034(18) -0.016(2) C13 0.028(2) 0.037(3) 0.022(2) -0.0073(19) -0.0007(17) -0.011(2) C14 0.025(2) 0.033(2) 0.027(2) -0.0086(19) 0.0007(18) -0.0071(19) C15 0.038(3) 0.038(3) 0.025(2) -0.008(2) 0.0008(19) -0.019(2) C16 0.033(2) 0.030(2) 0.026(2) -0.0088(19) 0.0018(19) -0.014(2) C17 0.029(2) 0.036(3) 0.030(2) -0.007(2) -0.0003(19) -0.016(2) C18 0.027(2) 0.035(2) 0.030(2) -0.010(2) 0.0031(18) -0.015(2) C19 0.032(2) 0.029(2) 0.027(2) -0.0066(19) 0.0037(18) -0.014(2) C20 0.027(2) 0.027(2) 0.029(2) -0.0089(19) 0.0013(18) -0.0120(19) C21 0.029(2) 0.033(2) 0.027(2) -0.0113(19) 0.0064(18) -0.0160(19) C22 0.030(2) 0.031(2) 0.030(2) -0.006(2) 0.0012(19) -0.011(2) C23 0.023(2) 0.028(2) 0.027(2) -0.0042(18) -0.0030(17) -0.0070(18) C24 0.025(2) 0.035(2) 0.030(2) -0.006(2) 0.0045(18) -0.011(2) C25 0.030(2) 0.034(2) 0.030(2) -0.010(2) 0.0014(19) -0.007(2) C26 0.033(2) 0.031(2) 0.032(2) -0.007(2) -0.001(2) -0.013(2) C27 0.026(2) 0.030(2) 0.027(2) -0.0020(19) -0.0002(18) -0.0081(19) C28 0.024(2) 0.030(2) 0.022(2) -0.0038(18) 0.0012(17) -0.0059(18) C29 0.026(2) 0.035(3) 0.035(3) -0.006(2) 0.0022(19) -0.014(2) C30 0.025(2) 0.033(2) 0.031(2) -0.007(2) 0.0010(18) -0.0111(19) C31 0.038(3) 0.040(3) 0.030(2) -0.012(2) 0.007(2) -0.015(2) C32 0.042(3) 0.038(3) 0.040(3) -0.020(2) 0.008(2) -0.012(2) C33 0.042(3) 0.032(3) 0.040(3) -0.011(2) 0.002(2) -0.014(2) C34 0.028(2) 0.034(2) 0.029(2) -0.008(2) 0.0021(18) -0.013(2) C35 0.026(2) 0.032(2) 0.030(2) -0.011(2) 0.0025(18) -0.0093(19) N1 0.046(3) 0.073(4) 0.038(3) -0.015(2) 0.009(2) -0.032(3) N2 0.045(2) 0.039(2) 0.036(2) -0.0178(19) 0.0128(18) -0.019(2) N3 0.050(3) 0.038(2) 0.047(3) -0.018(2) 0.015(2) -0.020(2) N4 0.131(6) 0.052(4) 0.059(4) -0.021(3) 0.042(4) -0.017(4) C36 0.041(3) 0.067(4) 0.050(3) -0.028(3) 0.008(3) -0.017(3) C37 0.042(3) 0.050(3) 0.040(3) -0.020(2) 0.004(2) -0.017(3) C38 0.035(3) 0.040(3) 0.035(3) -0.012(2) 0.001(2) -0.016(2) C39 0.050(3) 0.043(3) 0.052(3) -0.020(3) 0.011(3) -0.019(3) C40 0.059(4) 0.054(4) 0.050(3) -0.011(3) 0.009(3) -0.030(3) C41 0.038(3) 0.034(3) 0.036(3) -0.014(2) 0.002(2) -0.014(2) C42 0.064(4) 0.062(4) 0.040(3) -0.024(3) 0.007(3) -0.035(3) C43 0.064(4) 0.066(4) 0.048(3) -0.027(3) 0.017(3) -0.043(3) C44 0.054(3) 0.038(3) 0.040(3) -0.019(2) 0.004(2) -0.020(3) C45 0.052(3) 0.047(3) 0.040(3) -0.017(2) 0.006(2) -0.026(3) C46 0.063(4) 0.039(3) 0.048(3) -0.020(3) 0.023(3) -0.025(3) C47 0.056(3) 0.045(3) 0.052(3) -0.022(3) 0.022(3) -0.025(3) C48 0.048(3) 0.050(3) 0.046(3) -0.020(3) 0.008(2) -0.021(3) C49 0.050(3) 0.051(3) 0.049(3) -0.020(3) 0.012(3) -0.023(3) C50 0.063(4) 0.035(3) 0.047(3) -0.020(2) 0.014(3) -0.021(3) C51 0.055(4) 0.044(3) 0.051(3) -0.010(3) -0.002(3) -0.015(3) C52 0.046(3) 0.050(3) 0.064(4) -0.019(3) 0.004(3) -0.020(3) C53 0.071(4) 0.037(3) 0.046(3) -0.016(3) 0.015(3) -0.018(3) C54 0.077(5) 0.071(5) 0.058(4) -0.024(3) 0.026(3) -0.031(4) C55 0.107(6) 0.067(5) 0.080(6) -0.029(4) 0.048(5) -0.038(5) C56 0.135(8) 0.067(5) 0.052(4) -0.021(4) 0.015(5) -0.032(5) C57 0.100(6) 0.055(4) 0.047(4) -0.014(3) 0.009(4) -0.029(4) O21 0.090(4) 0.098(4) 0.084(3) -0.056(3) 0.013(3) -0.036(3) O22 0.085(4) 0.115(4) 0.069(3) -0.018(3) 0.013(3) -0.018(3) O23 0.102(4) 0.127(5) 0.149(5) -0.098(4) 0.016(4) -0.031(4) O24 0.135(5) 0.148(6) 0.098(4) -0.062(4) 0.010(4) -0.056(4) O25 0.221(8) 0.208(8) 0.192(8) -0.077(6) 0.019(6) -0.151(7) O26 0.176(7) 0.124(5) 0.134(6) -0.054(4) 0.040(5) -0.054(5) O27 0.216(8) 0.172(7) 0.132(6) -0.060(5) 0.042(6) -0.096(6) O28 0.161(7) 0.169(7) 0.211(8) -0.038(6) 0.056(6) -0.078(6) O29 0.242(8) 0.163(7) 0.142(6) -0.056(5) 0.113(6) -0.066(6) O30 0.105(7) 0.145(9) 0.166(10) -0.050(7) 0.009(6) -0.091(7) O31 0.132(8) 0.157(9) 0.100(7) -0.056(6) -0.008(6) -0.082(7) O32 0.120(8) 0.150(9) 0.088(7) -0.004(6) 0.029(6) -0.086(7) O33 0.090(7) 0.150(9) 0.111(8) -0.075(7) -0.005(6) -0.030(6) O34 0.133(10) 0.204(12) 0.189(11) -0.055(8) -0.008(8) -0.066(8) O36 0.116(12) 0.093(11) 0.123(12) -0.029(8) -0.029(8) -0.049(9) O37 0.083(9) 0.093(9) 0.087(10) -0.033(7) 0.014(7) -0.070(8) O38 0.071(9) 0.089(10) 0.072(9) -0.035(7) -0.013(7) -0.030(7) _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 S1 O4 1.396(7) . ? S1 O2 1.434(4) . ? S1 O3 1.450(7) . ? S1 C4 1.765(5) . ? S2 O8 1.442(4) . ? S2 O6 1.449(4) . ? S2 O7 1.454(4) . ? S2 C11 1.768(5) . ? S3 O12 1.433(4) . ? S3 O11 1.440(4) . ? S3 O10 1.456(5) . ? S3 C18 1.771(5) . ? S4 O14 1.436(4) . ? S4 O16 1.444(4) . ? S4 O15 1.466(4) . ? S4 C25 1.772(5) . ? S5 O19 1.427(6) . ? S5 O20 1.435(6) . ? S5 O18 1.450(5) . ? S5 C32 1.774(5) . ? O1 C7 1.391(6) . ? O1 H1 0.8200 . ? O5 C14 1.372(6) . ? O5 H5 0.8200 . ? O9 C21 1.368(5) . ? O9 H9 0.8200 . ? O13 C28 1.385(5) . ? O13 H13 0.8200 . ? O17 C35 1.368(6) . ? O17 H17 0.8200 . ? C1 C34 1.515(7) . ? C1 C2 1.520(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C7 1.391(7) . ? C2 C3 1.391(7) . ? C3 C4 1.391(7) . ? C3 H3 0.9300 . ? C4 C5 1.386(7) . ? C5 C6 1.388(7) . ? C5 H5A 0.9300 . ? C6 C7 1.403(7) . ? C6 C8 1.516(7) . ? C8 C9 1.516(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.393(7) . ? C9 C14 1.406(7) . ? C10 C11 1.394(7) . ? C10 H10 0.9300 . ? C11 C12 1.390(7) . ? C12 C13 1.385(7) . ? C12 H12 0.9300 . ? C13 C14 1.399(6) . ? C13 C15 1.513(7) . ? C15 C16 1.519(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.387(6) . ? C16 C21 1.400(6) . ? C17 C18 1.386(6) . ? C17 H17A 0.9300 . ? C18 C19 1.387(6) . ? C19 C20 1.394(6) . ? C19 H19 0.9300 . ? C20 C21 1.395(6) . ? C20 C22 1.525(6) . ? C22 C23 1.522(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.391(7) . ? C23 C28 1.402(6) . ? C24 C25 1.387(7) . ? C24 H24 0.9300 . ? C25 C26 1.390(7) . ? C26 C27 1.391(7) . ? C26 H26 0.9300 . ? C27 C28 1.390(7) . ? C27 C29 1.522(6) . ? C29 C30 1.512(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.378(7) . ? C30 C35 1.404(6) . ? C31 C32 1.379(7) . ? C31 H31 0.9300 . ? C32 C33 1.395(7) . ? C33 C34 1.379(7) . ? C33 H33 0.9300 . ? C34 C35 1.400(6) . ? N1 C36 1.319(8) . ? N1 C40 1.330(8) . ? N1 H1C 0.8600 . ? N2 C44 1.327(7) . ? N2 C43 1.336(7) . ? N2 C46 1.498(6) . ? N3 C52 1.339(7) . ? N3 C48 1.349(7) . ? N3 C47 1.484(7) . ? N4 C56 1.319(11) . ? N4 C55 1.330(11) . ? N4 H4 0.8600 . ? C36 C37 1.373(8) . ? C36 H36 0.9300 . ? C37 C38 1.398(7) . ? C37 H37 0.9300 . ? C38 C39 1.384(7) . ? C38 C41 1.481(7) . ? C39 C40 1.374(8) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C45 1.379(7) . ? C41 C42 1.392(7) . ? C42 C43 1.384(8) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C45 1.379(7) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.513(7) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.371(8) . ? C48 H48 0.9300 . ? C49 C50 1.397(8) . ? C49 H49 0.9300 . ? C50 C51 1.378(8) . ? C50 C53 1.498(8) . ? C51 C52 1.371(9) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.372(10) . ? C53 C57 1.378(9) . ? C54 C55 1.392(10) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C57 1.355(11) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? O33 O38 1.25(2) . ? 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 O4 S1 O2 113.7(4) . . ? O4 S1 O3 113.0(6) . . ? O2 S1 O3 109.9(4) . . ? O4 S1 C4 107.5(4) . . ? O2 S1 C4 107.4(3) . . ? O3 S1 C4 104.7(3) . . ? O8 S2 O6 113.3(3) . . ? O8 S2 O7 112.5(3) . . ? O6 S2 O7 111.1(3) . . ? O8 S2 C11 107.3(2) . . ? O6 S2 C11 105.8(2) . . ? O7 S2 C11 106.4(2) . . ? O12 S3 O11 114.4(3) . . ? O12 S3 O10 111.7(3) . . ? O11 S3 O10 111.1(3) . . ? O12 S3 C18 106.6(2) . . ? O11 S3 C18 106.3(2) . . ? O10 S3 C18 106.1(2) . . ? O14 S4 O16 113.7(3) . . ? O14 S4 O15 111.3(2) . . ? O16 S4 O15 111.7(3) . . ? O14 S4 C25 107.6(2) . . ? O16 S4 C25 106.5(2) . . ? O15 S4 C25 105.5(2) . . ? O19 S5 O20 114.5(5) . . ? O19 S5 O18 109.3(4) . . ? O20 S5 O18 111.8(4) . . ? O19 S5 C32 106.1(3) . . ? O20 S5 C32 107.4(3) . . ? O18 S5 C32 107.3(3) . . ? C7 O1 H1 109.5 . . ? C14 O5 H5 109.5 . . ? C21 O9 H9 109.5 . . ? C28 O13 H13 109.5 . . ? C35 O17 H17 109.5 . . ? C34 C1 C2 115.4(4) . . ? C34 C1 H1A 108.4 . . ? C2 C1 H1A 108.4 . . ? C34 C1 H1B 108.4 . . ? C2 C1 H1B 108.4 . . ? H1A C1 H1B 107.5 . . ? C7 C2 C3 118.2(5) . . ? C7 C2 C1 122.1(5) . . ? C3 C2 C1 119.7(4) . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.7(5) . . ? C5 C4 S1 118.8(4) . . ? C3 C4 S1 120.5(4) . . ? C4 C5 C6 120.8(5) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C7 117.5(4) . . ? C5 C6 C8 120.0(4) . . ? C7 C6 C8 122.5(4) . . ? O1 C7 C2 118.5(4) . . ? O1 C7 C6 118.8(4) . . ? C2 C7 C6 122.7(4) . . ? C9 C8 C6 114.5(4) . . ? C9 C8 H8A 108.6 . . ? C6 C8 H8A 108.6 . . ? C9 C8 H8B 108.6 . . ? C6 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C14 117.8(4) . . ? C10 C9 C8 120.8(4) . . ? C14 C9 C8 121.3(4) . . ? C9 C10 C11 121.1(4) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 119.6(4) . . ? C12 C11 S2 118.8(4) . . ? C10 C11 S2 121.5(4) . . ? C13 C12 C11 121.3(4) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 118.2(4) . . ? C12 C13 C15 120.7(4) . . ? C14 C13 C15 121.0(4) . . ? O5 C14 C13 116.4(4) . . ? O5 C14 C9 121.6(4) . . ? C13 C14 C9 122.0(4) . . ? C13 C15 C16 114.6(4) . . ? C13 C15 H15A 108.6 . . ? C16 C15 H15A 108.6 . . ? C13 C15 H15B 108.6 . . ? C16 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C21 118.9(4) . . ? C17 C16 C15 121.8(4) . . ? C21 C16 C15 119.2(4) . . ? C18 C17 C16 120.4(4) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C17 C18 C19 120.2(4) . . ? C17 C18 S3 119.2(3) . . ? C19 C18 S3 120.6(3) . . ? C18 C19 C20 120.8(4) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 118.3(4) . . ? C19 C20 C22 119.1(4) . . ? C21 C20 C22 122.5(4) . . ? O9 C21 C20 123.0(4) . . ? O9 C21 C16 115.5(4) . . ? C20 C21 C16 121.4(4) . . ? C23 C22 C20 116.5(4) . . ? C23 C22 H22A 108.2 . . ? C20 C22 H22A 108.2 . . ? C23 C22 H22B 108.2 . . ? C20 C22 H22B 108.2 . . ? H22A C22 H22B 107.3 . . ? C24 C23 C28 118.4(4) . . ? C24 C23 C22 120.0(4) . . ? C28 C23 C22 121.4(4) . . ? C25 C24 C23 119.9(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.6(4) . . ? C24 C25 S4 119.3(4) . . ? C26 C25 S4 119.8(4) . . ? C25 C26 C27 120.9(4) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 117.7(4) . . ? C28 C27 C29 121.6(4) . . ? C26 C27 C29 120.7(4) . . ? O13 C28 C27 121.3(4) . . ? O13 C28 C23 116.3(4) . . ? C27 C28 C23 122.4(4) . . ? C30 C29 C27 114.4(4) . . ? C30 C29 H29A 108.7 . . ? C27 C29 H29A 108.7 . . ? C30 C29 H29B 108.7 . . ? C27 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C31 C30 C35 118.2(4) . . ? C31 C30 C29 119.9(4) . . ? C35 C30 C29 121.8(4) . . ? C30 C31 C32 121.4(4) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C31 C32 C33 119.7(5) . . ? C31 C32 S5 118.7(4) . . ? C33 C32 S5 121.6(4) . . ? C34 C33 C32 121.0(5) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 118.2(4) . . ? C33 C34 C1 121.1(4) . . ? C35 C34 C1 120.5(4) . . ? O17 C35 C34 116.5(4) . . ? O17 C35 C30 122.0(4) . . ? C34 C35 C30 121.5(4) . . ? C36 N1 C40 123.2(5) . . ? C36 N1 H1C 118.4 . . ? C40 N1 H1C 118.4 . . ? C44 N2 C43 121.7(5) . . ? C44 N2 C46 118.8(4) . . ? C43 N2 C46 119.5(5) . . ? C52 N3 C48 121.1(5) . . ? C52 N3 C47 119.8(5) . . ? C48 N3 C47 119.1(5) . . ? C56 N4 C55 124.2(7) . . ? C56 N4 H4 117.9 . . ? C55 N4 H4 117.9 . . ? N1 C36 C37 119.7(5) . . ? N1 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 118.8(5) . . ? C36 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C39 C38 C37 119.6(5) . . ? C39 C38 C41 121.2(5) . . ? C37 C38 C41 119.2(5) . . ? C40 C39 C38 118.4(5) . . ? C40 C39 H39 120.8 . . ? C38 C39 H39 120.8 . . ? N1 C40 C39 120.2(6) . . ? N1 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C45 C41 C42 118.4(5) . . ? C45 C41 C38 122.1(5) . . ? C42 C41 C38 119.5(4) . . ? C43 C42 C41 119.4(5) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? N2 C43 C42 120.1(5) . . ? N2 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? N2 C44 C45 120.5(5) . . ? N2 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C41 C45 C44 119.8(5) . . ? C41 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? N2 C46 C47 111.1(4) . . ? N2 C46 H46A 109.4 . . ? C47 C46 H46A 109.4 . . ? N2 C46 H46B 109.4 . . ? C47 C46 H46B 109.4 . . ? H46A C46 H46B 108.0 . . ? N3 C47 C46 107.0(4) . . ? N3 C47 H47A 110.3 . . ? C46 C47 H47A 110.3 . . ? N3 C47 H47B 110.3 . . ? C46 C47 H47B 110.3 . . ? H47A C47 H47B 108.6 . . ? N3 C48 C49 120.3(5) . . ? N3 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C48 C49 C50 119.8(6) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C51 C50 C49 118.1(5) . . ? C51 C50 C53 121.3(6) . . ? C49 C50 C53 120.6(5) . . ? C52 C51 C50 120.5(6) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? N3 C52 C51 120.3(6) . . ? N3 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C54 C53 C57 118.8(6) . . ? C54 C53 C50 120.5(6) . . ? C57 C53 C50 120.6(6) . . ? C53 C54 C55 119.8(8) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? N4 C55 C54 117.7(8) . . ? N4 C55 H55 121.1 . . ? C54 C55 H55 121.1 . . ? N4 C56 C57 119.2(8) . . ? N4 C56 H56 120.4 . . ? C57 C56 H56 120.4 . . ? C56 C57 C53 120.3(8) . . ? C56 C57 H57 119.9 . . ? C53 C57 H57 119.9 . . ? 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 C34 C1 C2 C7 -72.9(6) . . . . ? C34 C1 C2 C3 108.3(5) . . . . ? C7 C2 C3 C4 1.1(7) . . . . ? C1 C2 C3 C4 180.0(4) . . . . ? C2 C3 C4 C5 -0.1(7) . . . . ? C2 C3 C4 S1 -179.6(4) . . . . ? O4 S1 C4 C5 47.0(6) . . . . ? O2 S1 C4 C5 169.7(4) . . . . ? O3 S1 C4 C5 -73.4(6) . . . . ? O4 S1 C4 C3 -133.4(6) . . . . ? O2 S1 C4 C3 -10.7(5) . . . . ? O3 S1 C4 C3 106.2(6) . . . . ? C3 C4 C5 C6 0.3(7) . . . . ? S1 C4 C5 C6 179.9(4) . . . . ? C4 C5 C6 C7 -1.5(7) . . . . ? C4 C5 C6 C8 178.5(4) . . . . ? C3 C2 C7 O1 -179.9(4) . . . . ? C1 C2 C7 O1 1.2(6) . . . . ? C3 C2 C7 C6 -2.4(7) . . . . ? C1 C2 C7 C6 178.7(4) . . . . ? C5 C6 C7 O1 -179.9(4) . . . . ? C8 C6 C7 O1 0.2(6) . . . . ? C5 C6 C7 C2 2.6(7) . . . . ? C8 C6 C7 C2 -177.3(4) . . . . ? C5 C6 C8 C9 -106.0(5) . . . . ? C7 C6 C8 C9 73.9(6) . . . . ? C6 C8 C9 C10 -114.7(5) . . . . ? C6 C8 C9 C14 67.5(6) . . . . ? C14 C9 C10 C11 -2.6(7) . . . . ? C8 C9 C10 C11 179.6(4) . . . . ? C9 C10 C11 C12 0.3(7) . . . . ? C9 C10 C11 S2 176.1(4) . . . . ? O8 S2 C11 C12 -156.9(4) . . . . ? O6 S2 C11 C12 82.0(4) . . . . ? O7 S2 C11 C12 -36.3(4) . . . . ? O8 S2 C11 C10 27.4(5) . . . . ? O6 S2 C11 C10 -93.8(4) . . . . ? O7 S2 C11 C10 147.9(4) . . . . ? C10 C11 C12 C13 2.2(7) . . . . ? S2 C11 C12 C13 -173.7(3) . . . . ? C11 C12 C13 C14 -2.3(7) . . . . ? C11 C12 C13 C15 173.2(4) . . . . ? C12 C13 C14 O5 -178.4(4) . . . . ? C15 C13 C14 O5 6.1(6) . . . . ? C12 C13 C14 C9 0.0(7) . . . . ? C15 C13 C14 C9 -175.5(4) . . . . ? C10 C9 C14 O5 -179.3(4) . . . . ? C8 C9 C14 O5 -1.5(7) . . . . ? C10 C9 C14 C13 2.4(7) . . . . ? C8 C9 C14 C13 -179.8(4) . . . . ? C12 C13 C15 C16 49.4(6) . . . . ? C14 C13 C15 C16 -135.2(4) . . . . ? C13 C15 C16 C17 -100.0(5) . . . . ? C13 C15 C16 C21 82.4(5) . . . . ? C21 C16 C17 C18 0.4(7) . . . . ? C15 C16 C17 C18 -177.3(4) . . . . ? C16 C17 C18 C19 0.4(7) . . . . ? C16 C17 C18 S3 179.4(4) . . . . ? O12 S3 C18 C17 -59.8(4) . . . . ? O11 S3 C18 C17 177.8(4) . . . . ? O10 S3 C18 C17 59.4(5) . . . . ? O12 S3 C18 C19 119.2(4) . . . . ? O11 S3 C18 C19 -3.2(5) . . . . ? O10 S3 C18 C19 -121.6(4) . . . . ? C17 C18 C19 C20 0.2(7) . . . . ? S3 C18 C19 C20 -178.8(4) . . . . ? C18 C19 C20 C21 -1.5(7) . . . . ? C18 C19 C20 C22 174.8(4) . . . . ? C19 C20 C21 O9 179.9(4) . . . . ? C22 C20 C21 O9 3.8(7) . . . . ? C19 C20 C21 C16 2.4(7) . . . . ? C22 C20 C21 C16 -173.8(4) . . . . ? C17 C16 C21 O9 -179.5(4) . . . . ? C15 C16 C21 O9 -1.8(6) . . . . ? C17 C16 C21 C20 -1.8(7) . . . . ? C15 C16 C21 C20 175.9(4) . . . . ? C19 C20 C22 C23 96.0(5) . . . . ? C21 C20 C22 C23 -87.9(5) . . . . ? C20 C22 C23 C24 -88.7(5) . . . . ? C20 C22 C23 C28 96.9(5) . . . . ? C28 C23 C24 C25 1.5(7) . . . . ? C22 C23 C24 C25 -173.1(4) . . . . ? C23 C24 C25 C26 0.1(7) . . . . ? C23 C24 C25 S4 174.5(3) . . . . ? O14 S4 C25 C24 36.3(4) . . . . ? O16 S4 C25 C24 158.5(4) . . . . ? O15 S4 C25 C24 -82.6(4) . . . . ? O14 S4 C25 C26 -149.2(4) . . . . ? O16 S4 C25 C26 -27.0(5) . . . . ? O15 S4 C25 C26 91.9(4) . . . . ? C24 C25 C26 C27 -1.5(7) . . . . ? S4 C25 C26 C27 -175.9(4) . . . . ? C25 C26 C27 C28 1.2(7) . . . . ? C25 C26 C27 C29 180.0(4) . . . . ? C26 C27 C28 O13 -178.0(4) . . . . ? C29 C27 C28 O13 3.2(7) . . . . ? C26 C27 C28 C23 0.4(7) . . . . ? C29 C27 C28 C23 -178.3(4) . . . . ? C24 C23 C28 O13 176.7(4) . . . . ? C22 C23 C28 O13 -8.8(6) . . . . ? C24 C23 C28 C27 -1.8(7) . . . . ? C22 C23 C28 C27 172.7(4) . . . . ? C28 C27 C29 C30 -88.7(6) . . . . ? C26 C27 C29 C30 92.6(5) . . . . ? C27 C29 C30 C31 -55.5(6) . . . . ? C27 C29 C30 C35 128.8(5) . . . . ? C35 C30 C31 C32 -0.1(7) . . . . ? C29 C30 C31 C32 -176.0(5) . . . . ? C30 C31 C32 C33 -0.8(8) . . . . ? C30 C31 C32 S5 175.3(4) . . . . ? O19 S5 C32 C31 -75.2(6) . . . . ? O20 S5 C32 C31 161.9(5) . . . . ? O18 S5 C32 C31 41.6(5) . . . . ? O19 S5 C32 C33 100.8(6) . . . . ? O20 S5 C32 C33 -22.1(6) . . . . ? O18 S5 C32 C33 -142.4(5) . . . . ? C31 C32 C33 C34 -0.3(8) . . . . ? S5 C32 C33 C34 -176.2(4) . . . . ? C32 C33 C34 C35 2.2(7) . . . . ? C32 C33 C34 C1 178.0(5) . . . . ? C2 C1 C34 C33 115.3(5) . . . . ? C2 C1 C34 C35 -68.9(6) . . . . ? C33 C34 C35 O17 178.2(4) . . . . ? C1 C34 C35 O17 2.3(6) . . . . ? C33 C34 C35 C30 -3.1(7) . . . . ? C1 C34 C35 C30 -179.0(4) . . . . ? C31 C30 C35 O17 -179.3(4) . . . . ? C29 C30 C35 O17 -3.5(7) . . . . ? C31 C30 C35 C34 2.1(7) . . . . ? C29 C30 C35 C34 177.9(4) . . . . ? C40 N1 C36 C37 -0.6(9) . . . . ? N1 C36 C37 C38 1.0(8) . . . . ? C36 C37 C38 C39 -0.3(8) . . . . ? C36 C37 C38 C41 178.8(5) . . . . ? C37 C38 C39 C40 -0.8(8) . . . . ? C41 C38 C39 C40 -179.9(5) . . . . ? C36 N1 C40 C39 -0.5(9) . . . . ? C38 C39 C40 N1 1.2(9) . . . . ? C39 C38 C41 C45 57.1(7) . . . . ? C37 C38 C41 C45 -121.9(6) . . . . ? C39 C38 C41 C42 -123.6(6) . . . . ? C37 C38 C41 C42 57.4(7) . . . . ? C45 C41 C42 C43 0.6(8) . . . . ? C38 C41 C42 C43 -178.7(5) . . . . ? C44 N2 C43 C42 -2.8(9) . . . . ? C46 N2 C43 C42 179.7(5) . . . . ? C41 C42 C43 N2 1.5(9) . . . . ? C43 N2 C44 C45 1.9(8) . . . . ? C46 N2 C44 C45 179.4(5) . . . . ? C42 C41 C45 C44 -1.5(8) . . . . ? C38 C41 C45 C44 177.8(5) . . . . ? N2 C44 C45 C41 0.3(8) . . . . ? C44 N2 C46 C47 124.7(5) . . . . ? C43 N2 C46 C47 -57.7(7) . . . . ? C52 N3 C47 C46 103.3(6) . . . . ? C48 N3 C47 C46 -75.9(6) . . . . ? N2 C46 C47 N3 -174.7(5) . . . . ? C52 N3 C48 C49 -1.2(8) . . . . ? C47 N3 C48 C49 178.0(5) . . . . ? N3 C48 C49 C50 0.2(8) . . . . ? C48 C49 C50 C51 0.9(8) . . . . ? C48 C49 C50 C53 179.9(5) . . . . ? C49 C50 C51 C52 -1.0(8) . . . . ? C53 C50 C51 C52 180.0(5) . . . . ? C48 N3 C52 C51 1.2(8) . . . . ? C47 N3 C52 C51 -178.1(5) . . . . ? C50 C51 C52 N3 0.0(9) . . . . ? C51 C50 C53 C54 144.1(6) . . . . ? C49 C50 C53 C54 -34.9(8) . . . . ? C51 C50 C53 C57 -36.6(8) . . . . ? C49 C50 C53 C57 144.4(6) . . . . ? C57 C53 C54 C55 2.0(10) . . . . ? C50 C53 C54 C55 -178.6(6) . . . . ? C56 N4 C55 C54 -1.1(12) . . . . ? C53 C54 C55 N4 -0.8(11) . . . . ? C55 N4 C56 C57 1.7(13) . . . . ? N4 C56 C57 C53 -0.4(12) . . . . ? C54 C53 C57 C56 -1.4(10) . . . . ? C50 C53 C57 C56 179.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.950 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.098 # Attachment 'complex 2.cif' data_051206a _database_code_depnum_ccdc_archive 'CCDC 600933' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H65 N4 O25.50 S5' _chemical_formula_weight 1398.45 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9113(14) _cell_length_b 16.1145(19) _cell_length_c 19.514(2) _cell_angle_alpha 94.990(2) _cell_angle_beta 91.308(2) _cell_angle_gamma 105.576(2) _cell_volume 3590.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4497 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 24.32 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1462 _exptl_absorpt_coefficient_mu 0.239 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.793299 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 18253 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12521 _reflns_number_gt 6575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.2000P)^2^+0.0000P] 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 12521 _refine_ls_number_parameters 848 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.1872 _refine_ls_R_factor_gt 0.1180 _refine_ls_wR_factor_ref 0.3824 _refine_ls_wR_factor_gt 0.3117 _refine_ls_goodness_of_fit_ref 1.265 _refine_ls_restrained_S_all 1.270 _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 S1 S -0.0262(2) 0.26108(14) 0.45878(13) 0.0873(7) Uani 1 1 d . . . S2 S 0.5164(2) 0.38877(16) 0.31431(12) 0.0813(7) Uani 1 1 d . . . S3 S 0.96603(18) 0.91691(15) 0.25521(12) 0.0742(6) Uani 1 1 d . . . S4 S 0.50796(14) 0.71084(12) 0.02086(8) 0.0569(5) Uani 1 1 d . . . S5 S -0.08108(16) 0.37921(12) 0.09571(9) 0.0615(5) Uani 1 1 d . . . O1 O 0.1754(4) 0.6228(3) 0.4053(2) 0.0646(13) Uani 1 1 d . . . H1 H 0.1403 0.6366 0.3734 0.097 Uiso 1 1 calc R . . O2 O -0.1446(8) 0.2363(5) 0.4386(6) 0.187(5) Uani 1 1 d . . . O3 O 0.0411(12) 0.2149(5) 0.4178(7) 0.221(6) Uani 1 1 d . . . O4 O -0.0055(6) 0.2560(4) 0.5306(4) 0.119(3) Uani 1 1 d . . . O5 O 0.5053(6) 0.6994(4) 0.4904(3) 0.0949(18) Uani 1 1 d . . . H5 H 0.4588 0.6879 0.5208 0.142 Uiso 1 1 calc R . . O6 O 0.4429(17) 0.3240(6) 0.3331(9) 0.338(12) Uani 1 1 d . . . O7 O 0.6337(8) 0.3865(7) 0.3139(6) 0.192(5) Uani 1 1 d . . . O8 O 0.4975(13) 0.4042(6) 0.2469(5) 0.202(5) Uani 1 1 d . . . O9 O 0.5014(4) 0.7623(4) 0.3567(3) 0.0813(16) Uani 1 1 d . . . H9 H 0.5007 0.7782 0.3978 0.122 Uiso 1 1 calc R . . O10 O 1.0427(7) 0.8737(7) 0.2784(7) 0.208(6) Uani 1 1 d . . . O11 O 0.9929(8) 1.0005(6) 0.2798(8) 0.227(6) Uani 1 1 d . . . O12 O 0.9587(9) 0.9042(10) 0.1860(5) 0.233(7) Uani 1 1 d . . . O13 O 0.2641(4) 0.8146(3) 0.2593(2) 0.0618(12) Uani 1 1 d . . . H13 H 0.2783 0.8675 0.2650 0.093 Uiso 1 1 calc R . . O14 O 0.4948(9) 0.6209(5) 0.0230(4) 0.153(4) Uani 1 1 d . . . O15 O 0.6242(5) 0.7579(6) 0.0291(4) 0.140(3) Uani 1 1 d . . . O16 O 0.4539(7) 0.7295(7) -0.0379(3) 0.160(4) Uani 1 1 d . . . O17 O 0.0771(5) 0.6896(3) 0.2951(2) 0.0647(13) Uani 1 1 d . . . H17 H 0.1325 0.7252 0.2811 0.097 Uiso 1 1 calc R . . O18 O 0.0153(7) 0.3397(5) 0.0916(4) 0.140(3) Uani 1 1 d . . . O19 O -0.1069(7) 0.4064(4) 0.0328(3) 0.115(2) Uani 1 1 d . . . O20 O -0.1797(7) 0.3239(5) 0.1229(4) 0.145(3) Uani 1 1 d . . . C1 C 0.1234(5) 0.5399(4) 0.4165(3) 0.0476(15) Uani 1 1 d . . . C2 C 0.0122(6) 0.4947(4) 0.3885(3) 0.0505(15) Uani 1 1 d . . . C3 C -0.0335(6) 0.4102(5) 0.4016(3) 0.0574(17) Uani 1 1 d . . . H3 H -0.1070 0.3793 0.3831 0.069 Uiso 1 1 calc R . . C4 C 0.0303(6) 0.3704(4) 0.4429(3) 0.0604(17) Uani 1 1 d . . . C5 C 0.1392(6) 0.4159(4) 0.4707(3) 0.0577(17) Uani 1 1 d . . . H5A H 0.1812 0.3887 0.4976 0.069 Uiso 1 1 calc R . . C6 C 0.1864(6) 0.5005(4) 0.4594(3) 0.0510(15) Uani 1 1 d . . . C7 C 0.3039(6) 0.5512(4) 0.4916(3) 0.0555(16) Uani 1 1 d . . . H7A H 0.3163 0.5273 0.5342 0.067 Uiso 1 1 calc R . . H7B H 0.3017 0.6104 0.5035 0.067 Uiso 1 1 calc R . . C8 C 0.4074(6) 0.5524(4) 0.4476(3) 0.0538(16) Uani 1 1 d . . . C9 C 0.4133(6) 0.4794(5) 0.4067(3) 0.0559(16) Uani 1 1 d . . . H9A H 0.3532 0.4288 0.4067 0.067 Uiso 1 1 calc R . . C10 C 0.5074(6) 0.4802(5) 0.3655(3) 0.0626(19) Uani 1 1 d . . . C11 C 0.5992(6) 0.5556(5) 0.3667(4) 0.0625(18) Uani 1 1 d . . . H11 H 0.6621 0.5566 0.3390 0.075 Uiso 1 1 calc R . . C12 C 0.5972(6) 0.6281(5) 0.4084(4) 0.0611(18) Uani 1 1 d . . . C13 C 0.5021(6) 0.6255(4) 0.4493(3) 0.0573(17) Uani 1 1 d . . . C14 C 0.6988(6) 0.7094(5) 0.4129(4) 0.070(2) Uani 1 1 d . . . H14A H 0.6964 0.7426 0.4565 0.084 Uiso 1 1 calc R . . H14B H 0.7705 0.6918 0.4140 0.084 Uiso 1 1 calc R . . C15 C 0.7055(6) 0.7690(4) 0.3566(3) 0.0556(16) Uani 1 1 d . . . C16 C 0.8133(6) 0.8064(4) 0.3310(3) 0.0559(16) Uani 1 1 d . . . H16 H 0.8781 0.7896 0.3454 0.067 Uiso 1 1 calc R . . C17 C 0.8262(6) 0.8665(5) 0.2856(3) 0.0588(17) Uani 1 1 d . . . C18 C 0.7310(6) 0.8934(5) 0.2622(3) 0.0590(17) Uani 1 1 d . . . H18 H 0.7412 0.9353 0.2312 0.071 Uiso 1 1 calc R . . C19 C 0.6210(5) 0.8570(4) 0.2856(3) 0.0504(15) Uani 1 1 d . . . C20 C 0.6102(5) 0.7962(4) 0.3334(3) 0.0541(16) Uani 1 1 d . . . C21 C 0.5177(6) 0.8855(4) 0.2617(3) 0.0570(17) Uani 1 1 d . . . H21A H 0.5449 0.9423 0.2452 0.068 Uiso 1 1 calc R . . H21B H 0.4695 0.8906 0.3004 0.068 Uiso 1 1 calc R . . C22 C 0.4440(5) 0.8229(4) 0.2044(3) 0.0470(14) Uani 1 1 d . . . C23 C 0.4985(5) 0.7966(4) 0.1460(3) 0.0478(14) Uani 1 1 d . . . H23 H 0.5793 0.8158 0.1443 0.057 Uiso 1 1 calc R . . C24 C 0.4357(5) 0.7439(4) 0.0922(3) 0.0486(15) Uani 1 1 d . . . C25 C 0.3136(5) 0.7144(4) 0.0928(3) 0.0450(14) Uani 1 1 d . . . H25 H 0.2714 0.6794 0.0554 0.054 Uiso 1 1 calc R . . C26 C 0.2560(5) 0.7376(4) 0.1493(3) 0.0441(14) Uani 1 1 d . . . C27 C 0.3231(5) 0.7916(4) 0.2050(3) 0.0456(14) Uani 1 1 d . . . C28 C 0.1243(5) 0.7112(4) 0.1492(3) 0.0469(14) Uani 1 1 d . . . H28A H 0.1003 0.7569 0.1755 0.056 Uiso 1 1 calc R . . H28B H 0.0946 0.7082 0.1021 0.056 Uiso 1 1 calc R . . C29 C 0.0657(5) 0.6268(4) 0.1774(3) 0.0455(14) Uani 1 1 d . . . C30 C 0.0263(5) 0.5505(4) 0.1319(3) 0.0454(14) Uani 1 1 d . . . H30 H 0.0422 0.5521 0.0856 0.055 Uiso 1 1 calc R . . C31 C -0.0352(5) 0.4740(4) 0.1552(3) 0.0492(15) Uani 1 1 d . . . C32 C -0.0597(5) 0.4705(4) 0.2242(3) 0.0529(16) Uani 1 1 d . . . H32 H -0.1000 0.4182 0.2396 0.063 Uiso 1 1 calc R . . C33 C -0.0248(5) 0.5439(5) 0.2703(3) 0.0517(16) Uani 1 1 d . . . C34 C 0.0412(5) 0.6205(4) 0.2472(3) 0.0483(15) Uani 1 1 d . . . C35 C -0.0596(6) 0.5387(5) 0.3452(3) 0.0529(16) Uani 1 1 d . . . H35A H -0.0511 0.5969 0.3665 0.063 Uiso 1 1 calc R . . H35B H -0.1413 0.5073 0.3457 0.063 Uiso 1 1 calc R . . N1 N 0.3217(5) 0.4779(4) 0.1444(3) 0.0606(15) Uani 1 1 d . . . N2 N 0.2425(5) 0.4311(4) -0.0453(3) 0.0584(14) Uani 1 1 d . . . C36 C 0.4045(7) 0.5532(6) 0.1629(4) 0.071(2) Uani 1 1 d . . . H36 H 0.4608 0.5759 0.1322 0.085 Uiso 1 1 calc R . . C37 C 0.4050(8) 0.5957(6) 0.2266(4) 0.082(2) Uani 1 1 d . . . H37 H 0.4617 0.6474 0.2391 0.098 Uiso 1 1 calc R . . C38 C 0.3230(9) 0.5628(7) 0.2722(4) 0.082(3) Uani 1 1 d . . . H38 H 0.3230 0.5923 0.3154 0.098 Uiso 1 1 calc R . . C39 C 0.2412(8) 0.4862(8) 0.2537(4) 0.086(3) Uani 1 1 d . . . H39 H 0.1855 0.4619 0.2842 0.103 Uiso 1 1 calc R . . C40 C 0.2431(6) 0.4452(6) 0.1879(4) 0.073(2) Uani 1 1 d . . . H40 H 0.1873 0.3933 0.1745 0.087 Uiso 1 1 calc R . . C41 C 0.3187(7) 0.4346(6) 0.0730(3) 0.072(2) Uani 1 1 d . . . H41A H 0.2882 0.3724 0.0732 0.087 Uiso 1 1 calc R . . H41B H 0.3968 0.4467 0.0561 0.087 Uiso 1 1 calc R . . C42 C 0.2409(7) 0.4690(5) 0.0269(3) 0.066(2) Uani 1 1 d . . . H42A H 0.1618 0.4537 0.0423 0.079 Uiso 1 1 calc R . . H42B H 0.2686 0.5316 0.0293 0.079 Uiso 1 1 calc R . . C43 C 0.2954(7) 0.4810(6) -0.0912(4) 0.078(2) Uani 1 1 d . . . H43 H 0.3324 0.5390 -0.0783 0.093 Uiso 1 1 calc R . . C44 C 0.2960(9) 0.4462(9) -0.1607(5) 0.104(3) Uani 1 1 d . . . H44 H 0.3342 0.4797 -0.1941 0.125 Uiso 1 1 calc R . . C45 C 0.2363(12) 0.3591(11) -0.1763(6) 0.119(4) Uani 1 1 d . . . H45 H 0.2348 0.3339 -0.2211 0.143 Uiso 1 1 calc R . . C46 C 0.1820(9) 0.3118(7) -0.1290(5) 0.096(3) Uani 1 1 d . . . H46 H 0.1412 0.2541 -0.1398 0.115 Uiso 1 1 calc R . . C47 C 0.1879(8) 0.3507(7) -0.0635(5) 0.086(2) Uani 1 1 d . . . H47 H 0.1504 0.3175 -0.0297 0.103 Uiso 1 1 calc R . . N3 N 0.3644(10) 0.9313(8) 0.0352(7) 0.129(3) Uani 1 1 d . . . C48 C 0.2844(14) 0.8730(10) -0.0102(8) 0.136(4) Uani 1 1 d . . . H48 H 0.3084 0.8480 -0.0500 0.164 Uiso 1 1 calc R . . C49 C 0.1673(13) 0.8527(9) 0.0052(9) 0.135(4) Uani 1 1 d . . . H49 H 0.1128 0.8121 -0.0240 0.162 Uiso 1 1 calc R . . C50 C 0.1308(14) 0.8916(11) 0.0626(9) 0.141(5) Uani 1 1 d . . . H50 H 0.0518 0.8813 0.0707 0.169 Uiso 1 1 calc R . . C51 C 0.2192(16) 0.9495(10) 0.1105(10) 0.159(7) Uani 1 1 d . . . H51 H 0.1998 0.9738 0.1520 0.191 Uiso 1 1 calc R . . C52 C 0.3265(14) 0.9652(9) 0.0922(7) 0.136(4) Uani 1 1 d . . . H52 H 0.3826 1.0041 0.1216 0.164 Uiso 1 1 calc R . . C53 C 0.4893(12) 0.9550(9) 0.0159(8) 0.150(5) Uani 1 1 d . . . H53A H 0.5031 0.9112 -0.0176 0.180 Uiso 1 1 calc R . . H53B H 0.5409 0.9604 0.0562 0.180 Uiso 1 1 calc R . . N4 N 1.1514(15) 0.0398(16) 0.5092(14) 0.181(13) Uiso 0.50 1 d PGD . . C54 C 1.200(2) 0.0937(15) 0.4596(12) 0.156(10) Uiso 0.50 1 d PG . . C55 C 1.320(3) 0.1140(17) 0.4511(13) 0.223(17) Uiso 0.50 1 d PG . . C56 C 1.3905(16) 0.080(2) 0.4922(17) 0.33(4) Uiso 0.50 1 d PG . . C57 C 1.341(2) 0.0264(17) 0.5418(13) 0.160(12) Uiso 0.50 1 d PG . . C58 C 1.222(2) 0.0061(13) 0.5503(11) 0.137(9) Uiso 0.50 1 d PG . . C59 C 1.0303(18) 0.045(3) 0.520(2) 0.15(2) Uiso 0.50 1 d PD . . N5 N 0.8443(10) -0.0311(10) 0.4672(9) 0.110(6) Uiso 0.50 1 d PGD . . C65 C 0.7586(15) -0.0769(10) 0.5073(8) 0.118(7) Uiso 0.50 1 d PG . . C64 C 0.6442(13) -0.0725(13) 0.4991(10) 0.141(10) Uiso 0.50 1 d PG . . C63 C 0.6154(11) -0.0223(15) 0.4507(11) 0.183(15) Uiso 0.50 1 d PG . . C62 C 0.7010(15) 0.0236(11) 0.4106(8) 0.113(7) Uiso 0.50 1 d PG . . C61 C 0.8154(13) 0.0192(10) 0.4188(8) 0.098(6) Uiso 0.50 1 d PG . . C60 C 0.9678(15) -0.032(2) 0.4675(18) 0.096(11) Uiso 0.50 1 d PD . . O21 O 0.1539(8) 0.8735(6) 0.4051(5) 0.160(3) Uani 1 1 d U . . O22 O 0.3950(15) 0.2753(11) 0.1485(7) 0.138(5) Uani 0.50 1 d PU . . O23 O 0.6923(14) 0.2678(9) 0.2243(8) 0.128(5) Uani 0.50 1 d PU . . O24 O 0.3720(13) 0.7595(10) 0.5780(8) 0.251(6) Uani 1 1 d U . . O25 O 0.3607(14) 0.8487(11) 0.4233(8) 0.260(6) Uani 1 1 d U . . O26 O 0.3117(16) 0.9872(11) 0.2903(10) 0.149(6) Uani 0.50 1 d PU . . O27 O 0.902(3) 1.008(2) 0.0972(16) 0.134(10) Uani 0.25 1 d PU . . O28 O 0.489(4) 0.112(3) 0.328(2) 0.188(16) Uani 0.25 1 d PU . . O29 O 0.233(4) 0.200(3) 0.346(2) 0.340(19) Uani 0.50 1 d PU . . 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 S1 0.1026(18) 0.0596(13) 0.0908(16) 0.0177(11) 0.0020(13) 0.0038(12) S2 0.0879(16) 0.0816(16) 0.0798(15) -0.0073(12) -0.0043(12) 0.0378(13) S3 0.0596(12) 0.0784(15) 0.0843(15) 0.0079(11) 0.0190(10) 0.0170(10) S4 0.0493(10) 0.0774(13) 0.0467(9) -0.0011(8) 0.0082(7) 0.0234(9) S5 0.0634(11) 0.0665(12) 0.0485(10) 0.0015(8) -0.0073(8) 0.0091(9) O1 0.081(3) 0.053(3) 0.061(3) 0.017(2) 0.006(2) 0.017(2) O2 0.160(8) 0.102(6) 0.260(11) 0.096(7) -0.098(8) -0.048(5) O3 0.295(14) 0.069(5) 0.301(14) 0.010(6) 0.169(12) 0.042(7) O4 0.143(6) 0.098(5) 0.102(5) 0.056(4) -0.015(4) -0.005(4) O5 0.097(5) 0.072(4) 0.100(5) -0.023(3) 0.009(3) 0.006(3) O6 0.53(3) 0.084(6) 0.38(2) -0.044(8) 0.35(2) 0.039(10) O7 0.129(7) 0.213(10) 0.241(12) -0.088(9) -0.015(7) 0.093(7) O8 0.360(17) 0.150(8) 0.101(7) -0.038(6) -0.014(8) 0.097(9) O9 0.049(3) 0.114(4) 0.077(4) 0.025(3) 0.004(2) 0.011(3) O10 0.094(6) 0.235(11) 0.349(16) 0.150(11) 0.096(8) 0.093(7) O11 0.132(7) 0.114(7) 0.407(18) -0.019(9) 0.161(10) -0.015(5) O12 0.143(8) 0.377(18) 0.105(7) -0.012(8) 0.058(6) -0.053(9) O13 0.060(3) 0.076(3) 0.051(3) -0.011(2) 0.010(2) 0.026(3) O14 0.240(9) 0.094(5) 0.148(6) 0.020(4) 0.140(7) 0.073(6) O15 0.068(4) 0.211(8) 0.103(5) -0.057(5) 0.034(3) -0.006(5) O16 0.162(7) 0.329(12) 0.045(3) 0.013(5) 0.018(4) 0.163(8) O17 0.087(4) 0.060(3) 0.049(3) 0.006(2) 0.017(2) 0.021(3) O18 0.122(6) 0.120(6) 0.182(8) -0.072(5) -0.059(5) 0.073(5) O19 0.198(7) 0.095(4) 0.046(3) 0.001(3) -0.036(4) 0.030(4) O20 0.151(7) 0.126(6) 0.099(5) -0.022(4) 0.038(5) -0.055(5) C1 0.058(4) 0.051(4) 0.035(3) 0.003(3) 0.005(3) 0.016(3) C2 0.058(4) 0.065(4) 0.035(3) 0.011(3) 0.014(3) 0.024(3) C3 0.061(4) 0.066(5) 0.041(3) 0.003(3) 0.005(3) 0.013(3) C4 0.072(5) 0.058(4) 0.049(4) 0.009(3) 0.006(3) 0.014(4) C5 0.065(4) 0.061(4) 0.047(4) 0.015(3) 0.002(3) 0.014(4) C6 0.061(4) 0.058(4) 0.036(3) 0.008(3) 0.006(3) 0.019(3) C7 0.064(4) 0.060(4) 0.043(3) 0.006(3) -0.002(3) 0.019(3) C8 0.064(4) 0.061(4) 0.039(3) 0.010(3) -0.010(3) 0.021(3) C9 0.056(4) 0.062(4) 0.051(4) 0.011(3) -0.008(3) 0.017(3) C10 0.068(5) 0.079(5) 0.050(4) 0.012(3) -0.008(3) 0.035(4) C11 0.059(4) 0.078(5) 0.057(4) 0.018(4) -0.004(3) 0.028(4) C12 0.063(4) 0.069(5) 0.054(4) 0.017(4) -0.009(3) 0.020(4) C13 0.063(4) 0.056(4) 0.051(4) 0.002(3) -0.008(3) 0.015(3) C14 0.059(4) 0.077(5) 0.070(5) 0.021(4) -0.017(4) 0.008(4) C15 0.054(4) 0.056(4) 0.055(4) -0.004(3) -0.013(3) 0.016(3) C16 0.046(4) 0.064(4) 0.058(4) -0.001(3) -0.005(3) 0.019(3) C17 0.051(4) 0.070(5) 0.054(4) -0.002(3) 0.005(3) 0.016(3) C18 0.059(4) 0.060(4) 0.057(4) -0.003(3) -0.003(3) 0.017(3) C19 0.051(4) 0.052(4) 0.045(3) -0.006(3) -0.006(3) 0.013(3) C20 0.048(4) 0.060(4) 0.050(4) -0.006(3) -0.007(3) 0.011(3) C21 0.059(4) 0.054(4) 0.058(4) -0.004(3) -0.002(3) 0.018(3) C22 0.045(3) 0.051(4) 0.050(3) -0.001(3) -0.005(3) 0.023(3) C23 0.038(3) 0.061(4) 0.045(3) 0.001(3) 0.001(3) 0.016(3) C24 0.046(3) 0.063(4) 0.042(3) 0.010(3) 0.004(3) 0.023(3) C25 0.045(3) 0.056(4) 0.038(3) 0.003(3) 0.000(2) 0.021(3) C26 0.042(3) 0.048(3) 0.047(3) 0.009(3) 0.000(3) 0.019(3) C27 0.051(4) 0.048(4) 0.043(3) 0.003(3) 0.003(3) 0.024(3) C28 0.046(3) 0.059(4) 0.041(3) 0.007(3) -0.002(3) 0.023(3) C29 0.039(3) 0.066(4) 0.037(3) 0.009(3) 0.001(2) 0.022(3) C30 0.041(3) 0.067(4) 0.035(3) 0.005(3) 0.000(2) 0.025(3) C31 0.050(4) 0.060(4) 0.038(3) 0.004(3) -0.005(3) 0.017(3) C32 0.047(4) 0.063(4) 0.048(4) 0.009(3) 0.000(3) 0.014(3) C33 0.045(3) 0.077(5) 0.040(3) 0.012(3) 0.002(3) 0.025(3) C34 0.047(3) 0.063(4) 0.041(3) 0.003(3) 0.001(3) 0.025(3) C35 0.052(4) 0.072(4) 0.039(3) 0.014(3) 0.011(3) 0.020(3) N1 0.064(4) 0.093(5) 0.039(3) 0.006(3) 0.006(3) 0.046(4) N2 0.064(4) 0.076(4) 0.041(3) -0.007(3) 0.000(3) 0.035(3) C36 0.079(5) 0.094(6) 0.052(4) 0.014(4) 0.002(4) 0.043(5) C37 0.096(6) 0.095(6) 0.062(5) -0.001(4) -0.018(5) 0.044(5) C38 0.101(7) 0.126(8) 0.041(4) 0.003(5) -0.012(4) 0.073(6) C39 0.076(6) 0.156(9) 0.049(4) 0.022(5) 0.008(4) 0.067(6) C40 0.057(4) 0.106(6) 0.057(4) 0.008(4) -0.004(4) 0.026(4) C41 0.083(5) 0.098(6) 0.049(4) -0.009(4) 0.005(4) 0.052(5) C42 0.078(5) 0.091(5) 0.041(4) -0.006(3) 0.000(3) 0.046(4) C43 0.078(5) 0.107(6) 0.055(4) -0.002(4) -0.005(4) 0.040(5) C44 0.101(7) 0.176(11) 0.052(5) 0.015(6) 0.015(5) 0.063(8) C45 0.124(9) 0.186(13) 0.064(6) -0.046(8) -0.023(6) 0.091(10) C46 0.099(7) 0.119(8) 0.070(6) -0.029(6) -0.020(5) 0.043(6) C47 0.075(6) 0.113(8) 0.077(6) 0.002(5) 0.000(4) 0.042(5) N3 0.107(8) 0.131(9) 0.160(11) 0.052(8) 0.024(8) 0.037(7) C48 0.131(12) 0.133(11) 0.158(13) 0.056(10) 0.029(10) 0.042(9) C49 0.119(11) 0.118(10) 0.169(14) 0.044(9) 0.031(9) 0.023(8) C50 0.123(11) 0.145(12) 0.152(13) 0.041(10) 0.032(10) 0.018(10) C51 0.158(14) 0.131(11) 0.220(18) 0.079(12) 0.105(14) 0.065(11) C52 0.141(12) 0.142(11) 0.119(10) 0.014(8) 0.031(9) 0.025(9) C53 0.143(11) 0.159(11) 0.193(14) 0.103(10) 0.064(9) 0.085(9) O21 0.156(6) 0.163(6) 0.143(6) 0.018(5) 0.037(5) 0.009(5) O22 0.153(9) 0.163(9) 0.085(7) -0.007(7) 0.022(7) 0.024(7) O23 0.141(8) 0.113(8) 0.133(8) 0.000(6) 0.067(7) 0.043(7) O24 0.233(9) 0.260(9) 0.252(10) -0.010(8) 0.034(8) 0.062(8) O25 0.255(10) 0.272(10) 0.241(9) 0.005(8) 0.018(8) 0.055(8) O26 0.149(9) 0.133(9) 0.171(10) -0.011(7) 0.016(8) 0.058(7) O27 0.137(13) 0.128(13) 0.129(13) 0.027(9) 0.002(9) 0.019(9) O28 0.191(18) 0.184(18) 0.182(18) 0.018(10) 0.004(10) 0.041(10) O29 0.34(2) 0.34(2) 0.34(2) 0.031(10) 0.029(10) 0.092(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 S1 O2 1.395(9) . ? S1 O4 1.431(7) . ? S1 O3 1.443(9) . ? S1 C4 1.767(7) . ? S2 O6 1.257(11) . ? S2 O8 1.385(10) . ? S2 O7 1.407(9) . ? S2 C10 1.736(8) . ? S3 O11 1.340(9) . ? S3 O12 1.345(9) . ? S3 O10 1.379(8) . ? S3 C17 1.785(7) . ? S4 O15 1.387(6) . ? S4 O16 1.397(7) . ? S4 O14 1.419(7) . ? S4 C24 1.770(6) . ? S5 O19 1.395(5) . ? S5 O20 1.416(7) . ? S5 O18 1.456(7) . ? S5 C31 1.787(6) . ? O1 C1 1.353(7) . ? O1 H1 0.8200 . ? O5 C13 1.368(8) . ? O5 H5 0.8200 . ? O9 C20 1.370(8) . ? O9 H9 0.8200 . ? O13 C27 1.365(7) . ? O13 H13 0.8200 . ? O17 C34 1.357(7) . ? O17 H17 0.8200 . ? C1 C2 1.401(9) . ? C1 C6 1.409(8) . ? C2 C3 1.373(9) . ? C2 C35 1.532(8) . ? C3 C4 1.399(9) . ? C3 H3 0.9300 . ? C4 C5 1.379(10) . ? C5 C6 1.366(9) . ? C5 H5A 0.9300 . ? C6 C7 1.510(9) . ? C7 C8 1.515(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.382(9) . ? C8 C13 1.393(9) . ? C9 C10 1.393(10) . ? C9 H9A 0.9300 . ? C10 C11 1.398(10) . ? C11 C12 1.370(10) . ? C11 H11 0.9300 . ? C12 C13 1.394(10) . ? C12 C14 1.520(10) . ? C14 C15 1.510(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.388(9) . ? C15 C20 1.402(9) . ? C16 C17 1.349(9) . ? C16 H16 0.9300 . ? C17 C18 1.400(9) . ? C18 C19 1.390(9) . ? C18 H18 0.9300 . ? C19 C20 1.394(9) . ? C19 C21 1.503(9) . ? C21 C22 1.523(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.393(8) . ? C22 C23 1.414(8) . ? C23 C24 1.360(8) . ? C23 H23 0.9300 . ? C24 C25 1.404(8) . ? C25 C26 1.388(8) . ? C25 H25 0.9300 . ? C26 C27 1.414(8) . ? C26 C28 1.511(8) . ? C28 C29 1.508(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C34 1.405(8) . ? C29 C30 1.415(8) . ? C30 C31 1.374(9) . ? C30 H30 0.9300 . ? C31 C32 1.387(8) . ? C32 C33 1.384(9) . ? C32 H32 0.9300 . ? C33 C34 1.392(9) . ? C33 C35 1.533(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? N1 C40 1.313(9) . ? N1 C36 1.357(10) . ? N1 C41 1.498(8) . ? N2 C47 1.297(11) . ? N2 C43 1.312(10) . ? N2 C42 1.490(8) . ? C36 C37 1.366(11) . ? C36 H36 0.9300 . ? C37 C38 1.368(12) . ? C37 H37 0.9300 . ? C38 C39 1.366(13) . ? C38 H38 0.9300 . ? C39 C40 1.396(11) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.516(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.424(12) . ? C43 H43 0.9300 . ? C44 C45 1.395(16) . ? C44 H44 0.9300 . ? C45 C46 1.317(16) . ? C45 H45 0.9300 . ? C46 C47 1.366(12) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? N3 C52 1.337(16) . ? N3 C48 1.382(17) . ? N3 C53 1.499(15) . ? C48 C49 1.391(17) . ? C48 H48 0.9300 . ? C49 C50 1.373(18) . ? C49 H49 0.9300 . ? C50 C51 1.46(2) . ? C50 H50 0.9300 . ? C51 C52 1.299(18) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C53 1.59(2) 2_675 ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? N4 N5 0.50(3) 2_756 ? N4 C65 1.15(4) 2_756 ? N4 C54 1.3900 . ? N4 C58 1.3900 . ? N4 C60 1.48(3) 2_756 ? N4 C59 1.483(10) . ? N4 C61 1.86(5) 2_756 ? C54 C65 0.90(5) 2_756 ? C54 C55 1.3900 . ? C54 N5 1.83(3) 2_756 ? C55 C65 1.31(5) 2_756 ? C55 C64 1.35(7) 2_756 ? C55 C56 1.3900 . ? C56 C64 0.44(4) 2_756 ? C56 C57 1.3900 . ? C56 C63 1.51(8) 2_756 ? C56 C65 1.76(3) 2_756 ? C57 C63 0.55(3) 2_756 ? C57 C64 1.12(7) 2_756 ? C57 C62 1.30(7) 2_756 ? C57 C58 1.3900 . ? C57 C65 1.90(5) 2_756 ? C57 C61 2.01(5) 2_756 ? C58 C61 0.83(6) 2_756 ? C58 N5 1.04(3) 2_756 ? C58 C62 1.39(4) 2_756 ? C58 C65 1.65(6) 2_756 ? C58 C63 1.89(3) 2_756 ? C58 C64 1.99(5) 2_756 ? C59 C60 0.33(6) 2_756 ? C59 C60 1.542(10) . ? C59 C59 1.55(7) 2_756 ? C59 N5 1.59(3) 2_756 ? N5 N4 0.50(3) 2_756 ? N5 C58 1.04(6) 2_756 ? N5 C65 1.3900 . ? N5 C61 1.3900 . ? N5 C60 1.477(10) . ? N5 C59 1.59(3) 2_756 ? N5 C54 1.83(8) 2_756 ? C65 C54 0.90(9) 2_756 ? C65 N4 1.15(3) 2_756 ? C65 C55 1.31(7) 2_756 ? C65 C64 1.3900 . ? C65 C58 1.65(10) 2_756 ? C65 C56 1.76(4) 2_756 ? C65 C57 1.90(8) 2_756 ? C64 C56 0.44(6) 2_756 ? C64 C57 1.12(12) 2_756 ? C64 C55 1.35(11) 2_756 ? C64 C63 1.3900 . ? C64 C58 1.99(8) 2_756 ? C63 C57 0.55(4) 2_756 ? C63 C62 1.3900 . ? C63 C56 1.51(13) 2_756 ? C63 C58 1.89(3) 2_756 ? C62 C57 1.30(11) 2_756 ? C62 C58 1.39(6) 2_756 ? C62 C61 1.3900 . ? C61 C58 0.83(9) 2_756 ? C61 N4 1.86(3) 2_756 ? C61 C57 2.01(7) 2_756 ? C60 C59 0.33(6) 2_756 ? C60 N4 1.48(3) 2_756 ? C60 C60 1.61(7) 2_756 ? 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 O2 S1 O4 113.0(6) . . ? O2 S1 O3 113.0(8) . . ? O4 S1 O3 110.7(7) . . ? O2 S1 C4 107.6(4) . . ? O4 S1 C4 107.3(4) . . ? O3 S1 C4 104.7(4) . . ? O6 S2 O8 113.8(12) . . ? O6 S2 O7 117.5(11) . . ? O8 S2 O7 100.9(8) . . ? O6 S2 C10 108.6(5) . . ? O8 S2 C10 106.4(5) . . ? O7 S2 C10 109.0(5) . . ? O11 S3 O12 113.7(9) . . ? O11 S3 O10 113.5(9) . . ? O12 S3 O10 107.5(9) . . ? O11 S3 C17 106.8(4) . . ? O12 S3 C17 107.8(5) . . ? O10 S3 C17 107.2(4) . . ? O15 S4 O16 111.8(6) . . ? O15 S4 O14 111.5(6) . . ? O16 S4 O14 112.8(6) . . ? O15 S4 C24 107.2(3) . . ? O16 S4 C24 106.6(3) . . ? O14 S4 C24 106.5(3) . . ? O19 S5 O20 112.7(5) . . ? O19 S5 O18 111.8(5) . . ? O20 S5 O18 111.2(6) . . ? O19 S5 C31 106.8(3) . . ? O20 S5 C31 106.8(4) . . ? O18 S5 C31 107.2(3) . . ? C1 O1 H1 109.5 . . ? C13 O5 H5 109.5 . . ? C20 O9 H9 109.5 . . ? C27 O13 H13 109.5 . . ? C34 O17 H17 109.5 . . ? O1 C1 C2 122.8(6) . . ? O1 C1 C6 116.5(6) . . ? C2 C1 C6 120.7(6) . . ? C3 C2 C1 119.1(6) . . ? C3 C2 C35 119.9(6) . . ? C1 C2 C35 121.0(6) . . ? C2 C3 C4 120.1(6) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.2(6) . . ? C5 C4 S1 119.2(5) . . ? C3 C4 S1 120.6(6) . . ? C6 C5 C4 121.1(6) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C5 C6 C1 118.7(6) . . ? C5 C6 C7 121.1(6) . . ? C1 C6 C7 120.2(6) . . ? C6 C7 C8 115.7(5) . . ? C6 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? C6 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C13 117.6(7) . . ? C9 C8 C7 120.9(6) . . ? C13 C8 C7 121.4(6) . . ? C8 C9 C10 121.3(7) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C9 C10 C11 119.5(7) . . ? C9 C10 S2 121.8(6) . . ? C11 C10 S2 118.7(6) . . ? C12 C11 C10 120.4(7) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.0(7) . . ? C11 C12 C14 121.1(7) . . ? C13 C12 C14 119.8(7) . . ? O5 C13 C8 121.4(7) . . ? O5 C13 C12 116.5(6) . . ? C8 C13 C12 122.1(7) . . ? C15 C14 C12 117.7(5) . . ? C15 C14 H14A 107.9 . . ? C12 C14 H14A 107.9 . . ? C15 C14 H14B 107.9 . . ? C12 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? C16 C15 C20 117.2(6) . . ? C16 C15 C14 119.1(6) . . ? C20 C15 C14 123.3(6) . . ? C17 C16 C15 121.6(6) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 121.2(7) . . ? C16 C17 S3 121.3(5) . . ? C18 C17 S3 117.5(6) . . ? C19 C18 C17 119.3(7) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 118.4(6) . . ? C18 C19 C21 120.3(6) . . ? C20 C19 C21 121.3(6) . . ? O9 C20 C19 117.4(6) . . ? O9 C20 C15 120.4(6) . . ? C19 C20 C15 122.2(6) . . ? C19 C21 C22 112.5(5) . . ? C19 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C19 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C27 C22 C23 117.1(5) . . ? C27 C22 C21 123.4(6) . . ? C23 C22 C21 119.5(5) . . ? C24 C23 C22 121.6(6) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 120.7(6) . . ? C23 C24 S4 120.0(5) . . ? C25 C24 S4 119.3(5) . . ? C26 C25 C24 120.0(6) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 118.3(5) . . ? C25 C26 C28 120.9(5) . . ? C27 C26 C28 120.6(5) . . ? O13 C27 C22 120.6(5) . . ? O13 C27 C26 117.1(5) . . ? C22 C27 C26 122.3(5) . . ? C29 C28 C26 117.7(5) . . ? C29 C28 H28A 107.9 . . ? C26 C28 H28A 107.9 . . ? C29 C28 H28B 107.9 . . ? C26 C28 H28B 107.9 . . ? H28A C28 H28B 107.2 . . ? C34 C29 C30 117.2(6) . . ? C34 C29 C28 123.1(6) . . ? C30 C29 C28 119.6(5) . . ? C31 C30 C29 121.1(5) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 120.2(6) . . ? C30 C31 S5 119.2(5) . . ? C32 C31 S5 120.6(5) . . ? C33 C32 C31 120.7(6) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 119.0(6) . . ? C32 C33 C35 119.3(6) . . ? C34 C33 C35 121.8(6) . . ? O17 C34 C33 116.5(5) . . ? O17 C34 C29 121.7(6) . . ? C33 C34 C29 121.7(6) . . ? C2 C35 C33 114.0(5) . . ? C2 C35 H35A 108.8 . . ? C33 C35 H35A 108.8 . . ? C2 C35 H35B 108.8 . . ? C33 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C40 N1 C36 120.2(6) . . ? C40 N1 C41 120.6(7) . . ? C36 N1 C41 119.1(6) . . ? C47 N2 C43 120.3(7) . . ? C47 N2 C42 120.4(7) . . ? C43 N2 C42 119.2(7) . . ? N1 C36 C37 119.8(8) . . ? N1 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 120.6(9) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C39 C38 C37 119.3(8) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 118.3(8) . . ? C38 C39 H39 120.8 . . ? C40 C39 H39 120.8 . . ? N1 C40 C39 121.8(8) . . ? N1 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? N1 C41 C42 108.3(5) . . ? N1 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? N1 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? N2 C42 C41 109.4(5) . . ? N2 C42 H42A 109.8 . . ? C41 C42 H42A 109.8 . . ? N2 C42 H42B 109.8 . . ? C41 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? N2 C43 C44 119.9(9) . . ? N2 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C45 C44 C43 116.5(10) . . ? C45 C44 H44 121.7 . . ? C43 C44 H44 121.7 . . ? C46 C45 C44 121.6(9) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C45 C46 C47 117.5(11) . . ? C45 C46 H46 121.3 . . ? C47 C46 H46 121.3 . . ? N2 C47 C46 124.1(10) . . ? N2 C47 H47 118.0 . . ? C46 C47 H47 118.0 . . ? C52 N3 C48 119.0(13) . . ? C52 N3 C53 123.8(14) . . ? C48 N3 C53 117.2(13) . . ? N3 C48 C49 118.3(15) . . ? N3 C48 H48 120.8 . . ? C49 C48 H48 120.8 . . ? C50 C49 C48 121.2(16) . . ? C50 C49 H49 119.4 . . ? C48 C49 H49 119.4 . . ? C49 C50 C51 118.2(15) . . ? C49 C50 H50 120.9 . . ? C51 C50 H50 120.9 . . ? C52 C51 C50 116.5(16) . . ? C52 C51 H51 121.8 . . ? C50 C51 H51 121.8 . . ? C51 C52 N3 126.6(16) . . ? C51 C52 H52 116.7 . . ? N3 C52 H52 116.7 . . ? N3 C53 C53 105.9(11) . 2_675 ? N3 C53 H53A 110.5 . . ? C53 C53 H53A 110.5 2_675 . ? N3 C53 H53B 110.5 . . ? C53 C53 H53B 110.5 2_675 . ? H53A C53 H53B 108.7 . . ? N5 N4 C65 109(4) 2_756 2_756 ? N5 N4 C54 147(3) 2_756 . ? C65 N4 C54 40(3) 2_756 . ? N5 N4 C58 38(3) 2_756 . ? C65 N4 C58 80(3) 2_756 . ? C54 N4 C58 120.0 . . ? N5 N4 C60 80(3) 2_756 2_756 ? C65 N4 C60 154(5) 2_756 2_756 ? C54 N4 C60 123(2) . 2_756 ? C58 N4 C60 116(2) . 2_756 ? N5 N4 C59 92(3) 2_756 . ? C65 N4 C59 144(4) 2_756 . ? C54 N4 C59 110(3) . . ? C58 N4 C59 129(3) . . ? C60 N4 C59 13(2) 2_756 . ? N5 N4 C61 18(2) 2_756 2_756 ? C65 N4 C61 104(2) 2_756 2_756 ? C54 N4 C61 144.3(15) . 2_756 ? C58 N4 C61 24.6(16) . 2_756 ? C60 N4 C61 91(2) 2_756 2_756 ? C59 N4 C61 104(3) . 2_756 ? C65 C54 N4 55(2) 2_756 . ? C65 C54 C55 66(3) 2_756 . ? N4 C54 C55 120.0 . . ? C65 C54 N5 48(3) 2_756 2_756 ? N4 C54 N5 8.6(10) . 2_756 ? C55 C54 N5 113.1(8) . 2_756 ? C65 C55 C64 63(3) 2_756 2_756 ? C65 C55 C56 81.5(19) 2_756 . ? C64 C55 C56 18.5(17) 2_756 . ? C65 C55 C54 39.0(18) 2_756 . ? C64 C55 C54 101.7(15) 2_756 . ? C56 C55 C54 120.0 . . ? C64 C56 C55 76(8) 2_756 . ? C64 C56 C57 45(9) 2_756 . ? C55 C56 C57 120.0 . . ? C64 C56 C63 66(9) 2_756 2_756 ? C55 C56 C63 141.6(13) . 2_756 ? C57 C56 C63 21.6(13) . 2_756 ? C64 C56 C65 28(7) 2_756 2_756 ? C55 C56 C65 47.2(19) . 2_756 ? C57 C56 C65 73.0(19) . 2_756 ? C63 C56 C65 95(3) 2_756 2_756 ? C63 C57 C64 107(8) 2_756 2_756 ? C63 C57 C62 87(8) 2_756 2_756 ? C64 C57 C62 166(4) 2_756 2_756 ? C63 C57 C58 149(8) 2_756 . ? C64 C57 C58 104.1(14) 2_756 . ? C62 C57 C58 61.9(17) 2_756 . ? C63 C57 C56 91(8) 2_756 . ? C64 C57 C56 16.1(17) 2_756 . ? C62 C57 C56 178.0(17) 2_756 . ? C58 C57 C56 120.0 . . ? C63 C57 C65 154(9) 2_756 2_756 ? C64 C57 C65 46.5(16) 2_756 2_756 ? C62 C57 C65 119(2) 2_756 2_756 ? C58 C57 C65 57.6(13) . 2_756 ? C56 C57 C65 62.6(13) . 2_756 ? C63 C57 C61 130(9) 2_756 2_756 ? C64 C57 C61 122(2) 2_756 2_756 ? C62 C57 C61 43.3(15) 2_756 2_756 ? C58 C57 C61 18.8(13) . 2_756 ? C56 C57 C61 138.5(14) . 2_756 ? C65 C57 C61 75.9(11) 2_756 2_756 ? C61 C58 N5 96(3) 2_756 2_756 ? C61 C58 C62 73(3) 2_756 2_756 ? N5 C58 C62 166(5) 2_756 2_756 ? C61 C58 C57 128(3) 2_756 . ? N5 C58 C57 133.6(15) 2_756 . ? C62 C58 C57 56(3) 2_756 . ? C61 C58 N4 111(3) 2_756 . ? N5 C58 N4 17.0(16) 2_756 . ? C62 C58 N4 176(3) 2_756 . ? C57 C58 N4 120.0 . . ? C61 C58 C65 152(5) 2_756 2_756 ? N5 C58 C65 57.1(14) 2_756 2_756 ? C62 C58 C65 133(3) 2_756 2_756 ? C57 C58 C65 76.9(10) . 2_756 ? N4 C58 C65 43.4(9) . 2_756 ? C61 C58 C63 120(3) 2_756 2_756 ? N5 C58 C63 142(3) 2_756 2_756 ? C62 C58 C63 47.3(10) 2_756 2_756 ? C57 C58 C63 9(2) . 2_756 ? N4 C58 C63 129(2) . 2_756 ? C65 C58 C63 86(2) 2_756 2_756 ? C61 C58 C64 160(4) 2_756 2_756 ? N5 C58 C64 101(2) 2_756 2_756 ? C62 C58 C64 89.2(18) 2_756 2_756 ? C57 C58 C64 33.2(16) . 2_756 ? N4 C58 C64 86.8(16) . 2_756 ? C65 C58 C64 43.7(13) 2_756 2_756 ? C63 C58 C64 42.0(10) 2_756 2_756 ? C60 C59 N4 83(5) 2_756 . ? C60 C59 C60 95(10) 2_756 . ? N4 C59 C60 97.6(19) . . ? C60 C59 C59 83(10) 2_756 2_756 ? N4 C59 C59 96(2) . 2_756 ? C60 C59 C59 12(2) . 2_756 ? C60 C59 N5 65(4) 2_756 2_756 ? N4 C59 N5 18.4(13) . 2_756 ? C60 C59 N5 104.2(18) . 2_756 ? C59 C59 N5 99(3) 2_756 2_756 ? N4 N5 C58 125(7) 2_756 2_756 ? N4 N5 C65 51(3) 2_756 . ? C58 N5 C65 84(5) 2_756 . ? N4 N5 C61 155(4) 2_756 . ? C58 N5 C61 36(5) 2_756 . ? C65 N5 C61 120.0 . . ? N4 N5 C60 80(3) 2_756 . ? C58 N5 C60 150(5) 2_756 . ? C65 N5 C60 126.3(18) . . ? C61 N5 C60 113.6(18) . . ? N4 N5 C59 69(3) 2_756 2_756 ? C58 N5 C59 161(5) 2_756 2_756 ? C65 N5 C59 114.5(19) . 2_756 ? C61 N5 C59 125.4(19) . 2_756 ? C60 N5 C59 12(2) . 2_756 ? N4 N5 C54 25(3) 2_756 2_756 ? C58 N5 C54 111(4) 2_756 2_756 ? C65 N5 C54 28.7(16) . 2_756 ? C61 N5 C54 148(2) . 2_756 ? C60 N5 C54 99(2) . 2_756 ? C59 N5 C54 87(2) 2_756 2_756 ? C54 C65 N4 85(2) 2_756 2_756 ? C54 C65 C55 75(6) 2_756 2_756 ? N4 C65 C55 157(6) 2_756 2_756 ? C54 C65 C64 135(4) 2_756 . ? N4 C65 C64 136.9(14) 2_756 . ? C55 C65 C64 60(4) 2_756 . ? C54 C65 N5 104(3) 2_756 . ? N4 C65 N5 19.9(15) 2_756 . ? C55 C65 N5 175(5) 2_756 . ? C64 C65 N5 120.0 . . ? C54 C65 C58 140(4) 2_756 2_756 ? N4 C65 C58 56.3(14) 2_756 2_756 ? C55 C65 C58 140(5) 2_756 2_756 ? C64 C65 C58 81.3(11) . 2_756 ? N5 C65 C58 38.9(13) . 2_756 ? C54 C65 C56 126(7) 2_756 2_756 ? N4 C65 C56 145(5) 2_756 2_756 ? C55 C65 C56 51.3(13) 2_756 2_756 ? C64 C65 C56 9(4) . 2_756 ? N5 C65 C56 129(4) . 2_756 ? C58 C65 C56 90(4) 2_756 2_756 ? C54 C65 C57 165(10) 2_756 2_756 ? N4 C65 C57 102(4) 2_756 2_756 ? C55 C65 C57 96(3) 2_756 2_756 ? C64 C65 C57 36(3) . 2_756 ? N5 C65 C57 84(3) . 2_756 ? C58 C65 C57 45(2) 2_756 2_756 ? C56 C65 C57 44.4(16) 2_756 2_756 ? C56 C64 C57 119(10) 2_756 2_756 ? C56 C64 C55 86(10) 2_756 2_756 ? C57 C64 C55 154(2) 2_756 2_756 ? C56 C64 C63 97(10) 2_756 . ? C57 C64 C63 22.4(14) 2_756 . ? C55 C64 C63 174(4) 2_756 . ? C56 C64 C65 143(10) 2_756 . ? C57 C64 C65 97.7(16) 2_756 . ? C55 C64 C65 57.0(18) 2_756 . ? C63 C64 C65 120.0 . . ? C56 C64 C58 161(10) 2_756 2_756 ? C57 C64 C58 43(2) 2_756 2_756 ? C55 C64 C58 111(2) 2_756 2_756 ? C63 C64 C58 65.1(18) . 2_756 ? C65 C64 C58 55.0(19) . 2_756 ? C57 C63 C64 50(10) 2_756 . ? C57 C63 C62 70(10) 2_756 . ? C64 C63 C62 120.0 . . ? C57 C63 C56 67(10) 2_756 2_756 ? C64 C63 C56 16.9(16) . 2_756 ? C62 C63 C56 136.8(13) . 2_756 ? C57 C63 C58 22(9) 2_756 2_756 ? C64 C63 C58 73(3) . 2_756 ? C62 C63 C58 47(3) . 2_756 ? C56 C63 C58 90(3) 2_756 2_756 ? C57 C62 C58 62(4) 2_756 2_756 ? C57 C62 C63 23.4(17) 2_756 . ? C58 C62 C63 86(3) 2_756 . ? C57 C62 C61 96.6(18) 2_756 . ? C58 C62 C61 35(3) 2_756 . ? C63 C62 C61 120.0 . . ? C58 C61 C62 72(3) 2_756 . ? C58 C61 N5 48(4) 2_756 . ? C62 C61 N5 120.0 . . ? C58 C61 N4 44(3) 2_756 2_756 ? C62 C61 N4 116.8(8) . 2_756 ? N5 C61 N4 6.5(12) . 2_756 ? C58 C61 C57 32.8(14) 2_756 2_756 ? C62 C61 C57 40(3) . 2_756 ? N5 C61 C57 80(3) . 2_756 ? N4 C61 C57 77(3) 2_756 2_756 ? C59 C60 N5 103(6) 2_756 . ? C59 C60 N4 84(5) 2_756 2_756 ? N5 C60 N4 19.5(12) . 2_756 ? C59 C60 C59 85(10) 2_756 . ? N5 C60 C59 104.2(18) . . ? N4 C60 C59 96.5(19) 2_756 . ? C59 C60 C60 73(10) 2_756 2_756 ? N5 C60 C60 106(2) . 2_756 ? N4 C60 C60 95(2) 2_756 2_756 ? C59 C60 C60 12(2) . 2_756 ? 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 C2 C3 179.0(5) . . . . ? C6 C1 C2 C3 -2.0(9) . . . . ? O1 C1 C2 C35 -2.5(9) . . . . ? C6 C1 C2 C35 176.5(5) . . . . ? C1 C2 C3 C4 0.4(9) . . . . ? C35 C2 C3 C4 -178.0(6) . . . . ? C2 C3 C4 C5 0.2(10) . . . . ? C2 C3 C4 S1 -178.7(5) . . . . ? O2 S1 C4 C5 167.1(8) . . . . ? O4 S1 C4 C5 45.3(7) . . . . ? O3 S1 C4 C5 -72.4(9) . . . . ? O2 S1 C4 C3 -13.9(8) . . . . ? O4 S1 C4 C3 -135.8(6) . . . . ? O3 S1 C4 C3 106.5(9) . . . . ? C3 C4 C5 C6 0.8(10) . . . . ? S1 C4 C5 C6 179.7(5) . . . . ? C4 C5 C6 C1 -2.2(10) . . . . ? C4 C5 C6 C7 178.0(6) . . . . ? O1 C1 C6 C5 -178.1(6) . . . . ? C2 C1 C6 C5 2.9(9) . . . . ? O1 C1 C6 C7 1.6(8) . . . . ? C2 C1 C6 C7 -177.4(6) . . . . ? C5 C6 C7 C8 94.0(7) . . . . ? C1 C6 C7 C8 -85.7(7) . . . . ? C6 C7 C8 C9 -38.7(8) . . . . ? C6 C7 C8 C13 144.2(6) . . . . ? C13 C8 C9 C10 -3.6(9) . . . . ? C7 C8 C9 C10 179.3(6) . . . . ? C8 C9 C10 C11 1.6(9) . . . . ? C8 C9 C10 S2 179.6(5) . . . . ? O6 S2 C10 C9 -14.4(13) . . . . ? O8 S2 C10 C9 108.4(8) . . . . ? O7 S2 C10 C9 -143.5(7) . . . . ? O6 S2 C10 C11 163.6(12) . . . . ? O8 S2 C10 C11 -73.6(8) . . . . ? O7 S2 C10 C11 34.5(8) . . . . ? C9 C10 C11 C12 0.4(9) . . . . ? S2 C10 C11 C12 -177.6(5) . . . . ? C10 C11 C12 C13 -0.3(9) . . . . ? C10 C11 C12 C14 177.2(5) . . . . ? C9 C8 C13 O5 -177.5(6) . . . . ? C7 C8 C13 O5 -0.4(9) . . . . ? C9 C8 C13 C12 3.7(9) . . . . ? C7 C8 C13 C12 -179.1(6) . . . . ? C11 C12 C13 O5 179.4(6) . . . . ? C14 C12 C13 O5 1.8(9) . . . . ? C11 C12 C13 C8 -1.8(10) . . . . ? C14 C12 C13 C8 -179.4(6) . . . . ? C11 C12 C14 C15 80.8(9) . . . . ? C13 C12 C14 C15 -101.7(8) . . . . ? C12 C14 C15 C16 -139.3(7) . . . . ? C12 C14 C15 C20 47.7(10) . . . . ? C20 C15 C16 C17 0.0(10) . . . . ? C14 C15 C16 C17 -173.4(7) . . . . ? C15 C16 C17 C18 -0.3(10) . . . . ? C15 C16 C17 S3 177.8(5) . . . . ? O11 S3 C17 C16 -113.4(9) . . . . ? O12 S3 C17 C16 124.0(9) . . . . ? O10 S3 C17 C16 8.6(9) . . . . ? O11 S3 C17 C18 64.9(9) . . . . ? O12 S3 C17 C18 -57.8(10) . . . . ? O10 S3 C17 C18 -173.2(8) . . . . ? C16 C17 C18 C19 -0.5(10) . . . . ? S3 C17 C18 C19 -178.8(5) . . . . ? C17 C18 C19 C20 1.7(9) . . . . ? C17 C18 C19 C21 179.4(6) . . . . ? C18 C19 C20 O9 178.9(6) . . . . ? C21 C19 C20 O9 1.2(9) . . . . ? C18 C19 C20 C15 -2.1(9) . . . . ? C21 C19 C20 C15 -179.8(6) . . . . ? C16 C15 C20 O9 -179.8(6) . . . . ? C14 C15 C20 O9 -6.7(10) . . . . ? C16 C15 C20 C19 1.3(9) . . . . ? C14 C15 C20 C19 174.4(6) . . . . ? C18 C19 C21 C22 99.8(7) . . . . ? C20 C19 C21 C22 -82.5(8) . . . . ? C19 C21 C22 C27 131.5(6) . . . . ? C19 C21 C22 C23 -50.9(8) . . . . ? C27 C22 C23 C24 0.8(9) . . . . ? C21 C22 C23 C24 -177.0(6) . . . . ? C22 C23 C24 C25 0.7(9) . . . . ? C22 C23 C24 S4 -178.7(5) . . . . ? O15 S4 C24 C23 -8.6(7) . . . . ? O16 S4 C24 C23 -128.4(7) . . . . ? O14 S4 C24 C23 110.9(7) . . . . ? O15 S4 C24 C25 172.1(6) . . . . ? O16 S4 C24 C25 52.2(7) . . . . ? O14 S4 C24 C25 -68.5(7) . . . . ? C23 C24 C25 C26 -1.4(9) . . . . ? S4 C24 C25 C26 178.0(4) . . . . ? C24 C25 C26 C27 0.6(8) . . . . ? C24 C25 C26 C28 176.2(5) . . . . ? C23 C22 C27 O13 -179.5(5) . . . . ? C21 C22 C27 O13 -1.8(9) . . . . ? C23 C22 C27 C26 -1.5(9) . . . . ? C21 C22 C27 C26 176.1(6) . . . . ? C25 C26 C27 O13 178.9(5) . . . . ? C28 C26 C27 O13 3.2(8) . . . . ? C25 C26 C27 C22 0.9(9) . . . . ? C28 C26 C27 C22 -174.8(5) . . . . ? C25 C26 C28 C29 91.3(7) . . . . ? C27 C26 C28 C29 -93.1(7) . . . . ? C26 C28 C29 C34 89.4(7) . . . . ? C26 C28 C29 C30 -94.6(6) . . . . ? C34 C29 C30 C31 1.2(8) . . . . ? C28 C29 C30 C31 -175.1(5) . . . . ? C29 C30 C31 C32 0.0(9) . . . . ? C29 C30 C31 S5 -179.1(4) . . . . ? O19 S5 C31 C30 -34.2(6) . . . . ? O20 S5 C31 C30 -155.0(6) . . . . ? O18 S5 C31 C30 85.7(7) . . . . ? O19 S5 C31 C32 146.7(6) . . . . ? O20 S5 C31 C32 25.9(7) . . . . ? O18 S5 C31 C32 -93.3(7) . . . . ? C30 C31 C32 C33 1.3(9) . . . . ? S5 C31 C32 C33 -179.7(5) . . . . ? C31 C32 C33 C34 -3.6(9) . . . . ? C31 C32 C33 C35 176.4(5) . . . . ? C32 C33 C34 O17 -177.4(5) . . . . ? C35 C33 C34 O17 2.6(9) . . . . ? C32 C33 C34 C29 4.9(9) . . . . ? C35 C33 C34 C29 -175.2(5) . . . . ? C30 C29 C34 O17 178.8(5) . . . . ? C28 C29 C34 O17 -5.1(9) . . . . ? C30 C29 C34 C33 -3.6(8) . . . . ? C28 C29 C34 C33 172.5(5) . . . . ? C3 C2 C35 C33 -101.1(7) . . . . ? C1 C2 C35 C33 80.5(7) . . . . ? C32 C33 C35 C2 76.5(7) . . . . ? C34 C33 C35 C2 -103.5(7) . . . . ? C40 N1 C36 C37 -1.0(10) . . . . ? C41 N1 C36 C37 176.9(6) . . . . ? N1 C36 C37 C38 0.3(11) . . . . ? C36 C37 C38 C39 0.9(11) . . . . ? C37 C38 C39 C40 -1.3(11) . . . . ? C36 N1 C40 C39 0.5(10) . . . . ? C41 N1 C40 C39 -177.4(6) . . . . ? C38 C39 C40 N1 0.7(11) . . . . ? C40 N1 C41 C42 88.2(8) . . . . ? C36 N1 C41 C42 -89.7(8) . . . . ? C47 N2 C42 C41 73.4(9) . . . . ? C43 N2 C42 C41 -109.7(8) . . . . ? N1 C41 C42 N2 176.4(6) . . . . ? C47 N2 C43 C44 -2.0(11) . . . . ? C42 N2 C43 C44 -178.9(6) . . . . ? N2 C43 C44 C45 1.4(12) . . . . ? C43 C44 C45 C46 0.2(15) . . . . ? C44 C45 C46 C47 -1.2(16) . . . . ? C43 N2 C47 C46 1.0(12) . . . . ? C42 N2 C47 C46 177.9(7) . . . . ? C45 C46 C47 N2 0.6(14) . . . . ? C52 N3 C48 C49 0.5(18) . . . . ? C53 N3 C48 C49 -177.4(9) . . . . ? N3 C48 C49 C50 2.3(19) . . . . ? C48 C49 C50 C51 -5(2) . . . . ? C49 C50 C51 C52 5(2) . . . . ? C50 C51 C52 N3 -3(2) . . . . ? C48 N3 C52 C51 0(2) . . . . ? C53 N3 C52 C51 177.6(12) . . . . ? C52 N3 C53 C53 -78.9(18) . . . 2_675 ? C48 N3 C53 C53 98.9(17) . . . 2_675 ? N5 N4 C54 C65 27(5) 2_756 . . 2_756 ? C58 N4 C54 C65 -11(6) . . . 2_756 ? C60 N4 C54 C65 154(8) 2_756 . . 2_756 ? C59 N4 C54 C65 156(7) . . . 2_756 ? C61 N4 C54 C65 -5(3) 2_756 . . 2_756 ? N5 N4 C54 C55 38(7) 2_756 . . . ? C65 N4 C54 C55 11(6) 2_756 . . . ? C58 N4 C54 C55 0.0 . . . . ? C60 N4 C54 C55 165(3) 2_756 . . . ? C59 N4 C54 C55 167(3) . . . . ? C61 N4 C54 C55 6(4) 2_756 . . . ? C65 N4 C54 N5 -27(5) 2_756 . . 2_756 ? C58 N4 C54 N5 -38(7) . . . 2_756 ? C60 N4 C54 N5 127(9) 2_756 . . 2_756 ? C59 N4 C54 N5 129(9) . . . 2_756 ? C61 N4 C54 N5 -32(4) 2_756 . . 2_756 ? N4 C54 C55 C65 -10(5) . . . 2_756 ? N5 C54 C55 C65 -4(4) 2_756 . . 2_756 ? C65 C54 C55 C64 8(2) 2_756 . . 2_756 ? N4 C54 C55 C64 -2(3) . . . 2_756 ? N5 C54 C55 C64 4(3) 2_756 . . 2_756 ? C65 C54 C55 C56 10(5) 2_756 . . . ? N4 C54 C55 C56 0.0 . . . . ? N5 C54 C55 C56 5.8(13) 2_756 . . . ? C65 C55 C56 C64 -1(7) 2_756 . . 2_756 ? C54 C55 C56 C64 -7(10) . . . 2_756 ? C65 C55 C56 C57 6(3) 2_756 . . . ? C64 C55 C56 C57 7(10) 2_756 . . . ? C54 C55 C56 C57 0.0 . . . . ? C65 C55 C56 C63 7(2) 2_756 . . 2_756 ? C64 C55 C56 C63 8(5) 2_756 . . 2_756 ? C54 C55 C56 C63 1(5) . . . 2_756 ? C64 C55 C56 C65 1(7) 2_756 . . 2_756 ? C54 C55 C56 C65 -6(3) . . . 2_756 ? C64 C56 C57 C63 -172(22) 2_756 . . 2_756 ? C55 C56 C57 C63 179(9) . . . 2_756 ? C65 C56 C57 C63 -176(11) 2_756 . . 2_756 ? C55 C56 C57 C64 -9(14) . . . 2_756 ? C63 C56 C57 C64 172(22) 2_756 . . 2_756 ? C65 C56 C57 C64 -5(12) 2_756 . . 2_756 ? C64 C56 C57 C62 -149(100) 2_756 . . 2_756 ? C55 C56 C57 C62 -159(100) . . . 2_756 ? C63 C56 C57 C62 22(100) 2_756 . . 2_756 ? C65 C56 C57 C62 -154(100) 2_756 . . 2_756 ? C64 C56 C57 C58 9(14) 2_756 . . . ? C55 C56 C57 C58 0.0 . . . . ? C63 C56 C57 C58 -179(9) 2_756 . . . ? C65 C56 C57 C58 5(2) 2_756 . . . ? C64 C56 C57 C65 5(11) 2_756 . . 2_756 ? C55 C56 C57 C65 -5(2) . . . 2_756 ? C63 C56 C57 C65 176(11) 2_756 . . 2_756 ? C64 C56 C57 C61 5(11) 2_756 . . 2_756 ? C55 C56 C57 C61 -5(4) . . . 2_756 ? C63 C56 C57 C61 177(12) 2_756 . . 2_756 ? C65 C56 C57 C61 0.2(17) 2_756 . . 2_756 ? C63 C57 C58 C61 12(11) 2_756 . . 2_756 ? C64 C57 C58 C61 -168(11) 2_756 . . 2_756 ? C62 C57 C58 C61 9(3) 2_756 . . 2_756 ? C56 C57 C58 C61 -171(7) . . . 2_756 ? C65 C57 C58 C61 -165(10) 2_756 . . 2_756 ? C63 C57 C58 N5 169(19) 2_756 . . 2_756 ? C64 C57 C58 N5 -10(3) 2_756 . . 2_756 ? C62 C57 C58 N5 166(7) 2_756 . . 2_756 ? C56 C57 C58 N5 -13(3) . . . 2_756 ? C65 C57 C58 N5 -7.9(19) 2_756 . . 2_756 ? C61 C57 C58 N5 158(10) 2_756 . . 2_756 ? C63 C57 C58 C62 3(13) 2_756 . . 2_756 ? C64 C57 C58 C62 -176(8) 2_756 . . 2_756 ? C56 C57 C58 C62 -179(4) . . . 2_756 ? C65 C57 C58 C62 -174(7) 2_756 . . 2_756 ? C61 C57 C58 C62 -9(3) 2_756 . . 2_756 ? C63 C57 C58 N4 -178(17) 2_756 . . . ? C64 C57 C58 N4 3(4) 2_756 . . . ? C62 C57 C58 N4 179(4) 2_756 . . . ? C56 C57 C58 N4 0.0 . . . . ? C65 C57 C58 N4 5(3) 2_756 . . . ? C61 C57 C58 N4 171(7) 2_756 . . . ? C63 C57 C58 C65 177(19) 2_756 . . 2_756 ? C64 C57 C58 C65 -2.4(17) 2_756 . . 2_756 ? C62 C57 C58 C65 174(7) 2_756 . . 2_756 ? C56 C57 C58 C65 -5(3) . . . 2_756 ? C61 C57 C58 C65 165(10) 2_756 . . 2_756 ? C64 C57 C58 C63 -180(100) 2_756 . . 2_756 ? C62 C57 C58 C63 -3(13) 2_756 . . 2_756 ? C56 C57 C58 C63 178(17) . . . 2_756 ? C65 C57 C58 C63 -177(19) 2_756 . . 2_756 ? C61 C57 C58 C63 -12(11) 2_756 . . 2_756 ? C63 C57 C58 C64 180(100) 2_756 . . 2_756 ? C62 C57 C58 C64 176(8) 2_756 . . 2_756 ? C56 C57 C58 C64 -3(4) . . . 2_756 ? C65 C57 C58 C64 2.4(17) 2_756 . . 2_756 ? C61 C57 C58 C64 168(11) 2_756 . . 2_756 ? N5 N4 C58 C61 26(4) 2_756 . . 2_756 ? C65 N4 C58 C61 165(10) 2_756 . . 2_756 ? C54 N4 C58 C61 172(6) . . . 2_756 ? C60 N4 C58 C61 6(5) 2_756 . . 2_756 ? C59 N4 C58 C61 8(5) . . . 2_756 ? C65 N4 C58 N5 139(10) 2_756 . . 2_756 ? C54 N4 C58 N5 146(7) . . . 2_756 ? C60 N4 C58 N5 -20(5) 2_756 . . 2_756 ? C59 N4 C58 N5 -18(5) . . . 2_756 ? C61 N4 C58 N5 -26(4) 2_756 . . 2_756 ? N5 N4 C58 C62 -137(57) 2_756 . . 2_756 ? C65 N4 C58 C62 3(49) 2_756 . . 2_756 ? C54 N4 C58 C62 10(52) . . . 2_756 ? C60 N4 C58 C62 -156(53) 2_756 . . 2_756 ? C59 N4 C58 C62 -154(54) . . . 2_756 ? C61 N4 C58 C62 -162(58) 2_756 . . 2_756 ? N5 N4 C58 C57 -146(7) 2_756 . . . ? C65 N4 C58 C57 -7(4) 2_756 . . . ? C54 N4 C58 C57 0.0 . . . . ? C60 N4 C58 C57 -166(3) 2_756 . . . ? C59 N4 C58 C57 -164(3) . . . . ? C61 N4 C58 C57 -172(6) 2_756 . . . ? N5 N4 C58 C65 -139(10) 2_756 . . 2_756 ? C54 N4 C58 C65 7(4) . . . 2_756 ? C60 N4 C58 C65 -159(6) 2_756 . . 2_756 ? C59 N4 C58 C65 -157(6) . . . 2_756 ? C61 N4 C58 C65 -165(10) 2_756 . . 2_756 ? N5 N4 C58 C63 -147(9) 2_756 . . 2_756 ? C65 N4 C58 C63 -7.6(15) 2_756 . . 2_756 ? C54 N4 C58 C63 0(3) . . . 2_756 ? C60 N4 C58 C63 -166(5) 2_756 . . 2_756 ? C59 N4 C58 C63 -164(5) . . . 2_756 ? C61 N4 C58 C63 -173(9) 2_756 . . 2_756 ? N5 N4 C58 C64 -145(9) 2_756 . . 2_756 ? C65 N4 C58 C64 -5.7(17) 2_756 . . 2_756 ? C54 N4 C58 C64 1(2) . . . 2_756 ? C60 N4 C58 C64 -164(4) 2_756 . . 2_756 ? C59 N4 C58 C64 -162(4) . . . 2_756 ? C61 N4 C58 C64 -171(8) 2_756 . . 2_756 ? N5 N4 C59 C60 -19(13) 2_756 . . 2_756 ? C65 N4 C59 C60 -146(13) 2_756 . . 2_756 ? C54 N4 C59 C60 -173(12) . . . 2_756 ? C58 N4 C59 C60 -8(14) . . . 2_756 ? C61 N4 C59 C60 -5(13) 2_756 . . 2_756 ? N5 N4 C59 C60 -113(5) 2_756 . . . ? C65 N4 C59 C60 120(8) 2_756 . . . ? C54 N4 C59 C60 93(2) . . . . ? C58 N4 C59 C60 -102(3) . . . . ? C60 N4 C59 C60 -94(12) 2_756 . . . ? C61 N4 C59 C60 -99(3) 2_756 . . . ? N5 N4 C59 C59 -100(5) 2_756 . . 2_756 ? C65 N4 C59 C59 132(8) 2_756 . . 2_756 ? C54 N4 C59 C59 105(3) . . . 2_756 ? C58 N4 C59 C59 -90(4) . . . 2_756 ? C60 N4 C59 C59 -82(12) 2_756 . . 2_756 ? C61 N4 C59 C59 -86(4) 2_756 . . 2_756 ? C65 N4 C59 N5 -127(11) 2_756 . . 2_756 ? C54 N4 C59 N5 -155(5) . . . 2_756 ? C58 N4 C59 N5 11(3) . . . 2_756 ? C60 N4 C59 N5 19(13) 2_756 . . 2_756 ? C61 N4 C59 N5 14(2) 2_756 . . 2_756 ? N4 N5 C65 C54 -16(4) 2_756 . . 2_756 ? C58 N5 C65 C54 -162(12) 2_756 . . 2_756 ? C61 N5 C65 C54 -167(7) . . . 2_756 ? C60 N5 C65 C54 16(6) . . . 2_756 ? C59 N5 C65 C54 15(6) 2_756 . . 2_756 ? C58 N5 C65 N4 -146(10) 2_756 . . 2_756 ? C61 N5 C65 N4 -152(6) . . . 2_756 ? C60 N5 C65 N4 31(5) . . . 2_756 ? C59 N5 C65 N4 30(5) 2_756 . . 2_756 ? C54 N5 C65 N4 16(4) 2_756 . . 2_756 ? N4 N5 C65 C55 64(49) 2_756 . . 2_756 ? C58 N5 C65 C55 -82(51) 2_756 . . 2_756 ? C61 N5 C65 C55 -88(50) . . . 2_756 ? C60 N5 C65 C55 95(50) . . . 2_756 ? C59 N5 C65 C55 94(50) 2_756 . . 2_756 ? C54 N5 C65 C55 80(49) 2_756 . . 2_756 ? N4 N5 C65 C64 152(6) 2_756 . . . ? C58 N5 C65 C64 6(5) 2_756 . . . ? C61 N5 C65 C64 0.0 . . . . ? C60 N5 C65 C64 -177(2) . . . . ? C59 N5 C65 C64 -178(2) 2_756 . . . ? C54 N5 C65 C64 167(7) 2_756 . . . ? N4 N5 C65 C58 146(10) 2_756 . . 2_756 ? C61 N5 C65 C58 -6(5) . . . 2_756 ? C60 N5 C65 C58 177(7) . . . 2_756 ? C59 N5 C65 C58 176(7) 2_756 . . 2_756 ? C54 N5 C65 C58 162(12) 2_756 . . 2_756 ? N4 N5 C65 C56 150(10) 2_756 . . 2_756 ? C58 N5 C65 C56 4.3(14) 2_756 . . 2_756 ? C61 N5 C65 C56 -1(5) . . . 2_756 ? C60 N5 C65 C56 -178(6) . . . 2_756 ? C59 N5 C65 C56 -179(6) 2_756 . . 2_756 ? C54 N5 C65 C56 166(12) 2_756 . . 2_756 ? N4 N5 C65 C57 151(8) 2_756 . . 2_756 ? C58 N5 C65 C57 5(2) 2_756 . . 2_756 ? C61 N5 C65 C57 -1(3) . . . 2_756 ? C60 N5 C65 C57 -178(5) . . . 2_756 ? C59 N5 C65 C57 -179(5) 2_756 . . 2_756 ? C54 N5 C65 C57 167(10) 2_756 . . 2_756 ? C54 C65 C64 C56 -10(18) 2_756 . . 2_756 ? N4 C65 C64 C56 -159(29) 2_756 . . 2_756 ? C55 C65 C64 C56 1(21) 2_756 . . 2_756 ? N5 C65 C64 C56 -173(27) . . . 2_756 ? C58 C65 C64 C56 -169(30) 2_756 . . 2_756 ? C57 C65 C64 C56 -172(33) 2_756 . . 2_756 ? C54 C65 C64 C57 161(15) 2_756 . . 2_756 ? N4 C65 C64 C57 12(4) 2_756 . . 2_756 ? C55 C65 C64 C57 173(12) 2_756 . . 2_756 ? N5 C65 C64 C57 -1(6) . . . 2_756 ? C58 C65 C64 C57 2(2) 2_756 . . 2_756 ? C56 C65 C64 C57 172(33) 2_756 . . 2_756 ? C54 C65 C64 C55 -11(3) 2_756 . . 2_756 ? N4 C65 C64 C55 -161(9) 2_756 . . 2_756 ? N5 C65 C64 C55 -174(6) . . . 2_756 ? C58 C65 C64 C55 -171(10) 2_756 . . 2_756 ? C56 C65 C64 C55 -1(21) 2_756 . . 2_756 ? C57 C65 C64 C55 -173(12) 2_756 . . 2_756 ? C54 C65 C64 C63 163(9) 2_756 . . . ? N4 C65 C64 C63 14(3) 2_756 . . . ? C55 C65 C64 C63 174(6) 2_756 . . . ? N5 C65 C64 C63 0.0 . . . . ? C58 C65 C64 C63 4(4) 2_756 . . . ? C56 C65 C64 C63 173(27) 2_756 . . . ? C57 C65 C64 C63 1(6) 2_756 . . . ? C54 C65 C64 C58 159(12) 2_756 . . 2_756 ? N4 C65 C64 C58 10.0(19) 2_756 . . 2_756 ? C55 C65 C64 C58 171(10) 2_756 . . 2_756 ? N5 C65 C64 C58 -4(4) . . . 2_756 ? C56 C65 C64 C58 169(30) 2_756 . . 2_756 ? C57 C65 C64 C58 -2(2) 2_756 . . 2_756 ? C56 C64 C63 C57 172(32) 2_756 . . 2_756 ? C55 C64 C63 C57 54(23) 2_756 . . 2_756 ? C65 C64 C63 C57 -3(16) . . . 2_756 ? C58 C64 C63 C57 0(12) 2_756 . . 2_756 ? C56 C64 C63 C62 176(16) 2_756 . . . ? C57 C64 C63 C62 3(16) 2_756 . . . ? C55 C64 C63 C62 58(37) 2_756 . . . ? C65 C64 C63 C62 0.0 . . . . ? C58 C64 C63 C62 3(3) 2_756 . . . ? C57 C64 C63 C56 -172(32) 2_756 . . 2_756 ? C55 C64 C63 C56 -118(52) 2_756 . . 2_756 ? C65 C64 C63 C56 -176(16) . . . 2_756 ? C58 C64 C63 C56 -173(19) 2_756 . . 2_756 ? C56 C64 C63 C58 173(19) 2_756 . . 2_756 ? C57 C64 C63 C58 0(12) 2_756 . . 2_756 ? C55 C64 C63 C58 54(34) 2_756 . . 2_756 ? C65 C64 C63 C58 -3(3) . . . 2_756 ? C64 C63 C62 C57 -3(13) . . . 2_756 ? C56 C63 C62 C57 -1(6) 2_756 . . 2_756 ? C58 C63 C62 C57 1(9) 2_756 . . 2_756 ? C57 C63 C62 C58 -1(9) 2_756 . . 2_756 ? C64 C63 C62 C58 -4(4) . . . 2_756 ? C56 C63 C62 C58 -2(3) 2_756 . . 2_756 ? C57 C63 C62 C61 3(13) 2_756 . . . ? C64 C63 C62 C61 0.0 . . . . ? C56 C63 C62 C61 2(7) 2_756 . . . ? C58 C63 C62 C61 4(4) 2_756 . . . ? C57 C62 C61 C58 -6(2) 2_756 . . 2_756 ? C63 C62 C61 C58 -7(7) . . . 2_756 ? C57 C62 C61 N5 1(5) 2_756 . . . ? C58 C62 C61 N5 7(7) 2_756 . . . ? C63 C62 C61 N5 0.0 . . . . ? C57 C62 C61 N4 -5(4) 2_756 . . 2_756 ? C58 C62 C61 N4 1(6) 2_756 . . 2_756 ? C63 C62 C61 N4 -6.4(14) . . . 2_756 ? C58 C62 C61 C57 6(2) 2_756 . . 2_756 ? C63 C62 C61 C57 -1(5) . . . 2_756 ? N4 N5 C61 C58 -53(8) 2_756 . . 2_756 ? C65 N5 C61 C58 10(9) . . . 2_756 ? C60 N5 C61 C58 -173(10) . . . 2_756 ? C59 N5 C61 C58 -173(10) 2_756 . . 2_756 ? C54 N5 C61 C58 -2(4) 2_756 . . 2_756 ? N4 N5 C61 C62 -62(8) 2_756 . . . ? C58 N5 C61 C62 -10(9) 2_756 . . . ? C65 N5 C61 C62 0.0 . . . . ? C60 N5 C61 C62 177(2) . . . . ? C59 N5 C61 C62 178(2) 2_756 . . . ? C54 N5 C61 C62 -11(6) 2_756 . . . ? C58 N5 C61 N4 53(8) 2_756 . . 2_756 ? C65 N5 C61 N4 62(8) . . . 2_756 ? C60 N5 C61 N4 -121(9) . . . 2_756 ? C59 N5 C61 N4 -120(9) 2_756 . . 2_756 ? C54 N5 C61 N4 51(7) 2_756 . . 2_756 ? N4 N5 C61 C57 -61(7) 2_756 . . 2_756 ? C58 N5 C61 C57 -9(6) 2_756 . . 2_756 ? C65 N5 C61 C57 1(3) . . . 2_756 ? C60 N5 C61 C57 178(5) . . . 2_756 ? C59 N5 C61 C57 179(5) 2_756 . . 2_756 ? C54 N5 C61 C57 -11(3) 2_756 . . 2_756 ? N4 N5 C60 C59 19(14) 2_756 . . 2_756 ? C58 N5 C60 C59 170(17) 2_756 . . 2_756 ? C65 N5 C60 C59 -5(14) . . . 2_756 ? C61 N5 C60 C59 178(13) . . . 2_756 ? C54 N5 C60 C59 3(14) 2_756 . . 2_756 ? C58 N5 C60 N4 151(16) 2_756 . . 2_756 ? C65 N5 C60 N4 -24(4) . . . 2_756 ? C61 N5 C60 N4 159(5) . . . 2_756 ? C59 N5 C60 N4 -19(14) 2_756 . . 2_756 ? C54 N5 C60 N4 -17(2) 2_756 . . 2_756 ? N4 N5 C60 C59 -69(5) 2_756 . . . ? C58 N5 C60 C59 82(13) 2_756 . . . ? C65 N5 C60 C59 -93(3) . . . . ? C61 N5 C60 C59 90(2) . . . . ? C59 N5 C60 C59 -88(13) 2_756 . . . ? C54 N5 C60 C59 -86(4) 2_756 . . . ? N4 N5 C60 C60 -57(5) 2_756 . . 2_756 ? C58 N5 C60 C60 94(13) 2_756 . . 2_756 ? C65 N5 C60 C60 -81(4) . . . 2_756 ? C61 N5 C60 C60 102(3) . . . 2_756 ? C59 N5 C60 C60 -76(13) 2_756 . . 2_756 ? C54 N5 C60 C60 -73(5) 2_756 . . 2_756 ? C60 C59 C60 C59 0.01(4) 2_756 . . 2_756 ? N4 C59 C60 C59 83(5) . . . 2_756 ? N5 C59 C60 C59 66(5) 2_756 . . 2_756 ? C60 C59 C60 N5 102(6) 2_756 . . . ? N4 C59 C60 N5 -175(3) . . . . ? C59 C59 C60 N5 102(6) 2_756 . . . ? N5 C59 C60 N5 168(2) 2_756 . . . ? C60 C59 C60 N4 84(6) 2_756 . . 2_756 ? N4 C59 C60 N4 167(3) . . . 2_756 ? C59 C59 C60 N4 84(6) 2_756 . . 2_756 ? N5 C59 C60 N4 150(3) 2_756 . . 2_756 ? N4 C59 C60 C60 83(5) . . . 2_756 ? C59 C59 C60 C60 -0.01(4) 2_756 . . 2_756 ? N5 C59 C60 C60 66(5) 2_756 . . 2_756 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.019 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.139