# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Jolliffe, Katrina A.' 'Young, Philip' 'Bhadbhade, Mohan' 'Clegg, Jack' _publ_contact_author_name 'Jolliffe, Katrina A.' _publ_contact_author_email jolliffe@chem.usyd.edu.au _publ_section_title ; Hybrid Cyclic Peptide-Thiourea Cages for Anion Recognition ; # Attachment '- combined.CIF' data_py34inp1 _database_code_depnum_ccdc_archive 'CCDC 783199' #TrackingRef '- combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C36 H51 N13 O6 S3), 2(C2 H F3 O2), 1.25(H2 O), 3.75(C H4 O) ; _chemical_formula_sum 'C79.75 H121.50 F6 N26 O21 S6' _chemical_formula_weight 2086.89 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' F F 0.0171 0.0103 '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) _symmetry_space_group_name_Hall P2yb _symmetry_Int_tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.302(4) _cell_length_b 15.233(3) _cell_length_c 21.662(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.54(3) _cell_angle_gamma 90.00 _cell_volume 5234.3(22) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5979 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.50 _exptl_crystal_description Plate _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.65256 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron BM' _diffrn_radiation_monochromator Si<111> _diffrn_measurement_device_type '3-BM1 Australian Synchrotron' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 'ADSC Q210' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56007 _diffrn_reflns_av_R_equivalents 0.1995 _diffrn_reflns_av_sigmaI/netI 0.3482 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 21.25 _reflns_number_total 14942 _reflns_number_gt 7088 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BLU-ICE (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.0000P)^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 SHELXL _refine_ls_extinction_coef 0.0087(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(1) _chemical_absolute_configuration syn _refine_ls_number_reflns 14942 _refine_ls_number_parameters 1258 _refine_ls_number_restraints 95 _refine_ls_R_factor_all 0.1770 _refine_ls_R_factor_gt 0.0978 _refine_ls_wR_factor_ref 0.3028 _refine_ls_wR_factor_gt 0.2399 _refine_ls_goodness_of_fit_ref 0.773 _refine_ls_restrained_S_all 0.775 _refine_ls_shift/su_max 0.001 _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 N1A N 0.6025(6) 0.5756(8) 0.9114(6) 0.070(3) Uani 1 1 d DU . . C11A C 0.6025(9) 0.6337(11) 0.9647(7) 0.080(4) Uani 1 1 d . . . H11A H 0.6058 0.6950 0.9509 0.096 Uiso 1 1 calc R . . H11B H 0.6539 0.6220 1.0057 0.096 Uiso 1 1 calc R . . C12A C 0.5244(11) 0.6250(12) 0.9829(8) 0.097(5) Uani 1 1 d . . . H12C H 0.5176 0.5626 0.9925 0.116 Uiso 1 1 calc R . . H12D H 0.5350 0.6589 1.0245 0.116 Uiso 1 1 calc R . . N13A N 0.4466(7) 0.6555(9) 0.9307(6) 0.075(3) Uani 1 1 d . . . H13A H 0.4146 0.6168 0.9016 0.090 Uiso 1 1 calc R . . C14A C 0.4203(9) 0.7390(9) 0.9240(7) 0.067(4) Uani 1 1 d . . . S15A S 0.4753(3) 0.8165(3) 0.9810(2) 0.1177(19) Uani 1 1 d . . . N16A N 0.3480(6) 0.7555(7) 0.8702(5) 0.062(3) Uani 1 1 d . . . H16A H 0.3288 0.7148 0.8389 0.074 Uiso 1 1 calc R . . C17A C 0.2990(8) 0.8374(8) 0.8607(7) 0.062(4) Uani 1 1 d . . . H17A H 0.3346 0.8834 0.8911 0.074 Uiso 1 1 calc R . . H17B H 0.2498 0.8272 0.8722 0.074 Uiso 1 1 calc R . . C18A C 0.2681(7) 0.8692(9) 0.7863(7) 0.063(4) Uani 1 1 d . . . H18A H 0.2414 0.8190 0.7563 0.075 Uiso 1 1 calc R . . H18B H 0.2242 0.9145 0.7784 0.075 Uiso 1 1 calc R . . C19A C 0.3369(8) 0.9070(8) 0.7664(7) 0.065(4) Uani 1 1 d . . . H19A H 0.3556 0.9636 0.7901 0.078 Uiso 1 1 calc R . . H19B H 0.3858 0.8667 0.7830 0.078 Uiso 1 1 calc R . . C21A C 0.6708(8) 0.6024(10) 0.8829(8) 0.080(4) Uani 1 1 d . . . H21A H 0.6614 0.5664 0.8425 0.096 Uiso 1 1 calc R . . H21B H 0.6614 0.6645 0.8684 0.096 Uiso 1 1 calc R . . C22A C 0.7550(10) 0.5926(14) 0.9281(9) 0.106(6) Uani 1 1 d . . . H22C H 0.7680 0.5297 0.9384 0.128 Uiso 1 1 calc R . . H22D H 0.7645 0.6237 0.9707 0.128 Uiso 1 1 calc R . . N23A N 0.8135(8) 0.6316(10) 0.8958(7) 0.097(4) Uani 1 1 d . . . H23A H 0.8372 0.5948 0.8773 0.117 Uiso 1 1 calc R . . C24A C 0.8302(9) 0.7163(10) 0.8944(8) 0.080(5) Uani 1 1 d . . . S25A S 0.8081(3) 0.7929(4) 0.9452(2) 0.1039(15) Uani 1 1 d . . . N26A N 0.8739(8) 0.7380(9) 0.8595(8) 0.103(5) Uani 1 1 d . . . H26A H 0.8965 0.6931 0.8471 0.124 Uiso 1 1 calc R . . C27A C 0.8931(9) 0.8272(13) 0.8361(8) 0.098(6) Uani 1 1 d . . . H71A H 0.8921 0.8726 0.8685 0.117 Uiso 1 1 calc R . . H71B H 0.9510 0.8255 0.8375 0.117 Uiso 1 1 calc R . . C28A C 0.8365(9) 0.8533(11) 0.7699(9) 0.088(5) Uani 1 1 d . . . H28A H 0.8600 0.9070 0.7582 0.105 Uiso 1 1 calc R . . H28B H 0.8376 0.8069 0.7383 0.105 Uiso 1 1 calc R . . C29A C 0.7506(7) 0.8706(11) 0.7565(9) 0.095(6) Uani 1 1 d . . . H29A H 0.7489 0.9190 0.7864 0.114 Uiso 1 1 calc R . . H29B H 0.7272 0.8179 0.7696 0.114 Uiso 1 1 calc R . . C31A C 0.6079(9) 0.4834(10) 0.9293(7) 0.084(4) Uani 1 1 d U . . H31C H 0.5624 0.4708 0.9448 0.100 Uiso 1 1 calc R . . H31D H 0.6621 0.4742 0.9683 0.100 Uiso 1 1 calc R . . C32A C 0.6020(9) 0.4145(9) 0.8755(7) 0.086(5) Uani 1 1 d . . . H32C H 0.6504 0.4223 0.8625 0.103 Uiso 1 1 calc R . . H32D H 0.6063 0.3552 0.8951 0.103 Uiso 1 1 calc R . . N33A N 0.5245(6) 0.4205(7) 0.8157(5) 0.063(3) Uani 1 1 d . . . H33A H 0.4778 0.4334 0.8207 0.076 Uiso 1 1 calc R . . C34A C 0.5198(6) 0.4068(7) 0.7497(6) 0.042(3) Uani 1 1 d . . . S35A S 0.60581(16) 0.3895(2) 0.73209(18) 0.0641(10) Uani 1 1 d . . . N36A N 0.4426(5) 0.4094(5) 0.7021(5) 0.042(2) Uani 1 1 d . . . H36A H 0.4005 0.4094 0.7150 0.051 Uiso 1 1 calc R . . C37A C 0.4218(6) 0.4123(7) 0.6301(6) 0.041(3) Uani 1 1 d . . . H37A H 0.3644 0.3884 0.6056 0.049 Uiso 1 1 calc R . . H37B H 0.4617 0.3747 0.6197 0.049 Uiso 1 1 calc R . . C38A C 0.4255(6) 0.5061(6) 0.6054(6) 0.041(3) Uani 1 1 d . . . H38A H 0.3886 0.5442 0.6190 0.049 Uiso 1 1 calc R . . H38B H 0.4839 0.5283 0.6282 0.049 Uiso 1 1 calc R . . C39A C 0.3988(5) 0.5140(6) 0.5295(6) 0.041(3) Uani 1 1 d . . . H39A H 0.3434 0.4852 0.5061 0.049 Uiso 1 1 calc R . . H39B H 0.4403 0.4830 0.5163 0.049 Uiso 1 1 calc R . . C41A C 0.3131(6) 0.9226(7) 0.6915(6) 0.041(3) Uani 1 1 d . . . H41A H 0.2580 0.9542 0.6706 0.049 Uiso 1 1 calc R . . C42A C 0.3831(6) 0.9732(6) 0.6813(5) 0.040(3) Uani 1 1 d . . . N43A N 0.4536(4) 0.9454(5) 0.6843(4) 0.037(2) Uani 1 1 d . . . C44A C 0.4955(6) 1.0205(6) 0.6723(6) 0.048(3) Uani 1 1 d . . . C45A C 0.4453(6) 1.0893(6) 0.6622(6) 0.048(3) Uani 1 1 d . . . O46A O 0.3719(4) 1.0628(5) 0.6697(4) 0.0479(19) Uani 1 1 d . . . C47A C 0.4527(7) 1.1856(7) 0.6508(7) 0.061(4) Uani 1 1 d . . . H47A H 0.4412 1.2193 0.6847 0.092 Uiso 1 1 calc R . . H47B H 0.4119 1.2017 0.6058 0.092 Uiso 1 1 calc R . . H47C H 0.5099 1.1986 0.6545 0.092 Uiso 1 1 calc R . . C48A C 0.5815(7) 1.0121(7) 0.6724(7) 0.054(3) Uani 1 1 d . . . N49A N 0.6081(5) 0.9283(6) 0.6826(6) 0.066(3) Uani 1 1 d . . . H49A H 0.5748 0.8895 0.6898 0.079 Uiso 1 1 calc R . . O50A O 0.6248(4) 1.0744(5) 0.6676(5) 0.071(3) Uani 1 1 d . . . C51A C 0.6903(7) 0.8953(9) 0.6828(8) 0.069(4) Uani 1 1 d U . . H51A H 0.7169 0.9429 0.6661 0.083 Uiso 1 1 calc R . . C52A C 0.6665(6) 0.8194(7) 0.6330(6) 0.050(3) Uani 1 1 d U . . N53A N 0.5946(5) 0.7793(6) 0.6064(6) 0.063(3) Uani 1 1 d . . . C54A C 0.6087(6) 0.7103(6) 0.5690(7) 0.047(3) Uani 1 1 d . . . C55A C 0.6883(7) 0.7129(7) 0.5709(6) 0.051(3) Uani 1 1 d U . . O56A O 0.7261(4) 0.7857(5) 0.6133(5) 0.072(3) Uani 1 1 d . . . C57A C 0.7408(6) 0.6559(8) 0.5443(7) 0.059(3) Uani 1 1 d . . . H57A H 0.7824 0.6227 0.5816 0.088 Uiso 1 1 calc R . . H57B H 0.7700 0.6933 0.5237 0.088 Uiso 1 1 calc R . . H57C H 0.7037 0.6149 0.5105 0.088 Uiso 1 1 calc R . . C58A C 0.5419(6) 0.6523(7) 0.5302(6) 0.049(3) Uani 1 1 d U . . N59A N 0.4695(4) 0.6609(5) 0.5404(4) 0.040(2) Uani 1 1 d . . . H59A H 0.4697 0.6998 0.5705 0.047 Uiso 1 1 calc R . . O60A O 0.5474(4) 0.5954(5) 0.4884(4) 0.057(2) Uani 1 1 d . . . C61A C 0.3926(5) 0.6121(6) 0.5067(6) 0.036(2) Uani 1 1 d . . . H61A H 0.3763 0.6147 0.4569 0.043 Uiso 1 1 calc R . . C62A C 0.3268(5) 0.6570(7) 0.5237(5) 0.036(2) Uani 1 1 d . . . N63A N 0.3366(4) 0.7139(5) 0.5729(4) 0.034(2) Uani 1 1 d . . . C64A C 0.2555(5) 0.7296(5) 0.5713(5) 0.027(2) Uani 1 1 d . . . C65A C 0.2005(5) 0.6822(6) 0.5204(5) 0.032(2) Uani 1 1 d U . . O66A O 0.2452(3) 0.6351(4) 0.4893(3) 0.0333(16) Uani 1 1 d . . . C67A C 0.1076(5) 0.6757(7) 0.4908(5) 0.034(2) Uani 1 1 d . . . H67A H 0.0906 0.6201 0.5046 0.051 Uiso 1 1 calc R . . H67B H 0.0868 0.6777 0.4416 0.051 Uiso 1 1 calc R . . H67C H 0.0839 0.7248 0.5067 0.051 Uiso 1 1 calc R . . C68A C 0.2398(5) 0.7972(6) 0.6165(5) 0.033(2) Uani 1 1 d . . . N69A N 0.3110(4) 0.8386(5) 0.6564(4) 0.040(2) Uani 1 1 d . . . H69A H 0.3595 0.8142 0.6621 0.048 Uiso 1 1 calc R . . O70A O 0.1705(3) 0.8108(4) 0.6172(3) 0.0336(16) Uani 1 1 d . . . N1B N 0.1092(6) 0.4966(8) 0.9057(5) 0.076(4) Uani 1 1 d D . . C11B C 0.0256(8) 0.5101(11) 0.9135(9) 0.085(5) Uani 1 1 d . . . H11C H 0.0258 0.5699 0.9313 0.102 Uiso 1 1 calc R . . H11D H -0.0207 0.5077 0.8681 0.102 Uiso 1 1 calc R . . C12B C 0.0054(8) 0.4456(12) 0.9584(8) 0.077(4) Uani 1 1 d . . . H12A H 0.0508 0.4500 1.0041 0.092 Uiso 1 1 calc R . . H12B H -0.0473 0.4656 0.9617 0.092 Uiso 1 1 calc R . . N13B N -0.0046(8) 0.3560(12) 0.9402(8) 0.111(5) Uani 1 1 d . . . H13B H 0.0400 0.3246 0.9447 0.133 Uiso 1 1 calc R . . C14B C -0.0814(8) 0.3173(12) 0.9161(8) 0.083(5) Uani 1 1 d . . . S15B S -0.1706(3) 0.3652(4) 0.9054(3) 0.126(2) Uani 1 1 d . . . N16B N -0.0748(8) 0.2263(10) 0.9048(7) 0.091(3) Uani 1 1 d U . . H16C H -0.0239 0.2048 0.9152 0.109 Uiso 1 1 calc R . . C17B C -0.1447(9) 0.1666(12) 0.8778(8) 0.093(4) Uani 1 1 d U . . H17C H -0.1945 0.1942 0.8814 0.111 Uiso 1 1 calc R . . H17D H -0.1311 0.1130 0.9060 0.111 Uiso 1 1 calc R . . C18B C -0.1688(9) 0.1388(11) 0.8036(8) 0.081(4) Uani 1 1 d U . . H18C H -0.1187 0.1120 0.7999 0.097 Uiso 1 1 calc R . . H18D H -0.2128 0.0929 0.7922 0.097 Uiso 1 1 calc R . . C19B C -0.2007(9) 0.2112(8) 0.7519(6) 0.064(4) Uani 1 1 d . . . H19C H -0.1641 0.2634 0.7687 0.077 Uiso 1 1 calc R . . H19D H -0.2583 0.2277 0.7467 0.077 Uiso 1 1 calc R . . C21B C 0.1144(8) 0.5450(9) 0.8459(7) 0.067(4) Uani 1 1 d . . . H21C H 0.1659 0.5254 0.8406 0.081 Uiso 1 1 calc R . . H21D H 0.0655 0.5272 0.8048 0.081 Uiso 1 1 calc R . . C22B C 0.1157(8) 0.6383(10) 0.8495(6) 0.072(4) Uani 1 1 d . . . H22A H 0.1681 0.6576 0.8869 0.086 Uiso 1 1 calc R . . H22B H 0.0674 0.6588 0.8592 0.086 Uiso 1 1 calc R . . N23B N 0.1110(5) 0.6798(6) 0.7844(6) 0.067(3) Uani 1 1 d . . . H23B H 0.1557 0.7059 0.7831 0.080 Uiso 1 1 calc R . . C24B C 0.0366(7) 0.6768(8) 0.7269(7) 0.053(3) Uani 1 1 d . . . S25B S -0.05610(16) 0.6554(2) 0.73154(17) 0.0597(9) Uani 1 1 d . . . N26B N 0.0469(5) 0.6959(5) 0.6689(6) 0.052(3) Uani 1 1 d . . . H26B H 0.0962 0.7159 0.6725 0.062 Uiso 1 1 calc R . . C27B C -0.0201(6) 0.6850(7) 0.6003(6) 0.048(3) Uani 1 1 d . . . H27A H -0.0063 0.7203 0.5677 0.057 Uiso 1 1 calc R . . H27B H -0.0747 0.7057 0.5994 0.057 Uiso 1 1 calc R . . C28B C -0.0266(6) 0.5887(6) 0.5807(6) 0.041(3) Uani 1 1 d . . . H28C H -0.0485 0.5558 0.6097 0.050 Uiso 1 1 calc R . . H28D H 0.0307 0.5664 0.5902 0.050 Uiso 1 1 calc R . . C29B C -0.0830(5) 0.5685(6) 0.5069(5) 0.031(2) Uani 1 1 d . . . H29C H -0.0586 0.5966 0.4776 0.038 Uiso 1 1 calc R . . H29D H -0.1394 0.5945 0.4959 0.038 Uiso 1 1 calc R . . C31B C 0.1849(8) 0.5125(12) 0.9702(8) 0.092(5) Uani 1 1 d . . . H31A H 0.1794 0.4775 1.0066 0.110 Uiso 1 1 calc R . . H31B H 0.1866 0.5753 0.9826 0.110 Uiso 1 1 calc R . . C32B C 0.2663(7) 0.4887(11) 0.9644(8) 0.076(4) Uani 1 1 d . . . H32A H 0.2741 0.5279 0.9309 0.091 Uiso 1 1 calc R . . H32B H 0.3135 0.4995 1.0084 0.091 Uiso 1 1 calc R . . N33B N 0.2704(6) 0.4011(8) 0.9455(7) 0.080(4) Uani 1 1 d . . . H33B H 0.2478 0.3607 0.9621 0.096 Uiso 1 1 calc R . . C34B C 0.3098(8) 0.3719(12) 0.8996(8) 0.081(5) Uani 1 1 d . B . S35B S 0.3557(2) 0.4497(2) 0.86419(18) 0.0753(11) Uani 1 1 d . . . N36B N 0.3060(7) 0.2879(8) 0.8847(6) 0.082(4) Uani 1 1 d D . . H36B H 0.2754 0.2515 0.8971 0.098 Uiso 1 1 calc R A 1 C37B C 0.3542(12) 0.2567(17) 0.8470(9) 0.068(4) Uani 0.50 1 d PD B 1 H37C H 0.3807 0.2003 0.8670 0.082 Uiso 0.50 1 calc PR B 1 H37D H 0.4003 0.2991 0.8541 0.082 Uiso 0.50 1 calc PR B 1 C37C C 0.3204(11) 0.2374(16) 0.8353(10) 0.068(4) Uani 0.50 1 d PD B 2 H37E H 0.3421 0.1781 0.8521 0.082 Uiso 0.50 1 calc PR B 2 H37F H 0.3594 0.2671 0.8189 0.082 Uiso 0.50 1 calc PR B 2 C38B C 0.3064(13) 0.2427(14) 0.7697(9) 0.068(4) Uani 0.50 1 d PD B 1 H38C H 0.2879 0.3006 0.7481 0.082 Uiso 0.50 1 calc PR B 1 H38D H 0.3461 0.2176 0.7519 0.082 Uiso 0.50 1 calc PR B 1 C38C C 0.2294(11) 0.2343(16) 0.7811(11) 0.068(4) Uani 0.50 1 d PD B 2 H38E H 0.1904 0.1997 0.7947 0.082 Uiso 0.50 1 calc PR B 2 H38F H 0.2056 0.2931 0.7646 0.082 Uiso 0.50 1 calc PR B 2 C39B C 0.2289(14) 0.1821(19) 0.7495(7) 0.068(4) Uani 0.50 1 d PD B 1 H39C H 0.1911 0.2062 0.7696 0.082 Uiso 0.50 1 calc PR B 1 H39D H 0.2484 0.1240 0.7704 0.082 Uiso 0.50 1 calc PR B 1 C39C C 0.2592(10) 0.1853(19) 0.7330(10) 0.068(4) Uani 0.50 1 d PD B 2 H39E H 0.2970 0.2222 0.7195 0.082 Uiso 0.50 1 calc PR B 2 H39F H 0.2885 0.1301 0.7532 0.082 Uiso 0.50 1 calc PR B 2 C41B C -0.2028(6) 0.1855(6) 0.6819(5) 0.034(2) Uani 1 1 d . . . H41B H -0.2431 0.1357 0.6633 0.041 Uiso 1 1 calc R . . C42B C -0.2303(6) 0.2614(6) 0.6329(5) 0.035(3) Uani 1 1 d . . . N43B N -0.1852(4) 0.3071(5) 0.6064(4) 0.036(2) Uani 1 1 d . . . C44B C -0.2420(5) 0.3642(6) 0.5619(5) 0.031(2) Uani 1 1 d . . . C45B C -0.3211(5) 0.3515(6) 0.5619(5) 0.031(2) Uani 1 1 d . . . O46B O -0.3130(4) 0.2824(4) 0.6086(4) 0.0384(17) Uani 1 1 d . . . C47B C -0.4035(6) 0.3911(7) 0.5295(6) 0.049(3) Uani 1 1 d . . . H47D H -0.4202 0.4172 0.5636 0.074 Uiso 1 1 calc R . . H47E H -0.4445 0.3461 0.5044 0.074 Uiso 1 1 calc R . . H47F H -0.4015 0.4368 0.4983 0.074 Uiso 1 1 calc R . . C48B C -0.2167(5) 0.4243(6) 0.5168(5) 0.030(2) Uani 1 1 d . . . N49B N -0.1325(4) 0.4237(5) 0.5339(4) 0.0303(19) Uani 1 1 d . . . H49B H -0.0997 0.3967 0.5710 0.036 Uiso 1 1 calc R . . O50B O -0.2655(4) 0.4670(4) 0.4705(4) 0.0377(17) Uani 1 1 d . . . C51B C -0.0932(5) 0.4679(6) 0.4913(5) 0.036(3) Uani 1 1 d . . . H51B H -0.1295 0.4586 0.4425 0.043 Uiso 1 1 calc R . . C52B C -0.0109(5) 0.4266(7) 0.5077(6) 0.035(2) Uani 1 1 d U . . N53B N 0.0258(4) 0.3691(5) 0.5524(4) 0.035(2) Uani 1 1 d . . . C54B C 0.1040(5) 0.3522(6) 0.5463(6) 0.037(3) Uani 1 1 d . . . C55B C 0.1076(6) 0.4018(7) 0.4951(6) 0.045(3) Uani 1 1 d . . . O56B O 0.0350(4) 0.4518(4) 0.4684(4) 0.0439(18) Uani 1 1 d . . . C57B C 0.1702(7) 0.4133(8) 0.4629(7) 0.065(4) Uani 1 1 d . . . H57D H 0.1478 0.3862 0.4182 0.097 Uiso 1 1 calc R . . H57E H 0.2236 0.3850 0.4911 0.097 Uiso 1 1 calc R . . H57F H 0.1798 0.4760 0.4587 0.097 Uiso 1 1 calc R . . C58B C 0.1642(6) 0.2874(6) 0.5890(6) 0.040(3) Uani 1 1 d . . . N59B N 0.1377(5) 0.2480(6) 0.6345(5) 0.046(3) Uani 1 1 d . B . H59B H 0.0952 0.2722 0.6408 0.056 Uiso 1 1 calc R . . O60B O 0.2299(4) 0.2686(5) 0.5810(4) 0.052(2) Uani 1 1 d . . . C61B C 0.1759(6) 0.1674(7) 0.6736(6) 0.057(4) Uani 1 1 d D . . H61B H 0.2081 0.1335 0.6522 0.069 Uiso 1 1 calc R B 1 C62B C 0.1050(6) 0.1163(7) 0.6752(6) 0.044(3) Uani 1 1 d . B . N63B N 0.0340(5) 0.1459(6) 0.6736(5) 0.045(2) Uani 1 1 d . . . C64B C -0.0084(7) 0.0708(7) 0.6826(6) 0.050(3) Uani 1 1 d . B . C65B C 0.0398(7) -0.0040(8) 0.6871(7) 0.059(4) Uani 1 1 d . . . O66B O 0.1144(4) 0.0259(4) 0.6853(4) 0.055(2) Uani 1 1 d . B . C67B C 0.0301(8) -0.0991(7) 0.6974(9) 0.081(5) Uani 1 1 d . B . H67D H 0.0416 -0.1331 0.6636 0.121 Uiso 1 1 calc R . . H67E H -0.0277 -0.1107 0.6928 0.121 Uiso 1 1 calc R . . H67F H 0.0698 -0.1163 0.7425 0.121 Uiso 1 1 calc R . . C68B C -0.0945(6) 0.0798(7) 0.6826(5) 0.041(3) Uani 1 1 d . . . N69B N -0.1210(5) 0.1605(5) 0.6829(4) 0.040(2) Uani 1 1 d . B . H69B H -0.0863 0.2033 0.6838 0.048 Uiso 1 1 calc R . . O70B O -0.1381(5) 0.0128(5) 0.6816(5) 0.070(3) Uani 1 1 d . B . C1C C 0.2191(6) 0.5184(7) 0.6856(6) 0.043(3) Uani 1 1 d . . . C2C C 0.2845(6) 0.5805(7) 0.7330(6) 0.041(3) Uani 1 1 d . . . O1C O 0.2570(4) 0.6415(5) 0.7579(4) 0.056(2) Uani 1 1 d . . . O2C O 0.3579(4) 0.5658(5) 0.7370(4) 0.056(2) Uani 1 1 d . . . H2C H 0.3914 0.6023 0.7632 0.084 Uiso 1 1 calc R . . F1C F 0.2532(3) 0.4392(4) 0.6790(3) 0.0559(18) Uani 1 1 d . . . F2C F 0.1564(3) 0.5003(4) 0.7070(3) 0.0556(18) Uani 1 1 d . . . F3C F 0.1831(3) 0.5516(4) 0.6229(3) 0.0551(18) Uani 1 1 d . . . C1D C 0.1052(7) 0.0287(7) 0.8908(6) 0.114(2) Uani 1 1 d D . . C2D C 0.1340(14) 0.1353(14) 0.8954(10) 0.114(2) Uani 1 1 d . C . O1D O 0.0757(8) 0.1866(9) 0.8801(6) 0.114(2) Uani 1 1 d . . . H1D H 0.0936 0.2379 0.8803 0.171 Uiso 1 1 calc R C . O2D O 0.2103(8) 0.1437(8) 0.9036(6) 0.114(2) Uani 1 1 d . . . F1D F 0.1767(8) -0.0206(13) 0.9178(8) 0.114(2) Uani 0.50 1 d PD C 1 F2D F 0.0516(10) -0.0022(12) 0.8299(6) 0.114(2) Uani 0.50 1 d PD C 1 F3D F 0.0647(10) 0.0312(13) 0.9344(8) 0.114(2) Uani 0.50 1 d PD C 1 F1D' F 0.1489(10) -0.0233(12) 0.9448(7) 0.114(2) Uani 0.50 1 d PD C 2 F2D' F 0.1255(11) 0.0026(13) 0.8375(7) 0.114(2) Uani 0.50 1 d PD C 2 F3D' F 0.0203(7) 0.0199(13) 0.8717(9) 0.114(2) Uani 0.50 1 d PD C 2 C1E C 0.5203(10) 0.6955(11) 0.7471(8) 0.088(5) Uani 1 1 d . . . H1E1 H 0.4739 0.7320 0.7170 0.133 Uiso 1 1 calc R . . H1E2 H 0.5322 0.6487 0.7211 0.133 Uiso 1 1 calc R . . H1E3 H 0.5707 0.7318 0.7687 0.133 Uiso 1 1 calc R . . O1E O 0.4977(5) 0.6586(8) 0.7960(5) 0.088(3) Uani 1 1 d . . . H1E H 0.5391 0.6316 0.8241 0.131 Uiso 1 1 calc RD . . O1F O 0.0916(6) 0.3428(7) 0.8315(6) 0.096(3) Uani 1 1 d . . . H1F H 0.0923 0.3903 0.8514 0.144 Uiso 1 1 calc RD . . C1F C 0.0272(10) 0.3467(10) 0.7637(8) 0.096(5) Uani 1 1 d . . . H1F1 H -0.0281 0.3541 0.7655 0.144 Uiso 1 1 calc R . . H1F2 H 0.0278 0.2921 0.7400 0.144 Uiso 1 1 calc R . . H1F3 H 0.0384 0.3964 0.7398 0.144 Uiso 1 1 calc R . . C1G C 0.4204(15) 0.414(2) 0.1428(14) 0.083(4) Uani 0.50 1 d P . . H1G1 H 0.4643 0.3929 0.1835 0.124 Uiso 0.50 1 d PR . . H1G2 H 0.3880 0.3652 0.1174 0.124 Uiso 0.50 1 d PR . . H1G3 H 0.3844 0.4532 0.1538 0.124 Uiso 0.50 1 d PR . . O1G O 0.4567(9) 0.4558(15) 0.1036(9) 0.083(4) Uani 0.50 1 d P . . H1G H 0.4395 0.5065 0.0977 0.124 Uiso 0.50 1 d PR . . O1H O 0.4078(19) 0.635(2) 0.1034(16) 0.066(9) Uiso 0.25 1 d PD D 1 H1H H 0.4472 0.6693 0.1152 0.099 Uiso 0.25 1 d PR D 1 C1H C 0.338(2) 0.681(3) 0.0534(19) 0.045(11) Uiso 0.25 1 d PD D 1 H1H1 H 0.3266 0.6564 0.0088 0.067 Uiso 0.25 1 calc PR D 1 H1H2 H 0.3535 0.7434 0.0538 0.067 Uiso 0.25 1 calc PR D 1 H1H3 H 0.2884 0.6760 0.0636 0.067 Uiso 0.25 1 calc PR D 1 C1I C 0.5059(15) 0.1614(15) 0.8313(15) 0.083(4) Uani 0.50 1 d PD E 2 H1I1 H 0.4841 0.1955 0.8592 0.124 Uiso 0.50 1 calc PR E 2 H1I2 H 0.4718 0.1734 0.7837 0.124 Uiso 0.50 1 calc PR E 2 H1I3 H 0.5646 0.1781 0.8420 0.124 Uiso 0.50 1 calc PR E 2 O1I O 0.5019(10) 0.0707(14) 0.8443(10) 0.083(4) Uani 0.50 1 d PD E 2 H1I H 0.4513 0.0558 0.8329 0.124 Uiso 0.50 1 calc PR E 2 O3W O 0.258(3) 0.064(3) 0.293(2) 0.081(12) Uiso 0.25 1 d P F 1 C1J C 0.2130(18) 0.002(2) 0.2780(13) 0.081(9) Uani 0.50 1 d P G 2 H1J1 H 0.2625 0.0401 0.2976 0.122 Uiso 0.50 1 calc PR G 2 H1J2 H 0.2295 -0.0590 0.2914 0.122 Uiso 0.50 1 calc PR G 2 H1J3 H 0.1701 0.0200 0.2943 0.122 Uiso 0.50 1 calc PR G 2 O1J O 0.1800(12) 0.0085(13) 0.2074(10) 0.083(6) Uani 0.50 1 d P G 2 H1J5 H 0.1591 -0.0477 0.1876 0.125 Uiso 0.50 1 d PR G 2 O1W O 0.6615(8) 0.0307(11) 0.8510(7) 0.052(4) Uani 0.50 1 d PU H 2 O2W O 0.6096(14) 0.1877(15) 0.8110(11) 0.109(7) Uani 0.50 1 d PU I 2 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 N1A 0.049(6) 0.077(7) 0.074(8) 0.001(7) 0.015(5) 0.004(5) C11A 0.064(9) 0.091(11) 0.066(10) -0.019(9) 0.005(7) -0.001(8) C12A 0.125(14) 0.100(13) 0.066(11) -0.006(9) 0.038(10) 0.008(11) N13A 0.065(7) 0.094(10) 0.058(7) 0.003(7) 0.018(6) 0.005(7) C14A 0.075(9) 0.064(9) 0.052(9) -0.012(7) 0.015(7) 0.010(7) S15A 0.116(4) 0.105(4) 0.083(3) -0.038(3) -0.013(3) 0.010(3) N16A 0.052(6) 0.072(7) 0.057(7) -0.024(6) 0.017(6) -0.013(5) C17A 0.055(7) 0.054(8) 0.072(10) 0.002(7) 0.020(7) 0.001(6) C18A 0.045(7) 0.057(8) 0.085(10) 0.008(7) 0.025(7) 0.000(6) C19A 0.083(9) 0.050(8) 0.078(10) -0.016(7) 0.049(8) -0.008(7) C21A 0.052(8) 0.077(10) 0.108(12) 0.018(9) 0.028(8) 0.005(7) C22A 0.079(11) 0.134(17) 0.097(13) 0.024(11) 0.025(10) 0.006(11) N23A 0.085(9) 0.102(11) 0.093(10) -0.013(8) 0.022(8) 0.004(8) C24A 0.069(9) 0.068(10) 0.111(13) -0.023(9) 0.042(9) -0.037(8) S25A 0.083(3) 0.141(4) 0.103(3) -0.010(3) 0.053(3) -0.007(3) N26A 0.095(10) 0.081(9) 0.152(14) -0.005(9) 0.068(10) -0.032(8) C27A 0.062(9) 0.138(16) 0.075(12) -0.007(11) 0.009(8) -0.014(10) C28A 0.075(9) 0.079(10) 0.114(14) 0.006(9) 0.043(10) 0.002(8) C29A 0.031(6) 0.086(11) 0.156(16) -0.004(10) 0.025(8) 0.013(7) C31A 0.077(9) 0.099(9) 0.063(10) 0.017(9) 0.015(8) -0.006(8) C32A 0.094(10) 0.057(8) 0.057(9) -0.003(7) -0.023(8) 0.023(8) N33A 0.050(6) 0.072(7) 0.056(7) 0.010(6) 0.009(5) 0.019(5) C34A 0.026(5) 0.033(6) 0.060(8) -0.001(5) 0.008(5) 0.005(4) S35A 0.0241(13) 0.075(2) 0.082(2) -0.0064(18) 0.0093(14) 0.0100(13) N36A 0.023(4) 0.034(5) 0.070(7) 0.002(5) 0.018(4) 0.002(4) C37A 0.031(5) 0.034(6) 0.055(8) -0.003(5) 0.014(5) 0.004(4) C38A 0.035(5) 0.025(6) 0.058(8) 0.001(5) 0.015(5) 0.001(4) C39A 0.016(4) 0.022(5) 0.066(8) 0.004(5) -0.003(5) 0.000(4) C41A 0.024(5) 0.043(6) 0.061(8) -0.003(6) 0.023(5) -0.005(4) C42A 0.040(6) 0.026(6) 0.033(6) -0.001(5) -0.005(5) 0.003(5) N43A 0.024(4) 0.022(4) 0.063(6) -0.015(4) 0.014(4) -0.007(3) C44A 0.021(5) 0.020(5) 0.100(10) 0.011(6) 0.020(6) -0.004(4) C45A 0.024(5) 0.026(6) 0.085(9) -0.008(5) 0.013(5) -0.014(5) O46A 0.034(4) 0.034(4) 0.065(5) -0.001(4) 0.009(3) -0.001(3) C47A 0.037(6) 0.029(6) 0.109(11) 0.006(6) 0.020(6) -0.002(5) C48A 0.040(6) 0.026(6) 0.093(10) -0.007(6) 0.023(6) -0.003(5) N49A 0.031(5) 0.031(5) 0.144(10) -0.020(6) 0.044(6) -0.009(4) O50A 0.030(4) 0.043(5) 0.143(8) 0.008(5) 0.036(5) -0.006(4) C51A 0.053(6) 0.054(7) 0.112(8) -0.003(6) 0.044(6) -0.006(5) C52A 0.029(5) 0.040(6) 0.082(7) -0.002(5) 0.025(5) -0.002(4) N53A 0.031(5) 0.044(6) 0.129(10) -0.009(6) 0.048(6) 0.001(4) C54A 0.030(5) 0.013(5) 0.106(10) -0.003(6) 0.035(6) 0.007(4) C55A 0.045(5) 0.026(5) 0.082(7) -0.005(5) 0.026(5) -0.005(4) O56A 0.026(4) 0.046(5) 0.155(9) -0.008(5) 0.048(5) 0.000(3) C57A 0.039(6) 0.056(8) 0.099(10) -0.001(7) 0.047(6) 0.010(6) C58A 0.039(5) 0.037(6) 0.076(7) 0.000(5) 0.027(5) 0.019(5) N59A 0.028(4) 0.035(5) 0.066(6) 0.000(4) 0.030(4) 0.009(4) O60A 0.037(4) 0.051(5) 0.098(7) -0.005(5) 0.042(4) -0.010(4) C61A 0.024(5) 0.038(6) 0.049(7) -0.002(5) 0.018(5) 0.004(4) C62A 0.025(5) 0.034(6) 0.044(7) 0.011(5) 0.009(5) -0.001(4) N63A 0.014(4) 0.033(5) 0.055(6) 0.017(5) 0.012(4) 0.007(3) C64A 0.023(5) 0.012(5) 0.044(6) 0.000(4) 0.011(4) -0.001(4) C65A 0.022(4) 0.025(5) 0.052(6) 0.010(4) 0.018(4) 0.010(4) O66A 0.022(3) 0.033(4) 0.047(4) 0.007(3) 0.016(3) 0.012(3) C67A 0.016(4) 0.042(6) 0.034(6) -0.004(5) -0.001(4) 0.004(4) C68A 0.022(5) 0.014(5) 0.061(7) 0.002(5) 0.015(5) 0.005(4) N69A 0.023(4) 0.024(4) 0.067(7) -0.009(4) 0.013(4) 0.003(3) O70A 0.021(3) 0.033(4) 0.048(5) -0.004(3) 0.015(3) 0.006(3) N1B 0.046(6) 0.118(10) 0.045(7) -0.001(7) -0.002(5) -0.010(6) C11B 0.047(7) 0.109(12) 0.106(12) 0.001(10) 0.038(8) 0.005(8) C12B 0.043(7) 0.101(12) 0.089(11) -0.007(10) 0.029(7) -0.005(8) N13B 0.073(9) 0.119(13) 0.139(13) 0.019(10) 0.039(9) 0.007(9) C14B 0.047(8) 0.112(14) 0.086(11) -0.010(10) 0.022(7) -0.011(8) S15B 0.058(2) 0.144(5) 0.161(5) -0.056(4) 0.027(3) 0.009(3) N16B 0.066(6) 0.111(9) 0.100(8) 0.001(7) 0.038(6) -0.009(6) C17B 0.080(7) 0.111(8) 0.089(7) -0.003(7) 0.036(6) -0.018(6) C18B 0.080(7) 0.096(9) 0.083(7) 0.001(7) 0.050(6) -0.012(7) C19B 0.094(10) 0.048(7) 0.057(9) 0.014(6) 0.036(7) 0.018(7) C21B 0.061(8) 0.062(9) 0.066(10) -0.016(7) 0.013(7) -0.001(7) C22B 0.049(7) 0.111(13) 0.037(8) -0.003(8) -0.002(6) 0.013(7) N23B 0.035(5) 0.046(6) 0.099(9) -0.024(6) 0.004(5) -0.010(4) C24B 0.042(6) 0.045(7) 0.070(9) -0.030(7) 0.021(6) 0.014(5) S25B 0.0312(14) 0.080(2) 0.068(2) -0.0114(18) 0.0198(14) -0.0035(15) N26B 0.030(5) 0.035(5) 0.081(8) -0.020(5) 0.013(5) -0.005(4) C27B 0.037(6) 0.033(6) 0.081(9) -0.009(6) 0.032(6) -0.004(5) C28B 0.036(6) 0.027(6) 0.061(8) -0.002(5) 0.020(5) 0.001(4) C29B 0.019(4) 0.024(5) 0.043(6) 0.004(5) 0.003(4) 0.011(4) C31B 0.065(9) 0.109(13) 0.078(11) 0.000(9) 0.005(8) -0.006(9) C32B 0.039(7) 0.093(12) 0.088(11) -0.012(9) 0.017(7) 0.011(7) N33B 0.041(6) 0.078(9) 0.101(10) 0.032(8) 0.008(6) 0.004(6) C34B 0.039(7) 0.102(13) 0.069(10) 0.026(9) -0.012(7) 0.006(7) S35B 0.096(3) 0.064(2) 0.064(2) 0.0105(19) 0.030(2) 0.018(2) N36B 0.081(8) 0.042(7) 0.076(9) 0.020(6) -0.017(6) 0.010(6) C37B 0.048(7) 0.039(6) 0.070(7) -0.001(5) -0.026(6) -0.008(6) C37C 0.048(7) 0.039(6) 0.070(7) -0.001(5) -0.026(6) -0.008(6) C38B 0.048(7) 0.039(6) 0.070(7) -0.001(5) -0.026(6) -0.008(6) C38C 0.048(7) 0.039(6) 0.070(7) -0.001(5) -0.026(6) -0.008(6) C39B 0.048(7) 0.039(6) 0.070(7) -0.001(5) -0.026(6) -0.008(6) C39C 0.048(7) 0.039(6) 0.070(7) -0.001(5) -0.026(6) -0.008(6) C41B 0.035(5) 0.025(5) 0.048(7) 0.003(5) 0.021(5) 0.006(4) C42B 0.025(5) 0.023(5) 0.047(7) -0.014(5) 0.003(5) -0.002(4) N43B 0.018(4) 0.029(4) 0.057(6) 0.002(4) 0.010(4) -0.007(3) C44B 0.018(4) 0.028(5) 0.043(6) -0.003(5) 0.009(4) -0.008(4) C45B 0.017(4) 0.023(5) 0.049(7) -0.009(5) 0.007(4) -0.005(4) O46B 0.025(3) 0.024(4) 0.069(5) -0.004(4) 0.022(3) -0.006(3) C47B 0.028(5) 0.038(6) 0.090(9) 0.013(6) 0.033(6) 0.010(5) C48B 0.016(4) 0.023(5) 0.046(7) -0.010(5) 0.007(4) -0.012(4) N49B 0.017(4) 0.026(4) 0.048(5) 0.005(4) 0.013(4) 0.002(3) O50B 0.018(3) 0.029(4) 0.059(5) 0.000(4) 0.008(3) 0.000(3) C51B 0.020(5) 0.036(6) 0.046(7) -0.007(5) 0.006(5) -0.008(4) C52B 0.020(4) 0.036(5) 0.052(6) -0.004(5) 0.018(4) -0.003(4) N53B 0.018(4) 0.029(5) 0.054(6) -0.014(4) 0.011(4) -0.008(3) C54B 0.014(4) 0.020(5) 0.075(8) -0.009(5) 0.015(5) -0.010(4) C55B 0.020(5) 0.028(6) 0.083(9) -0.018(6) 0.015(5) 0.000(4) O56B 0.036(4) 0.033(4) 0.069(5) -0.006(4) 0.028(4) -0.001(3) C57B 0.046(6) 0.041(7) 0.122(12) -0.010(7) 0.049(7) -0.009(5) C58B 0.031(6) 0.026(6) 0.052(7) -0.005(5) 0.004(5) -0.002(5) N59B 0.019(4) 0.038(5) 0.066(7) -0.006(5) 0.000(4) 0.007(4) O60B 0.014(3) 0.054(5) 0.084(6) -0.008(4) 0.014(4) 0.007(3) C61B 0.031(5) 0.021(6) 0.106(10) 0.022(6) 0.012(6) 0.015(5) C62B 0.031(6) 0.042(7) 0.046(7) -0.003(5) 0.001(5) 0.000(5) N63B 0.032(5) 0.039(5) 0.060(6) 0.010(5) 0.013(4) 0.014(4) C64B 0.048(6) 0.031(6) 0.066(8) 0.024(6) 0.018(6) 0.025(5) C65B 0.040(6) 0.044(7) 0.112(11) 0.014(7) 0.051(7) 0.008(5) O66B 0.055(5) 0.029(4) 0.073(6) 0.011(4) 0.018(4) 0.017(3) C67B 0.052(7) 0.028(7) 0.171(16) -0.004(8) 0.053(9) 0.004(5) C68B 0.043(6) 0.028(6) 0.055(7) 0.002(5) 0.021(5) 0.009(5) N69B 0.036(4) 0.029(5) 0.056(6) 0.009(4) 0.019(4) 0.001(4) O70B 0.072(5) 0.037(5) 0.122(8) 0.005(5) 0.061(6) 0.007(4) C1C 0.024(5) 0.043(7) 0.061(8) -0.010(6) 0.018(5) -0.006(5) C2C 0.022(5) 0.027(6) 0.060(8) -0.001(5) 0.000(5) -0.008(4) O1C 0.034(4) 0.034(4) 0.092(6) -0.014(4) 0.018(4) -0.005(3) O2C 0.026(4) 0.062(5) 0.070(6) -0.024(4) 0.008(4) -0.015(4) F1C 0.026(3) 0.041(4) 0.081(5) -0.011(3) 0.000(3) 0.004(3) F2C 0.029(3) 0.057(4) 0.082(5) -0.013(3) 0.024(3) -0.020(3) F3C 0.037(3) 0.054(4) 0.051(4) 0.019(3) -0.007(3) -0.008(3) C1D 0.119(5) 0.114(4) 0.103(4) 0.011(3) 0.038(4) 0.009(4) C2D 0.119(5) 0.114(4) 0.103(4) 0.011(3) 0.038(4) 0.009(4) O1D 0.119(5) 0.114(4) 0.103(4) 0.011(3) 0.038(4) 0.009(4) O2D 0.119(5) 0.114(4) 0.103(4) 0.011(3) 0.038(4) 0.009(4) F1D 0.119(5) 0.114(4) 0.103(4) 0.011(3) 0.038(4) 0.009(4) F2D 0.119(5) 0.114(4) 0.103(4) 0.011(3) 0.038(4) 0.009(4) F3D 0.119(5) 0.114(4) 0.103(4) 0.011(3) 0.038(4) 0.009(4) F1D' 0.119(5) 0.114(4) 0.103(4) 0.011(3) 0.038(4) 0.009(4) F2D' 0.119(5) 0.114(4) 0.103(4) 0.011(3) 0.038(4) 0.009(4) F3D' 0.119(5) 0.114(4) 0.103(4) 0.011(3) 0.038(4) 0.009(4) C1E 0.083(10) 0.089(11) 0.083(11) 0.006(9) 0.023(9) 0.003(9) O1E 0.042(5) 0.148(10) 0.054(6) 0.025(6) 0.001(4) -0.032(6) O1F 0.059(6) 0.094(8) 0.121(9) -0.029(7) 0.021(6) -0.007(5) C1F 0.103(12) 0.056(9) 0.095(12) -0.017(8) 0.005(10) -0.017(9) C1G 0.039(5) 0.132(10) 0.072(8) 0.019(8) 0.016(5) 0.011(6) O1G 0.039(5) 0.132(10) 0.072(8) 0.019(8) 0.016(5) 0.011(6) C1I 0.039(5) 0.132(10) 0.072(8) 0.019(8) 0.016(5) 0.011(6) O1I 0.039(5) 0.132(10) 0.072(8) 0.019(8) 0.016(5) 0.011(6) C1J 0.072(18) 0.12(3) 0.030(16) 0.012(16) -0.004(13) 0.024(19) O1J 0.094(13) 0.088(14) 0.094(16) 0.035(11) 0.064(12) 0.048(11) O1W 0.029(6) 0.085(8) 0.044(7) -0.003(6) 0.017(5) 0.003(6) O2W 0.094(10) 0.098(10) 0.112(10) -0.027(8) 0.016(8) 0.008(8) _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 N1A C31A 1.449(18) . ? N1A C11A 1.454(18) . ? N1A C21A 1.590(18) . ? C11A C12A 1.56(2) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A N13A 1.445(19) . ? C12A H12C 0.9900 . ? C12A H12D 0.9900 . ? N13A C14A 1.340(17) . ? N13A H13A 0.8800 . ? C14A N16A 1.349(16) . ? C14A S15A 1.698(14) . ? N16A C17A 1.477(16) . ? N16A H16A 0.8800 . ? C17A C18A 1.558(18) . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C18A C19A 1.531(17) . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? C19A C41A 1.524(17) . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? C21A C22A 1.401(19) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C22A N23A 1.56(2) . ? C22A H22C 0.9900 . ? C22A H22D 0.9900 . ? N23A C24A 1.325(18) . ? N23A H23A 0.8800 . ? C24A N26A 1.309(19) . ? C24A S25A 1.748(17) . ? N26A C27A 1.53(2) . ? N26A H26A 0.8800 . ? C27A C28A 1.43(2) . ? C27A H71A 0.9900 . ? C27A H71B 0.9900 . ? C28A C29A 1.421(18) . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C29A C51A 1.57(2) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C31A C32A 1.54(2) . ? C31A H31C 0.9900 . ? C31A H31D 0.9900 . ? C32A N33A 1.448(15) . ? C32A H32C 0.9900 . ? C32A H32D 0.9900 . ? N33A C34A 1.415(15) . ? N33A H33A 0.8800 . ? C34A N36A 1.323(12) . ? C34A S35A 1.698(11) . ? N36A C37A 1.455(14) . ? N36A H36A 0.8800 . ? C37A C38A 1.536(14) . ? C37A H37A 0.9900 . ? C37A H37B 0.9900 . ? C38A C39A 1.526(15) . ? C38A H38A 0.9900 . ? C38A H38B 0.9900 . ? C39A C61A 1.565(13) . ? C39A H39A 0.9900 . ? C39A H39B 0.9900 . ? C41A N69A 1.481(13) . ? C41A C42A 1.525(14) . ? C41A H41A 1.0000 . ? C42A N43A 1.267(12) . ? C42A O46A 1.387(12) . ? N43A C44A 1.433(12) . ? C44A C45A 1.322(13) . ? C44A C48A 1.493(15) . ? C45A O46A 1.404(12) . ? C45A C47A 1.501(14) . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? C48A O50A 1.239(13) . ? C48A N49A 1.345(14) . ? N49A C51A 1.507(14) . ? N49A H49A 0.8800 . ? C51A C52A 1.521(17) . ? C51A H51A 1.0000 . ? C52A N53A 1.296(13) . ? C52A O56A 1.364(13) . ? N53A C54A 1.406(14) . ? C54A C55A 1.362(15) . ? C54A C58A 1.430(15) . ? C55A O56A 1.421(14) . ? C55A C57A 1.528(15) . ? C57A H57A 0.9800 . ? C57A H57B 0.9800 . ? C57A H57C 0.9800 . ? C58A O60A 1.285(13) . ? C58A N59A 1.361(12) . ? N59A C61A 1.442(12) . ? N59A H59A 0.8800 . ? C61A C62A 1.494(14) . ? C61A H61A 1.0000 . ? C62A N63A 1.332(13) . ? C62A O66A 1.349(10) . ? N63A C64A 1.409(11) . ? C64A C65A 1.344(13) . ? C64A C68A 1.518(14) . ? C65A O66A 1.406(11) . ? C65A C67A 1.477(12) . ? C67A H67A 0.9800 . ? C67A H67B 0.9800 . ? C67A H67C 0.9800 . ? C68A O70A 1.222(10) . ? C68A N69A 1.347(11) . ? N69A H69A 0.8800 . ? N1B C31B 1.505(16) . ? N1B C21B 1.524(18) . ? N1B C11B 1.535(16) . ? C11B C12B 1.52(2) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B N13B 1.41(2) . ? C12B H12A 0.9900 . ? C12B H12B 0.9900 . ? N13B C14B 1.353(18) . ? N13B H13B 0.8800 . ? C14B N16B 1.42(2) . ? C14B S15B 1.637(15) . ? N16B C17B 1.438(19) . ? N16B H16C 0.8800 . ? C17B C18B 1.55(2) . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C18B C19B 1.510(19) . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? C19B C41B 1.553(16) . ? C19B H19C 0.9900 . ? C19B H19D 0.9900 . ? C21B C22B 1.423(19) . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? C22B N23B 1.517(18) . ? C22B H22A 0.9900 . ? C22B H22B 0.9900 . ? N23B C24B 1.390(15) . ? N23B H23B 0.8800 . ? C24B N26B 1.369(16) . ? C24B S25B 1.679(13) . ? N26B C27B 1.485(14) . ? N26B H26B 0.8800 . ? C27B C28B 1.519(14) . ? C27B H27A 0.9900 . ? C27B H27B 0.9900 . ? C28B C29B 1.535(14) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C29B C51B 1.563(13) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C31B C32B 1.506(19) . ? C31B H31A 0.9900 . ? C31B H31B 0.9900 . ? C32B N33B 1.406(18) . ? C32B H32A 0.9900 . ? C32B H32B 0.9900 . ? N33B C34B 1.48(2) . ? N33B H33B 0.8800 . ? C34B N36B 1.315(19) . ? C34B S35B 1.765(17) . ? N36B C37C 1.417(10) . ? N36B C37B 1.459(10) . ? N36B H36B 0.8800 . ? C37B C38B 1.558(10) . ? C37B H37C 0.9900 . ? C37B H37D 0.9900 . ? C37C C38C 1.544(10) . ? C37C H37E 0.9900 . ? C37C H37F 0.9900 . ? C38B C39B 1.540(10) . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? C38C C39C 1.529(10) . ? C38C H38E 0.9900 . ? C38C H38F 0.9900 . ? C39B C61B 1.546(10) . ? C39B H39C 0.9900 . ? C39B H39D 0.9900 . ? C39C C61B 1.525(10) . ? C39C H39E 0.9900 . ? C39C H39F 0.9900 . ? C41B N69B 1.457(12) . ? C41B C42B 1.512(14) . ? C41B H41B 1.0000 . ? C42B N43B 1.334(13) . ? C42B O46B 1.351(10) . ? N43B C44B 1.377(12) . ? C44B C45B 1.383(12) . ? C44B C48B 1.525(14) . ? C45B O46B 1.428(12) . ? C45B C47B 1.445(12) . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? C48B O50B 1.211(11) . ? C48B N49B 1.353(10) . ? N49B C51B 1.507(13) . ? N49B H49B 0.8800 . ? C51B C52B 1.464(13) . ? C51B H51B 1.0000 . ? C52B N53B 1.272(13) . ? C52B O56B 1.428(12) . ? N53B C54B 1.434(12) . ? C54B C55B 1.364(16) . ? C54B C58B 1.464(14) . ? C55B O56B 1.384(11) . ? C55B C57B 1.514(16) . ? C57B H57D 0.9800 . ? C57B H57E 0.9800 . ? C57B H57F 0.9800 . ? C58B O60B 1.250(12) . ? C58B N59B 1.381(14) . ? N59B C61B 1.489(13) . ? N59B H59B 0.8800 . ? C61B C62B 1.465(15) . ? C61B H61B 1.0000 . ? C62B N63B 1.295(13) . ? C62B O66B 1.395(12) . ? N63B C64B 1.415(14) . ? C64B C65B 1.393(15) . ? C64B C68B 1.495(15) . ? C65B O66B 1.383(12) . ? C65B C67B 1.485(16) . ? C67B H67D 0.9800 . ? C67B H67E 0.9800 . ? C67B H67F 0.9800 . ? C68B O70B 1.265(13) . ? C68B N69B 1.313(13) . ? N69B H69B 0.8800 . ? C1C F3C 1.346(13) . ? C1C F2C 1.369(12) . ? C1C F1C 1.375(11) . ? C1C C2C 1.517(13) . ? C2C O2C 1.259(12) . ? C2C O1C 1.259(13) . ? O2C H2C 0.8400 . ? C1D F2D 1.357(7) . ? C1D F1D' 1.364(8) . ? C1D F1D 1.362(7) . ? C1D F3D' 1.364(7) . ? C1D F3D 1.383(7) . ? C1D F2D' 1.392(8) . ? C1D C2D 1.69(2) . ? C2D O1D 1.21(2) . ? C2D O2D 1.27(2) . ? O1D H1D 0.8400 . ? C1E O1E 1.384(17) . ? C1E H1E1 0.9800 . ? C1E H1E2 0.9800 . ? C1E H1E3 0.9800 . ? O1E H1E 0.8400 . ? O1F C1F 1.446(17) . ? O1F H1F 0.8400 . ? C1F H1F1 0.9800 . ? C1F H1F2 0.9800 . ? C1F H1F3 0.9800 . ? C1G O1G 1.39(3) . ? C1G H1G1 0.9600 . ? C1G H1G2 0.9600 . ? C1G H1G3 0.9600 . ? O1G H1G 0.8200 . ? O1H C1H 1.443(10) . ? O1H H1H 0.8200 . ? C1H H1H1 0.9800 . ? C1H H1H2 0.9800 . ? C1H H1H3 0.9800 . ? C1I O1I 1.418(10) . ? C1I H1I1 0.9800 . ? C1I H1I2 0.9800 . ? C1I H1I3 0.9800 . ? O1I H1I 0.8400 . ? C1J O1J 1.41(3) . ? C1J H1J1 0.9800 . ? C1J H1J2 0.9800 . ? C1J H1J3 0.9800 . ? O1J H1J5 0.9600 . ? 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 C31A N1A C11A 113.5(12) . . ? C31A N1A C21A 111.9(11) . . ? C11A N1A C21A 112.8(11) . . ? N1A C11A C12A 115.1(12) . . ? N1A C11A H11A 108.5 . . ? C12A C11A H11A 108.5 . . ? N1A C11A H11B 108.5 . . ? C12A C11A H11B 108.5 . . ? H11A C11A H11B 107.5 . . ? N13A C12A C11A 113.9(13) . . ? N13A C12A H12C 108.8 . . ? C11A C12A H12C 108.8 . . ? N13A C12A H12D 108.8 . . ? C11A C12A H12D 108.8 . . ? H12C C12A H12D 107.7 . . ? C14A N13A C12A 124.0(13) . . ? C14A N13A H13A 118.0 . . ? C12A N13A H13A 118.0 . . ? N13A C14A N16A 115.3(11) . . ? N13A C14A S15A 120.9(10) . . ? N16A C14A S15A 123.8(11) . . ? C14A N16A C17A 124.0(10) . . ? C14A N16A H16A 118.0 . . ? C17A N16A H16A 118.0 . . ? N16A C17A C18A 110.3(11) . . ? N16A C17A H17A 109.6 . . ? C18A C17A H17A 109.6 . . ? N16A C17A H17B 109.6 . . ? C18A C17A H17B 109.6 . . ? H17A C17A H17B 108.1 . . ? C19A C18A C17A 115.1(10) . . ? C19A C18A H18A 108.5 . . ? C17A C18A H18A 108.5 . . ? C19A C18A H18B 108.5 . . ? C17A C18A H18B 108.5 . . ? H18A C18A H18B 107.5 . . ? C41A C19A C18A 116.7(10) . . ? C41A C19A H19A 108.1 . . ? C18A C19A H19A 108.1 . . ? C41A C19A H19B 108.1 . . ? C18A C19A H19B 108.1 . . ? H19A C19A H19B 107.3 . . ? C22A C21A N1A 115.3(13) . . ? C22A C21A H21A 108.4 . . ? N1A C21A H21A 108.4 . . ? C22A C21A H21B 108.4 . . ? N1A C21A H21B 108.4 . . ? H21A C21A H21B 107.5 . . ? C21A C22A N23A 109.1(14) . . ? C21A C22A H22C 109.9 . . ? N23A C22A H22C 109.9 . . ? C21A C22A H22D 109.9 . . ? N23A C22A H22D 109.9 . . ? H22C C22A H22D 108.3 . . ? C24A N23A C22A 124.5(15) . . ? C24A N23A H23A 117.7 . . ? C22A N23A H23A 117.7 . . ? N26A C24A N23A 116.1(15) . . ? N26A C24A S25A 121.2(12) . . ? N23A C24A S25A 122.1(13) . . ? C24A N26A C27A 131.8(15) . . ? C24A N26A H26A 114.1 . . ? C27A N26A H26A 114.1 . . ? C28A C27A N26A 115.2(13) . . ? C28A C27A H71A 108.5 . . ? N26A C27A H71A 108.5 . . ? C28A C27A H71B 108.5 . . ? N26A C27A H71B 108.5 . . ? H71A C27A H71B 107.5 . . ? C29A C28A C27A 119.7(16) . . ? C29A C28A H28A 107.4 . . ? C27A C28A H28A 107.4 . . ? C29A C28A H28B 107.4 . . ? C27A C28A H28B 107.4 . . ? H28A C28A H28B 106.9 . . ? C28A C29A C51A 117.9(15) . . ? C28A C29A H29A 107.8 . . ? C51A C29A H29A 107.8 . . ? C28A C29A H29B 107.8 . . ? C51A C29A H29B 107.8 . . ? H29A C29A H29B 107.2 . . ? N1A C31A C32A 118.7(12) . . ? N1A C31A H31C 107.6 . . ? C32A C31A H31C 107.6 . . ? N1A C31A H31D 107.6 . . ? C32A C31A H31D 107.6 . . ? H31C C31A H31D 107.1 . . ? N33A C32A C31A 113.0(11) . . ? N33A C32A H32C 109.0 . . ? C31A C32A H32C 109.0 . . ? N33A C32A H32D 109.0 . . ? C31A C32A H32D 109.0 . . ? H32C C32A H32D 107.8 . . ? C34A N33A C32A 123.5(11) . . ? C34A N33A H33A 118.2 . . ? C32A N33A H33A 118.2 . . ? N36A C34A N33A 114.6(9) . . ? N36A C34A S35A 122.1(10) . . ? N33A C34A S35A 123.3(7) . . ? C34A N36A C37A 125.3(9) . . ? C34A N36A H36A 117.3 . . ? C37A N36A H36A 117.3 . . ? N36A C37A C38A 112.0(8) . . ? N36A C37A H37A 109.2 . . ? C38A C37A H37A 109.2 . . ? N36A C37A H37B 109.2 . . ? C38A C37A H37B 109.2 . . ? H37A C37A H37B 107.9 . . ? C39A C38A C37A 114.3(8) . . ? C39A C38A H38A 108.7 . . ? C37A C38A H38A 108.7 . . ? C39A C38A H38B 108.7 . . ? C37A C38A H38B 108.7 . . ? H38A C38A H38B 107.6 . . ? C38A C39A C61A 111.6(8) . . ? C38A C39A H39A 109.3 . . ? C61A C39A H39A 109.3 . . ? C38A C39A H39B 109.3 . . ? C61A C39A H39B 109.3 . . ? H39A C39A H39B 108.0 . . ? N69A C41A C19A 110.6(9) . . ? N69A C41A C42A 102.7(8) . . ? C19A C41A C42A 110.0(8) . . ? N69A C41A H41A 111.1 . . ? C19A C41A H41A 111.1 . . ? C42A C41A H41A 111.1 . . ? N43A C42A O46A 113.7(9) . . ? N43A C42A C41A 128.8(9) . . ? O46A C42A C41A 117.5(9) . . ? C42A N43A C44A 105.6(8) . . ? C45A C44A N43A 108.5(8) . . ? C45A C44A C48A 131.0(9) . . ? N43A C44A C48A 120.5(8) . . ? C44A C45A O46A 108.5(8) . . ? C44A C45A C47A 135.2(10) . . ? O46A C45A C47A 116.1(9) . . ? C42A O46A C45A 103.7(8) . . ? C45A C47A H47A 109.5 . . ? C45A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C45A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? O50A C48A N49A 124.2(10) . . ? O50A C48A C44A 124.7(9) . . ? N49A C48A C44A 110.9(9) . . ? C48A N49A C51A 125.2(10) . . ? C48A N49A H49A 117.4 . . ? C51A N49A H49A 117.4 . . ? N49A C51A C52A 105.3(9) . . ? N49A C51A C29A 109.0(11) . . ? C52A C51A C29A 114.9(11) . . ? N49A C51A H51A 109.2 . . ? C52A C51A H51A 109.2 . . ? C29A C51A H51A 109.2 . . ? N53A C52A O56A 113.2(10) . . ? N53A C52A C51A 127.9(10) . . ? O56A C52A C51A 118.9(9) . . ? C52A N53A C54A 104.7(8) . . ? C55A C54A N53A 111.4(9) . . ? C55A C54A C58A 127.4(10) . . ? N53A C54A C58A 121.0(9) . . ? C54A C55A O56A 104.0(9) . . ? C54A C55A C57A 135.9(10) . . ? O56A C55A C57A 119.9(9) . . ? C52A O56A C55A 106.6(8) . . ? C55A C57A H57A 109.5 . . ? C55A C57A H57B 109.5 . . ? H57A C57A H57B 109.5 . . ? C55A C57A H57C 109.5 . . ? H57A C57A H57C 109.5 . . ? H57B C57A H57C 109.5 . . ? O60A C58A N59A 120.7(10) . . ? O60A C58A C54A 124.1(9) . . ? N59A C58A C54A 115.2(10) . . ? C58A N59A C61A 126.2(9) . . ? C58A N59A H59A 116.9 . . ? C61A N59A H59A 116.9 . . ? N59A C61A C62A 106.2(8) . . ? N59A C61A C39A 113.5(7) . . ? C62A C61A C39A 108.8(8) . . ? N59A C61A H61A 109.4 . . ? C62A C61A H61A 109.4 . . ? C39A C61A H61A 109.4 . . ? N63A C62A O66A 111.8(8) . . ? N63A C62A C61A 129.0(8) . . ? O66A C62A C61A 119.0(9) . . ? C62A N63A C64A 106.6(7) . . ? C65A C64A N63A 107.4(8) . . ? C65A C64A C68A 130.0(8) . . ? N63A C64A C68A 122.2(8) . . ? C64A C65A O66A 108.8(7) . . ? C64A C65A C67A 133.1(9) . . ? O66A C65A C67A 118.0(8) . . ? C62A O66A C65A 105.3(8) . . ? C65A C67A H67A 109.5 . . ? C65A C67A H67B 109.5 . . ? H67A C67A H67B 109.5 . . ? C65A C67A H67C 109.5 . . ? H67A C67A H67C 109.5 . . ? H67B C67A H67C 109.5 . . ? O70A C68A N69A 124.3(9) . . ? O70A C68A C64A 123.5(8) . . ? N69A C68A C64A 112.2(8) . . ? C68A N69A C41A 124.2(7) . . ? C68A N69A H69A 117.9 . . ? C41A N69A H69A 117.9 . . ? C31B N1B C21B 112.7(11) . . ? C31B N1B C11B 112.7(12) . . ? C21B N1B C11B 114.0(11) . . ? C12B C11B N1B 116.9(12) . . ? C12B C11B H11C 108.1 . . ? N1B C11B H11C 108.1 . . ? C12B C11B H11D 108.1 . . ? N1B C11B H11D 108.1 . . ? H11C C11B H11D 107.3 . . ? N13B C12B C11B 118.7(15) . . ? N13B C12B H12A 107.6 . . ? C11B C12B H12A 107.6 . . ? N13B C12B H12B 107.6 . . ? C11B C12B H12B 107.6 . . ? H12A C12B H12B 107.1 . . ? C14B N13B C12B 121.4(14) . . ? C14B N13B H13B 119.3 . . ? C12B N13B H13B 119.3 . . ? N13B C14B N16B 110.9(14) . . ? N13B C14B S15B 125.9(14) . . ? N16B C14B S15B 123.1(11) . . ? C14B N16B C17B 125.1(13) . . ? C14B N16B H16C 117.4 . . ? C17B N16B H16C 117.4 . . ? N16B C17B C18B 115.5(13) . . ? N16B C17B H17C 108.4 . . ? C18B C17B H17C 108.4 . . ? N16B C17B H17D 108.4 . . ? C18B C17B H17D 108.4 . . ? H17C C17B H17D 107.5 . . ? C19B C18B C17B 115.9(13) . . ? C19B C18B H18C 108.3 . . ? C17B C18B H18C 108.3 . . ? C19B C18B H18D 108.3 . . ? C17B C18B H18D 108.3 . . ? H18C C18B H18D 107.4 . . ? C18B C19B C41B 113.5(10) . . ? C18B C19B H19C 108.9 . . ? C41B C19B H19C 108.9 . . ? C18B C19B H19D 108.9 . . ? C41B C19B H19D 108.9 . . ? H19C C19B H19D 107.7 . . ? C22B C21B N1B 116.2(12) . . ? C22B C21B H21C 108.2 . . ? N1B C21B H21C 108.2 . . ? C22B C21B H21D 108.2 . . ? N1B C21B H21D 108.2 . . ? H21C C21B H21D 107.4 . . ? C21B C22B N23B 111.8(12) . . ? C21B C22B H22A 109.3 . . ? N23B C22B H22A 109.3 . . ? C21B C22B H22B 109.3 . . ? N23B C22B H22B 109.3 . . ? H22A C22B H22B 107.9 . . ? C24B N23B C22B 120.4(11) . . ? C24B N23B H23B 119.8 . . ? C22B N23B H23B 119.8 . . ? N26B C24B N23B 113.7(11) . . ? N26B C24B S25B 125.0(9) . . ? N23B C24B S25B 121.2(12) . . ? C24B N26B C27B 124.1(9) . . ? C24B N26B H26B 118.0 . . ? C27B N26B H26B 118.0 . . ? N26B C27B C28B 109.2(9) . . ? N26B C27B H27A 109.8 . . ? C28B C27B H27A 109.8 . . ? N26B C27B H27B 109.8 . . ? C28B C27B H27B 109.8 . . ? H27A C27B H27B 108.3 . . ? C27B C28B C29B 115.5(8) . . ? C27B C28B H28C 108.4 . . ? C29B C28B H28C 108.4 . . ? C27B C28B H28D 108.4 . . ? C29B C28B H28D 108.4 . . ? H28C C28B H28D 107.5 . . ? C28B C29B C51B 113.0(8) . . ? C28B C29B H29C 109.0 . . ? C51B C29B H29C 109.0 . . ? C28B C29B H29D 109.0 . . ? C51B C29B H29D 109.0 . . ? H29C C29B H29D 107.8 . . ? N1B C31B C32B 112.4(13) . . ? N1B C31B H31A 109.1 . . ? C32B C31B H31A 109.1 . . ? N1B C31B H31B 109.1 . . ? C32B C31B H31B 109.1 . . ? H31A C31B H31B 107.9 . . ? N33B C32B C31B 114.3(13) . . ? N33B C32B H32A 108.7 . . ? C31B C32B H32A 108.7 . . ? N33B C32B H32B 108.7 . . ? C31B C32B H32B 108.7 . . ? H32A C32B H32B 107.6 . . ? C32B N33B C34B 124.9(13) . . ? C32B N33B H33B 117.5 . . ? C34B N33B H33B 117.5 . . ? N36B C34B N33B 117.8(14) . . ? N36B C34B S35B 122.3(15) . . ? N33B C34B S35B 119.9(13) . . ? C34B N36B C37C 135.0(17) . . ? C34B N36B C37B 118.1(17) . . ? C34B N36B H36B 121.0 . . ? C37C N36B H36B 101.4 . . ? C37B N36B H36B 121.0 . . ? N36B C37B C38B 118.0(18) . . ? N36B C37B H37C 107.8 . . ? C38B C37B H37C 107.8 . . ? N36B C37B H37D 107.8 . . ? C38B C37B H37D 107.8 . . ? H37C C37B H37D 107.1 . . ? N36B C37C C38C 99.1(14) . . ? N36B C37C H37E 112.0 . . ? C38C C37C H37E 112.0 . . ? N36B C37C H37F 112.0 . . ? C38C C37C H37F 112.0 . . ? H37E C37C H37F 109.6 . . ? C39B C38B C37B 114.6(16) . . ? C39B C38B H38C 108.6 . . ? C37B C38B H38C 108.6 . . ? C39B C38B H38D 108.6 . . ? C37B C38B H38D 108.6 . . ? H38C C38B H38D 107.6 . . ? C39C C38C C37C 90.8(12) . . ? C39C C38C H38E 113.5 . . ? C37C C38C H38E 113.5 . . ? C39C C38C H38F 113.5 . . ? C37C C38C H38F 113.5 . . ? H38E C38C H38F 110.8 . . ? C38B C39B C61B 117.9(14) . . ? C38B C39B H39C 107.8 . . ? C61B C39B H39C 107.8 . . ? C38B C39B H39D 107.8 . . ? C61B C39B H39D 107.8 . . ? H39C C39B H39D 107.2 . . ? C61B C39C C38C 101.5(14) . . ? C61B C39C H39E 111.5 . . ? C38C C39C H39E 111.5 . . ? C61B C39C H39F 111.5 . . ? C38C C39C H39F 111.5 . . ? H39E C39C H39F 109.3 . . ? N69B C41B C42B 104.0(8) . . ? N69B C41B C19B 114.0(9) . . ? C42B C41B C19B 111.8(8) . . ? N69B C41B H41B 108.9 . . ? C42B C41B H41B 108.9 . . ? C19B C41B H41B 108.9 . . ? N43B C42B O46B 114.9(8) . . ? N43B C42B C41B 128.7(8) . . ? O46B C42B C41B 116.2(9) . . ? C42B N43B C44B 104.7(7) . . ? N43B C44B C45B 110.0(8) . . ? N43B C44B C48B 121.4(8) . . ? C45B C44B C48B 128.4(8) . . ? C44B C45B O46B 106.6(7) . . ? C44B C45B C47B 136.5(10) . . ? O46B C45B C47B 116.9(8) . . ? C42B O46B C45B 103.9(7) . . ? C45B C47B H47D 109.5 . . ? C45B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C45B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? O50B C48B N49B 123.3(9) . . ? O50B C48B C44B 124.8(7) . . ? N49B C48B C44B 112.0(8) . . ? C48B N49B C51B 122.0(8) . . ? C48B N49B H49B 119.0 . . ? C51B N49B H49B 119.0 . . ? C52B C51B N49B 106.9(8) . . ? C52B C51B C29B 110.8(7) . . ? N49B C51B C29B 110.1(8) . . ? C52B C51B H51B 109.6 . . ? N49B C51B H51B 109.6 . . ? C29B C51B H51B 109.6 . . ? N53B C52B O56B 114.3(8) . . ? N53B C52B C51B 128.6(9) . . ? O56B C52B C51B 117.1(9) . . ? C52B N53B C54B 104.9(9) . . ? C55B C54B N53B 109.0(9) . . ? C55B C54B C58B 129.4(9) . . ? N53B C54B C58B 121.5(10) . . ? C54B C55B O56B 108.4(9) . . ? C54B C55B C57B 135.3(9) . . ? O56B C55B C57B 116.3(11) . . ? C55B O56B C52B 103.4(8) . . ? C55B C57B H57D 109.5 . . ? C55B C57B H57E 109.5 . . ? H57D C57B H57E 109.5 . . ? C55B C57B H57F 109.5 . . ? H57D C57B H57F 109.5 . . ? H57E C57B H57F 109.5 . . ? O60B C58B N59B 125.4(9) . . ? O60B C58B C54B 121.7(11) . . ? N59B C58B C54B 112.8(9) . . ? C58B N59B C61B 124.5(9) . . ? C58B N59B H59B 117.8 . . ? C61B N59B H59B 117.8 . . ? C62B C61B N59B 105.4(7) . . ? C62B C61B C39C 126.4(15) . . ? N59B C61B C39C 112.8(14) . . ? C62B C61B C39B 101.4(11) . . ? N59B C61B C39B 115.2(13) . . ? C62B C61B H61B 111.4 . . ? N59B C61B H61B 111.4 . . ? C39C C61B H61B 88.2 . . ? C39B C61B H61B 111.4 . . ? N63B C62B O66B 113.5(9) . . ? N63B C62B C61B 127.5(10) . . ? O66B C62B C61B 118.8(9) . . ? C62B N63B C64B 104.7(8) . . ? C65B C64B N63B 110.0(9) . . ? C65B C64B C68B 130.1(10) . . ? N63B C64B C68B 119.8(8) . . ? O66B C65B C64B 105.6(9) . . ? O66B C65B C67B 119.2(9) . . ? C64B C65B C67B 135.0(10) . . ? C65B O66B C62B 106.1(8) . . ? C65B C67B H67D 109.5 . . ? C65B C67B H67E 109.5 . . ? H67D C67B H67E 109.5 . . ? C65B C67B H67F 109.5 . . ? H67D C67B H67F 109.5 . . ? H67E C67B H67F 109.5 . . ? O70B C68B N69B 123.2(9) . . ? O70B C68B C64B 120.9(9) . . ? N69B C68B C64B 115.9(10) . . ? C68B N69B C41B 125.7(8) . . ? C68B N69B H69B 117.1 . . ? C41B N69B H69B 117.1 . . ? F3C C1C F2C 107.9(7) . . ? F3C C1C F1C 105.7(9) . . ? F2C C1C F1C 106.9(8) . . ? F3C C1C C2C 111.6(9) . . ? F2C C1C C2C 111.9(9) . . ? F1C C1C C2C 112.5(8) . . ? O2C C2C O1C 130.2(9) . . ? O2C C2C C1C 113.2(10) . . ? O1C C2C C1C 116.3(8) . . ? C2C O2C H2C 109.5 . . ? F2D C1D F1D' 124.1(14) . . ? F2D C1D F1D 112.2(8) . . ? F1D' C1D F3D' 111.4(8) . . ? F1D C1D F3D' 139.4(13) . . ? F2D C1D F3D 109.6(8) . . ? F1D' C1D F3D 71.9(9) . . ? F1D C1D F3D 110.1(8) . . ? F3D' C1D F3D 55.3(8) . . ? F2D C1D F2D' 52.8(8) . . ? F1D' C1D F2D' 108.0(8) . . ? F1D C1D F2D' 73.4(9) . . ? F3D' C1D F2D' 108.5(7) . . ? F3D C1D F2D' 159.8(12) . . ? F2D C1D C2D 117.4(13) . . ? F1D' C1D C2D 117.3(13) . . ? F1D C1D C2D 108.0(14) . . ? F3D' C1D C2D 111.6(13) . . ? F3D C1D C2D 98.7(13) . . ? F2D' C1D C2D 99.0(13) . . ? O1D C2D O2D 133(2) . . ? O1D C2D C1D 114.2(18) . . ? O2D C2D C1D 111.8(17) . . ? C2D O1D H1D 109.5 . . ? O1E C1E H1E1 109.5 . . ? O1E C1E H1E2 109.5 . . ? H1E1 C1E H1E2 109.5 . . ? O1E C1E H1E3 109.5 . . ? H1E1 C1E H1E3 109.5 . . ? H1E2 C1E H1E3 109.5 . . ? C1E O1E H1E 109.5 . . ? C1F O1F H1F 109.5 . . ? O1F C1F H1F1 109.5 . . ? O1F C1F H1F2 109.5 . . ? H1F1 C1F H1F2 109.5 . . ? O1F C1F H1F3 109.5 . . ? H1F1 C1F H1F3 109.5 . . ? H1F2 C1F H1F3 109.5 . . ? O1G C1G H1G1 109.2 . . ? O1G C1G H1G2 108.0 . . ? H1G1 C1G H1G2 109.5 . . ? O1G C1G H1G3 111.2 . . ? H1G1 C1G H1G3 109.5 . . ? H1G2 C1G H1G3 109.5 . . ? C1G O1G H1G 107.6 . . ? C1H O1H H1H 106 . . ? O1I C1I H1I1 109.5 . . ? O1I C1I H1I2 109.5 . . ? H1I1 C1I H1I2 109.5 . . ? O1I C1I H1I3 109.5 . . ? H1I1 C1I H1I3 109.5 . . ? H1I2 C1I H1I3 109.5 . . ? C1I O1I H1I 109.5 . . ? O1J C1J H1J1 109.5 . . ? O1J C1J H1J2 109.5 . . ? H1J1 C1J H1J2 109.5 . . ? O1J C1J H1J3 109.5 . . ? H1J1 C1J H1J3 109.5 . . ? H1J2 C1J H1J3 109.5 . . ? C1J O1J H1J5 109.9 . . ? 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 C31A N1A C11A C12A -65.2(16) . . . . ? C21A N1A C11A C12A 166.2(12) . . . . ? N1A C11A C12A N13A -68.6(18) . . . . ? C11A C12A N13A C14A -86.7(18) . . . . ? C12A N13A C14A N16A 177.0(13) . . . . ? C12A N13A C14A S15A -4(2) . . . . ? N13A C14A N16A C17A 167.1(12) . . . . ? S15A C14A N16A C17A -12.0(19) . . . . ? C14A N16A C17A C18A 137.5(13) . . . . ? N16A C17A C18A C19A -72.4(13) . . . . ? C17A C18A C19A C41A 168.7(11) . . . . ? C31A N1A C21A C22A -62.5(18) . . . . ? C11A N1A C21A C22A 67.0(18) . . . . ? N1A C21A C22A N23A -173.4(12) . . . . ? C21A C22A N23A C24A 80(2) . . . . ? C22A N23A C24A N26A -173.5(13) . . . . ? C22A N23A C24A S25A 15(2) . . . . ? N23A C24A N26A C27A 168.4(15) . . . . ? S25A C24A N26A C27A -20(2) . . . . ? C24A N26A C27A C28A -94(2) . . . . ? N26A C27A C28A C29A 65(2) . . . . ? C27A C28A C29A C51A -177.7(15) . . . . ? C11A N1A C31A C32A 175.6(12) . . . . ? C21A N1A C31A C32A -55.3(16) . . . . ? N1A C31A C32A N33A -58.2(19) . . . . ? C31A C32A N33A C34A 142.5(13) . . . . ? C32A N33A C34A N36A 175.7(11) . . . . ? C32A N33A C34A S35A -4.9(16) . . . . ? N33A C34A N36A C37A 168.9(9) . . . . ? S35A C34A N36A C37A -10.4(14) . . . . ? C34A N36A C37A C38A -83.4(11) . . . . ? N36A C37A C38A C39A -176.4(8) . . . . ? C37A C38A C39A C61A 172.5(8) . . . . ? C18A C19A C41A N69A -76.0(12) . . . . ? C18A C19A C41A C42A 171.2(10) . . . . ? N69A C41A C42A N43A -40.9(14) . . . . ? C19A C41A C42A N43A 76.9(14) . . . . ? N69A C41A C42A O46A 142.1(8) . . . . ? C19A C41A C42A O46A -100.1(10) . . . . ? O46A C42A N43A C44A -1.5(12) . . . . ? C41A C42A N43A C44A -178.6(11) . . . . ? C42A N43A C44A C45A -0.6(13) . . . . ? C42A N43A C44A C48A 179.8(11) . . . . ? N43A C44A C45A O46A 2.3(13) . . . . ? C48A C44A C45A O46A -178.1(12) . . . . ? N43A C44A C45A C47A 176.2(14) . . . . ? C48A C44A C45A C47A -4(3) . . . . ? N43A C42A O46A C45A 2.9(11) . . . . ? C41A C42A O46A C45A -179.7(9) . . . . ? C44A C45A O46A C42A -3.1(12) . . . . ? C47A C45A O46A C42A -178.3(10) . . . . ? C45A C44A C48A O50A 6(2) . . . . ? N43A C44A C48A O50A -174.3(12) . . . . ? C45A C44A C48A N49A -177.6(14) . . . . ? N43A C44A C48A N49A 1.9(17) . . . . ? O50A C48A N49A C51A -7(2) . . . . ? C44A C48A N49A C51A 177.2(11) . . . . ? C48A N49A C51A C52A -127.1(13) . . . . ? C48A N49A C51A C29A 109.1(15) . . . . ? C28A C29A C51A N49A -168.7(13) . . . . ? C28A C29A C51A C52A 73.5(17) . . . . ? N49A C51A C52A N53A -12.7(18) . . . . ? C29A C51A C52A N53A 107.2(14) . . . . ? N49A C51A C52A O56A 168.7(10) . . . . ? C29A C51A C52A O56A -71.3(15) . . . . ? O56A C52A N53A C54A 3.5(14) . . . . ? C51A C52A N53A C54A -175.1(12) . . . . ? C52A N53A C54A C55A -3.2(14) . . . . ? C52A N53A C54A C58A -178.1(11) . . . . ? N53A C54A C55A O56A 1.7(13) . . . . ? C58A C54A C55A O56A 176.2(11) . . . . ? N53A C54A C55A C57A 176.5(13) . . . . ? C58A C54A C55A C57A -9(2) . . . . ? N53A C52A O56A C55A -2.5(14) . . . . ? C51A C52A O56A C55A 176.2(11) . . . . ? C54A C55A O56A C52A 0.3(12) . . . . ? C57A C55A O56A C52A -175.5(11) . . . . ? C55A C54A C58A O60A -3(2) . . . . ? N53A C54A C58A O60A 170.8(11) . . . . ? C55A C54A C58A N59A 176.7(11) . . . . ? N53A C54A C58A N59A -9.3(16) . . . . ? O60A C58A N59A C61A -1.7(16) . . . . ? C54A C58A N59A C61A 178.4(9) . . . . ? C58A N59A C61A C62A -168.4(10) . . . . ? C58A N59A C61A C39A 72.1(13) . . . . ? C38A C39A C61A N59A 56.2(11) . . . . ? C38A C39A C61A C62A -61.8(10) . . . . ? N59A C61A C62A N63A -17.1(14) . . . . ? C39A C61A C62A N63A 105.4(11) . . . . ? N59A C61A C62A O66A 168.2(8) . . . . ? C39A C61A C62A O66A -69.3(11) . . . . ? O66A C62A N63A C64A 0.9(10) . . . . ? C61A C62A N63A C64A -174.2(9) . . . . ? C62A N63A C64A C65A -0.9(10) . . . . ? C62A N63A C64A C68A -174.9(8) . . . . ? N63A C64A C65A O66A 0.6(10) . . . . ? C68A C64A C65A O66A 173.9(9) . . . . ? N63A C64A C65A C67A -175.2(10) . . . . ? C68A C64A C65A C67A -1.9(18) . . . . ? N63A C62A O66A C65A -0.5(10) . . . . ? C61A C62A O66A C65A 175.1(8) . . . . ? C64A C65A O66A C62A -0.1(10) . . . . ? C67A C65A O66A C62A 176.4(8) . . . . ? C65A C64A C68A O70A 9.2(16) . . . . ? N63A C64A C68A O70A -178.4(9) . . . . ? C65A C64A C68A N69A -172.2(10) . . . . ? N63A C64A C68A N69A 0.2(12) . . . . ? O70A C68A N69A C41A -18.9(16) . . . . ? C64A C68A N69A C41A 162.5(9) . . . . ? C19A C41A N69A C68A 105.1(11) . . . . ? C42A C41A N69A C68A -137.6(10) . . . . ? C31B N1B C11B C12B -66.6(18) . . . . ? C21B N1B C11B C12B 163.3(12) . . . . ? N1B C11B C12B N13B -62.5(17) . . . . ? C11B C12B N13B C14B -107.6(18) . . . . ? C12B N13B C14B N16B -177.0(15) . . . . ? C12B N13B C14B S15B -1(3) . . . . ? N13B C14B N16B C17B -178.3(14) . . . . ? S15B C14B N16B C17B 5(2) . . . . ? C14B N16B C17B C18B 104.9(19) . . . . ? N16B C17B C18B C19B -64.5(18) . . . . ? C17B C18B C19B C41B 165.7(11) . . . . ? C31B N1B C21B C22B -63.3(16) . . . . ? C11B N1B C21B C22B 66.8(14) . . . . ? N1B C21B C22B N23B -173.7(9) . . . . ? C21B C22B N23B C24B 71.2(14) . . . . ? C22B N23B C24B N26B -164.1(10) . . . . ? C22B N23B C24B S25B 18.2(14) . . . . ? N23B C24B N26B C27B 171.0(9) . . . . ? S25B C24B N26B C27B -11.4(15) . . . . ? C24B N26B C27B C28B -78.5(12) . . . . ? N26B C27B C28B C29B -170.6(9) . . . . ? C27B C28B C29B C51B -175.3(9) . . . . ? C21B N1B C31B C32B -56.2(17) . . . . ? C11B N1B C31B C32B 173.0(13) . . . . ? N1B C31B C32B N33B -57.5(18) . . . . ? C31B C32B N33B C34B 142.0(12) . . . . ? C32B N33B C34B N36B -177.7(11) . . . . ? C32B N33B C34B S35B -0.3(15) . . . . ? N33B C34B N36B C37C 165.7(14) . . . . ? S35B C34B N36B C37C -12(2) . . . . ? N33B C34B N36B C37B -172.0(12) . . . . ? S35B C34B N36B C37B 10.7(16) . . . . ? C34B N36B C37B C38B -100(2) . . . . ? C37C N36B C37B C38B 40(3) . . . . ? C34B N36B C37C C38C -93(2) . . . . ? C37B N36B C37C C38C -147(5) . . . . ? N36B C37B C38B C39B -54(3) . . . . ? N36B C37C C38C C39C 176(2) . . . . ? C37B C38B C39B C61B 178(2) . . . . ? C37C C38C C39C C61B 176(2) . . . . ? C18B C19B C41B N69B -59.1(13) . . . . ? C18B C19B C41B C42B -176.8(10) . . . . ? N69B C41B C42B N43B -12.0(13) . . . . ? C19B C41B C42B N43B 111.5(12) . . . . ? N69B C41B C42B O46B 163.0(8) . . . . ? C19B C41B C42B O46B -73.5(11) . . . . ? O46B C42B N43B C44B 1.2(11) . . . . ? C41B C42B N43B C44B 176.2(9) . . . . ? C42B N43B C44B C45B -0.4(11) . . . . ? C42B N43B C44B C48B -175.3(8) . . . . ? N43B C44B C45B O46B -0.4(10) . . . . ? C48B C44B C45B O46B 174.0(9) . . . . ? N43B C44B C45B C47B 177.4(11) . . . . ? C48B C44B C45B C47B -8.2(19) . . . . ? N43B C42B O46B C45B -1.4(10) . . . . ? C41B C42B O46B C45B -177.0(8) . . . . ? C44B C45B O46B C42B 1.0(9) . . . . ? C47B C45B O46B C42B -177.3(9) . . . . ? N43B C44B C48B O50B 169.3(9) . . . . ? C45B C44B C48B O50B -4.5(16) . . . . ? N43B C44B C48B N49B -9.8(12) . . . . ? C45B C44B C48B N49B 176.4(9) . . . . ? O50B C48B N49B C51B -7.5(14) . . . . ? C44B C48B N49B C51B 171.6(8) . . . . ? C48B N49B C51B C52B -157.8(8) . . . . ? C48B N49B C51B C29B 81.7(10) . . . . ? C28B C29B C51B C52B -57.8(12) . . . . ? C28B C29B C51B N49B 60.3(10) . . . . ? N49B C51B C52B N53B -4.9(14) . . . . ? C29B C51B C52B N53B 115.1(11) . . . . ? N49B C51B C52B O56B 173.9(7) . . . . ? C29B C51B C52B O56B -66.1(12) . . . . ? O56B C52B N53B C54B 1.0(11) . . . . ? C51B C52B N53B C54B 179.8(10) . . . . ? C52B N53B C54B C55B -1.3(11) . . . . ? C52B N53B C54B C58B -178.8(9) . . . . ? N53B C54B C55B O56B 1.1(11) . . . . ? C58B C54B C55B O56B 178.3(9) . . . . ? N53B C54B C55B C57B -178.7(11) . . . . ? C58B C54B C55B C57B -1(2) . . . . ? C54B C55B O56B C52B -0.5(10) . . . . ? C57B C55B O56B C52B 179.4(9) . . . . ? N53B C52B O56B C55B -0.4(10) . . . . ? C51B C52B O56B C55B -179.3(8) . . . . ? C55B C54B C58B O60B -1.5(16) . . . . ? N53B C54B C58B O60B 175.5(9) . . . . ? C55B C54B C58B N59B -178.1(10) . . . . ? N53B C54B C58B N59B -1.1(13) . . . . ? O60B C58B N59B C61B -10.2(15) . . . . ? C54B C58B N59B C61B 166.3(8) . . . . ? C58B N59B C61B C62B -141.1(10) . . . . ? C58B N59B C61B C39C 77.3(16) . . . . ? C58B N59B C61B C39B 108.0(14) . . . . ? C38C C39C C61B C62B -60(2) . . . . ? C38C C39C C61B N59B 72(2) . . . . ? C38C C39C C61B C39B -30(3) . . . . ? C38B C39B C61B C62B -174(2) . . . . ? C38B C39B C61B N59B -61(3) . . . . ? C38B C39B C61B C39C 31(3) . . . . ? N59B C61B C62B N63B -29.6(16) . . . . ? C39C C61B C62B N63B 105.1(17) . . . . ? C39B C61B C62B N63B 90.8(17) . . . . ? N59B C61B C62B O66B 156.3(9) . . . . ? C39C C61B C62B O66B -69.0(18) . . . . ? C39B C61B C62B O66B -83.2(16) . . . . ? O66B C62B N63B C64B -0.5(12) . . . . ? C61B C62B N63B C64B -174.8(11) . . . . ? C62B N63B C64B C65B -2.1(13) . . . . ? C62B N63B C64B C68B -179.2(10) . . . . ? N63B C64B C65B O66B 3.8(14) . . . . ? C68B C64B C65B O66B -179.6(11) . . . . ? N63B C64B C65B C67B 178.9(16) . . . . ? C68B C64B C65B C67B -4(3) . . . . ? C64B C65B O66B C62B -3.9(13) . . . . ? C67B C65B O66B C62B -180.0(13) . . . . ? N63B C62B O66B C65B 2.8(13) . . . . ? C61B C62B O66B C65B 177.7(10) . . . . ? C65B C64B C68B O70B -6(2) . . . . ? N63B C64B C68B O70B 170.6(11) . . . . ? C65B C64B C68B N69B 174.9(13) . . . . ? N63B C64B C68B N69B -8.7(15) . . . . ? O70B C68B N69B C41B -0.3(17) . . . . ? C64B C68B N69B C41B 179.0(9) . . . . ? C42B C41B N69B C68B -137.8(10) . . . . ? C19B C41B N69B C68B 100.2(12) . . . . ? F3C C1C C2C O2C -92.7(11) . . . . ? F2C C1C C2C O2C 146.3(9) . . . . ? F1C C1C C2C O2C 26.0(14) . . . . ? F3C C1C C2C O1C 82.3(12) . . . . ? F2C C1C C2C O1C -38.7(14) . . . . ? F1C C1C C2C O1C -159.0(10) . . . . ? F2D C1D C2D O1D 60(2) . . . . ? F1D' C1D C2D O1D -131.4(15) . . . . ? F1D C1D C2D O1D -171.8(15) . . . . ? F3D' C1D C2D O1D -1(2) . . . . ? F3D C1D C2D O1D -57.3(17) . . . . ? F2D' C1D C2D O1D 112.9(17) . . . . ? F2D C1D C2D O2D -109.2(16) . . . . ? F1D' C1D C2D O2D 59.2(19) . . . . ? F1D C1D C2D O2D 18.8(18) . . . . ? F3D' C1D C2D O2D -170.6(14) . . . . ? F3D C1D C2D O2D 133.3(15) . . . . ? F2D' C1D C2D O2D -56.5(16) . . . . ? 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 N13A H13A S35B 0.88 2.74 3.544(13) 152.6 . N16A H16A O1C 0.88 2.03 2.890(12) 164.8 . N23A H23A O1J 0.88 2.18 2.95(2) 146.8 2_656 N26A H26A S25B 0.88 2.99 3.662(16) 135.1 1_655 N33A H33A S35B 0.88 2.64 3.504(12) 165.6 . N36A H36A F1C 0.88 2.39 3.144(9) 143.8 . N36A H36A O2C 0.88 2.59 3.046(11) 113.0 . N49A H49A N43A 0.88 2.22 2.701(11) 113.8 . N59A H59A N63A 0.88 2.33 2.780(11) 111.5 . N13B H13B S25A 0.88 2.80 3.450(14) 132.2 2_647 N16B H16C O1D 0.88 2.16 2.922(19) 144.5 . N23B H23B O1C 0.88 2.26 2.866(13) 126.1 . N26B H26B O70A 0.88 2.53 3.289(13) 144.4 . N33B H33B S25A 0.88 2.75 3.569(14) 154.6 2_647 N36B H36B O2D 0.88 2.03 2.878(18) 161.9 . O2C H2C O1E 0.84 1.89 2.648(10) 149.2 . O1D H1D O1F 0.84 1.91 2.661(18) 148.3 . O1E H1E N1A 0.84 1.96 2.743(13) 153.9 . O1F H1F N1B 0.84 1.95 2.789(13) 172.3 . O1G H1G O1I 0.82 1.60 2.05(3) 112.1 2_656 O1G H1G O1H 0.82 2.04 2.85(4) 168.5 . O2W H1I3 O1I 1.22 1.97 2.87(3) 126.1 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 21.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.998 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.085 #####END Data_lj297sad _database_code_depnum_ccdc_archive 'CCDC 783200' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H162 N25 O31.50 S6' _chemical_formula_sum 'C92 H162 N25 O31.50 S6' _chemical_formula_weight 2314.83 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 P1 _symmetry_space_group_name_Hall 'P 1' _symmetry_Intl_tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 13.8640(12) _cell_length_b 14.5750(10) _cell_length_c 16.8430(12) _cell_angle_alpha 69.705(5) _cell_angle_beta 77.952(3) _cell_angle_gamma 75.179(3) _cell_volume 3058.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2348 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 19.323 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1241 _exptl_absorpt_coefficient_mu 0.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5797 _exptl_absorpt_correction_T_max 0.7445 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEXII-FR591 _diffrn_measurement_method \w+\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 62257 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 20.91 _reflns_number_total 12759 _reflns_number_gt 10214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.0747P)^2^+0.9979P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration syn _refine_ls_abs_structure_Flack 0.01(7) _refine_ls_number_reflns 12759 _refine_ls_number_parameters 1531 _refine_ls_number_restraints 83 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _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 0.2586(5) 1.0038(4) 0.8592(4) 0.0222(14) Uani 1 1 d . . . C2 C 0.1993(5) 0.9277(4) 0.9911(4) 0.0249(16) Uani 1 1 d . . . C3 C 0.3005(5) 0.8955(4) 0.9782(3) 0.0201(14) Uani 1 1 d . . . C4 C 0.1188(5) 0.9060(5) 1.0644(4) 0.0303(16) Uani 1 1 d . . . H4A H 0.0829 0.9682 1.0760 0.046 Uiso 1 1 calc R . . H4B H 0.1489 0.8596 1.1149 0.046 Uiso 1 1 calc R . . H4C H 0.0716 0.8758 1.0505 0.046 Uiso 1 1 calc R . . C5 C 0.3698(5) 0.8242(4) 1.0370(4) 0.0239(15) Uani 1 1 d . . . C6 C 0.5511(4) 0.7471(4) 1.0392(4) 0.0280(16) Uani 1 1 d . . . H6 H 0.5373 0.7395 1.1016 0.034 Uiso 1 1 calc R . . C7 C 0.6371(5) 0.8019(4) 0.9974(4) 0.0302(16) Uani 1 1 d . . . C8 C 0.7734(5) 0.8541(5) 0.9865(4) 0.0384(18) Uani 1 1 d . . . C9 C 0.7426(5) 0.8845(4) 0.9089(4) 0.0284(16) Uani 1 1 d . . . C10 C 0.8571(6) 0.8668(6) 1.0211(5) 0.057(2) Uani 1 1 d . . . H10A H 0.8975 0.9094 0.9753 0.085 Uiso 1 1 calc R . . H10B H 0.8995 0.8014 1.0448 0.085 Uiso 1 1 calc R . . H10C H 0.8298 0.8980 1.0663 0.085 Uiso 1 1 calc R . . C11 C 0.7827(5) 0.9471(5) 0.8273(4) 0.0332(17) Uani 1 1 d . . . C12 C 0.7414(5) 1.0386(4) 0.6791(4) 0.0285(16) Uani 1 1 d . . . H12 H 0.7931 1.0763 0.6775 0.034 Uiso 1 1 calc R . . C13 C 0.6428(5) 1.1087(5) 0.6666(4) 0.0238(15) Uani 1 1 d U . . C14 C 0.5371(5) 1.2460(4) 0.6155(4) 0.0253(15) Uani 1 1 d . . . C15 C 0.4859(5) 1.1756(4) 0.6671(4) 0.0259(16) Uani 1 1 d . . . C16 C 0.5082(5) 1.3523(4) 0.5614(4) 0.0337(17) Uani 1 1 d . . . H16A H 0.4347 1.3731 0.5681 0.051 Uiso 1 1 calc R . . H16B H 0.5335 1.3581 0.5013 0.051 Uiso 1 1 calc R . . H16C H 0.5374 1.3952 0.5793 0.051 Uiso 1 1 calc R . . C17 C 0.3774(5) 1.1780(5) 0.6911(4) 0.0253(15) Uani 1 1 d . . . C18 C 0.2553(4) 1.0680(4) 0.7707(4) 0.0253(15) Uani 1 1 d . . . H18 H 0.2076 1.1326 0.7698 0.030 Uiso 1 1 calc R . . C19 C 0.5783(5) 0.6429(4) 1.0257(4) 0.0317(16) Uani 1 1 d . . . H19A H 0.5879 0.6516 0.9638 0.038 Uiso 1 1 calc R . . H19B H 0.6426 0.6058 1.0479 0.038 Uiso 1 1 calc R . . C20 C 0.4980(5) 0.5831(4) 1.0698(4) 0.0329(16) Uani 1 1 d . . . H20A H 0.4314 0.6264 1.0585 0.040 Uiso 1 1 calc R . . H20B H 0.4998 0.5607 1.1322 0.040 Uiso 1 1 calc R . . C21 C 0.5103(5) 0.4920(5) 1.0408(4) 0.0359(17) Uani 1 1 d . . . H21A H 0.5803 0.4534 1.0434 0.043 Uiso 1 1 calc R . . H21B H 0.4644 0.4481 1.0789 0.043 Uiso 1 1 calc R . . C22 C 0.5007(5) 0.4672(5) 0.9041(4) 0.0322(16) Uani 1 1 d . . . C23 C 0.4784(5) 0.4609(5) 0.7624(4) 0.0340(17) Uani 1 1 d . . . H23A H 0.4155 0.4378 0.7676 0.041 Uiso 1 1 calc R . . H23B H 0.5342 0.4019 0.7719 0.041 Uiso 1 1 calc R . . C24 C 0.7744(4) 0.9889(5) 0.6082(4) 0.0294(16) Uani 1 1 d . . . H24A H 0.7194 0.9582 0.6062 0.035 Uiso 1 1 calc R . . H24B H 0.7844 1.0413 0.5527 0.035 Uiso 1 1 calc R . . C25 C 0.8690(5) 0.9105(5) 0.6186(4) 0.0335(16) Uani 1 1 d . . . H25A H 0.8590 0.8568 0.6732 0.040 Uiso 1 1 calc R . . H25B H 0.9243 0.9404 0.6216 0.040 Uiso 1 1 calc R . . C26 C 0.8997(5) 0.8652(5) 0.5448(4) 0.0371(17) Uani 1 1 d . . . H26A H 0.9171 0.9174 0.4912 0.044 Uiso 1 1 calc R . . H26B H 0.9604 0.8117 0.5561 0.044 Uiso 1 1 calc R . . C27 C 0.8206(5) 0.7288(4) 0.5474(4) 0.0253(15) Uani 1 1 d . . . C28 C 0.7257(5) 0.6211(4) 0.5192(4) 0.0318(16) Uani 1 1 d . . . H28A H 0.7741 0.5634 0.5501 0.038 Uiso 1 1 calc R . . H28B H 0.7383 0.6247 0.4582 0.038 Uiso 1 1 calc R . . C29 C 0.2202(5) 1.0185(4) 0.7179(4) 0.0260(15) Uani 1 1 d . . . H29A H 0.2704 0.9576 0.7142 0.031 Uiso 1 1 calc R . . H29B H 0.1555 0.9983 0.7468 0.031 Uiso 1 1 calc R . . C30 C 0.2067(4) 1.0889(4) 0.6286(4) 0.0239(15) Uani 1 1 d . . . H30A H 0.1536 1.1477 0.6329 0.029 Uiso 1 1 calc R . . H30B H 0.2702 1.1128 0.6020 0.029 Uiso 1 1 calc R . . C31 C 0.1792(5) 1.0430(5) 0.5722(4) 0.0289(16) Uani 1 1 d U . . H31A H 0.1184 1.0145 0.5999 0.035 Uiso 1 1 calc R . . H31B H 0.1637 1.0946 0.5175 0.035 Uiso 1 1 calc R . . C32 C 0.2558(5) 0.8916(5) 0.5282(4) 0.0257(15) Uani 1 1 d . . . C33 C 0.3550(4) 0.7316(4) 0.5017(4) 0.0251(15) Uani 1 1 d . . . H33A H 0.3711 0.7454 0.4391 0.030 Uiso 1 1 calc R . . H33B H 0.2925 0.7045 0.5211 0.030 Uiso 1 1 calc R . . C34 C 0.4990(5) 0.5338(4) 0.6726(4) 0.0274(16) Uani 1 1 d . . . C35 C 0.5999(5) 0.5426(4) 0.6391(4) 0.0285(16) Uani 1 1 d . . . C36 C 0.6192(5) 0.6074(4) 0.5558(4) 0.0256(15) Uani 1 1 d . . . C37 C 0.5390(5) 0.6640(4) 0.5099(4) 0.0268(16) Uani 1 1 d . . . C38 C 0.4398(5) 0.6587(4) 0.5455(4) 0.0212(15) Uani 1 1 d . . . C39 C 0.4186(5) 0.5932(5) 0.6275(4) 0.0257(16) Uani 1 1 d . . . C40 C 0.6843(5) 0.4824(5) 0.6897(4) 0.0389(18) Uani 1 1 d . . . H40A H 0.6586 0.4671 0.7514 0.047 Uiso 1 1 calc R . . H40B H 0.7365 0.5227 0.6775 0.047 Uiso 1 1 calc R . . C41 C 0.7328(5) 0.3836(5) 0.6694(5) 0.0448(19) Uani 1 1 d . . . H41A H 0.6871 0.3366 0.6946 0.067 Uiso 1 1 calc R . . H41B H 0.7965 0.3548 0.6933 0.067 Uiso 1 1 calc R . . H41C H 0.7455 0.3970 0.6073 0.067 Uiso 1 1 calc R . . C42 C 0.5609(5) 0.7342(5) 0.4202(4) 0.0332(16) Uani 1 1 d . . . H42A H 0.6273 0.7512 0.4143 0.040 Uiso 1 1 calc R . . H42B H 0.5097 0.7969 0.4130 0.040 Uiso 1 1 calc R . . C43 C 0.5614(6) 0.6923(5) 0.3487(4) 0.049(2) Uani 1 1 d . . . H43A H 0.6074 0.6272 0.3579 0.073 Uiso 1 1 calc R . . H43B H 0.5837 0.7383 0.2936 0.073 Uiso 1 1 calc R . . H43C H 0.4933 0.6843 0.3486 0.073 Uiso 1 1 calc R . . C44 C 0.3094(4) 0.5914(5) 0.6675(4) 0.0319(16) Uani 1 1 d . . . H44A H 0.2696 0.6606 0.6534 0.038 Uiso 1 1 calc R . . H44B H 0.3064 0.5642 0.7304 0.038 Uiso 1 1 calc R . . C45 C 0.2621(5) 0.5274(5) 0.6357(4) 0.0412(18) Uani 1 1 d . . . H45A H 0.2669 0.5528 0.5733 0.062 Uiso 1 1 calc R . . H45B H 0.1912 0.5311 0.6604 0.062 Uiso 1 1 calc R . . H45C H 0.2982 0.4579 0.6532 0.062 Uiso 1 1 calc R . . C46 C -0.1103(5) 0.1329(4) 0.0971(4) 0.0269(15) Uani 1 1 d . . . C47 C -0.1369(5) 0.1709(5) -0.0336(4) 0.0309(16) Uani 1 1 d . . . C48 C -0.0453(5) 0.1864(4) -0.0319(4) 0.0236(15) Uani 1 1 d . . . C49 C -0.1968(5) 0.1825(6) -0.1003(4) 0.050(2) Uani 1 1 d . . . H49A H -0.1688 0.2247 -0.1552 0.075 Uiso 1 1 calc R . . H49B H -0.2666 0.2137 -0.0854 0.075 Uiso 1 1 calc R . . H49C H -0.1948 0.1167 -0.1048 0.075 Uiso 1 1 calc R . . C50 C 0.0315(5) 0.2235(4) -0.1011(4) 0.0294(16) Uani 1 1 d . . . C51 C 0.2021(4) 0.2653(4) -0.1294(4) 0.0265(15) Uani 1 1 d . . . H51 H 0.2039 0.2574 -0.1864 0.032 Uiso 1 1 calc R . . C52 C 0.2884(5) 0.1939(5) -0.0882(4) 0.0273(16) Uani 1 1 d U . . C53 C 0.4467(5) 0.1292(5) -0.0737(4) 0.0271(16) Uani 1 1 d . . . C54 C 0.3882(5) 0.0905(4) -0.0030(4) 0.0271(16) Uani 1 1 d . . . C55 C 0.5550(5) 0.1147(5) -0.1035(4) 0.0417(18) Uani 1 1 d . . . H55A H 0.5919 0.0702 -0.0562 0.063 Uiso 1 1 calc R . . H55B H 0.5758 0.1793 -0.1246 0.063 Uiso 1 1 calc R . . H55C H 0.5697 0.0849 -0.1498 0.063 Uiso 1 1 calc R . . C56 C 0.4209(7) 0.0110(5) 0.0762(4) 0.0379(18) Uani 1 1 d . . . C57 C 0.3453(5) -0.0811(5) 0.2211(4) 0.048(2) Uani 1 1 d D . . H57 H 0.3831 -0.1420 0.2053 0.057 Uiso 1 1 calc R A 1 C58 C 0.2430(5) -0.1035(5) 0.2535(4) 0.0298(17) Uani 1 1 d . B . C59 C 0.1290(5) -0.1883(5) 0.3317(4) 0.0269(16) Uani 1 1 d . B . C60 C 0.0844(5) -0.0986(5) 0.2853(4) 0.0257(15) Uani 1 1 d . B . C61 C 0.0965(5) -0.2777(5) 0.3950(4) 0.0347(17) Uani 1 1 d . . . H61A H 0.0229 -0.2672 0.4030 0.052 Uiso 1 1 calc R . . H61B H 0.1198 -0.2898 0.4495 0.052 Uiso 1 1 calc R . . H61C H 0.1252 -0.3356 0.3746 0.052 Uiso 1 1 calc R . . C62 C -0.0240(6) -0.0543(5) 0.2773(4) 0.0320(17) Uani 1 1 d . . . C63 C -0.1353(5) 0.0957(5) 0.1935(4) 0.0313(16) Uani 1 1 d . . . H63 H -0.1832 0.0493 0.2093 0.038 Uiso 1 1 calc R . . C64 C 0.2043(5) 0.3724(4) -0.1421(4) 0.0345(17) Uani 1 1 d . . . H64A H 0.2593 0.3933 -0.1879 0.041 Uiso 1 1 calc R . . H64B H 0.1400 0.4154 -0.1606 0.041 Uiso 1 1 calc R . . C65 C 0.2194(5) 0.3867(5) -0.0642(4) 0.0400(18) Uani 1 1 d . . . H65A H 0.2876 0.3504 -0.0501 0.048 Uiso 1 1 calc R . . H65B H 0.1701 0.3570 -0.0166 0.048 Uiso 1 1 calc R . . C66 C 0.2081(6) 0.4985(5) -0.0711(4) 0.0443(18) Uani 1 1 d . . . H66A H 0.2555 0.5305 -0.1194 0.053 Uiso 1 1 calc R . . H66B H 0.1387 0.5354 -0.0805 0.053 Uiso 1 1 calc R . . C67 C 0.1966(5) 0.5748(5) 0.0426(4) 0.0349(17) Uani 1 1 d . . . C68 C 0.1911(6) 0.6157(5) 0.1772(4) 0.0431(19) Uani 1 1 d . . . H68A H 0.1332 0.6695 0.1573 0.052 Uiso 1 1 calc R M . H68B H 0.2471 0.6467 0.1769 0.052 Uiso 1 1 calc R . . C69 C 0.4109(7) -0.0718(6) 0.2755(7) 0.050(3) Uani 0.75 1 d PD B 1 H69A H 0.4789 -0.0654 0.2441 0.060 Uiso 0.75 1 calc PR B 1 H69B H 0.4171 -0.1302 0.3277 0.060 Uiso 0.75 1 calc PR B 1 C70 C 0.3580(7) 0.0214(7) 0.2970(5) 0.047(3) Uani 0.75 1 d PD B 1 H70A H 0.2934 0.0114 0.3339 0.056 Uiso 0.75 1 calc PR B 1 H70B H 0.3437 0.0773 0.2443 0.056 Uiso 0.75 1 calc PR B 1 C71 C 0.4317(9) 0.0460(11) 0.3468(12) 0.068(3) Uani 0.75 1 d PD B 1 H71A H 0.4520 -0.0113 0.3969 0.082 Uiso 0.75 1 calc PR B 1 H71B H 0.4925 0.0660 0.3085 0.082 Uiso 0.75 1 calc PR B 1 C69A C 0.350(2) -0.033(3) 0.2903(17) 0.050(3) Uani 0.25 1 d PD B 2 H69C H 0.2901 0.0219 0.2904 0.060 Uiso 0.25 1 calc PR B 2 H69D H 0.3451 -0.0838 0.3472 0.060 Uiso 0.25 1 calc PR B 2 C70A C 0.4454(19) 0.010(2) 0.2771(15) 0.047(3) Uani 0.25 1 d PD B 2 H70C H 0.5061 -0.0424 0.2718 0.056 Uiso 0.25 1 calc PR B 2 H70D H 0.4468 0.0667 0.2238 0.056 Uiso 0.25 1 calc PR B 2 C71A C 0.4455(18) 0.044(3) 0.354(3) 0.068(3) Uani 0.25 1 d PD B 2 H71C H 0.4428 -0.0145 0.4057 0.082 Uiso 0.25 1 calc PR B 2 H71D H 0.5115 0.0625 0.3471 0.082 Uiso 0.25 1 calc PR B 2 C72 C 0.3828(5) 0.1925(5) 0.4073(4) 0.0295(16) Uani 1 1 d . B . C73 C 0.2957(5) 0.3483(4) 0.4448(4) 0.0294(16) Uani 1 1 d . B . H73A H 0.3607 0.3708 0.4266 0.035 Uiso 1 1 calc R . . H73B H 0.2783 0.3347 0.5073 0.035 Uiso 1 1 calc R . . C74 C -0.1811(5) 0.1810(4) 0.2307(4) 0.0331(16) Uani 1 1 d . . . H74A H -0.2409 0.2218 0.2028 0.040 Uiso 1 1 calc R . . H74B H -0.1316 0.2243 0.2179 0.040 Uiso 1 1 calc R . . C75 C -0.2120(5) 0.1447(4) 0.3271(4) 0.0276(15) Uani 1 1 d . . . H75A H -0.2677 0.1088 0.3392 0.033 Uiso 1 1 calc R . . H75B H -0.1543 0.0966 0.3541 0.033 Uiso 1 1 calc R . . C76 C -0.2451(5) 0.2268(5) 0.3675(4) 0.0299(16) Uani 1 1 d . . . H76A H -0.2971 0.2797 0.3365 0.036 Uiso 1 1 calc R . . H76B H -0.2750 0.2000 0.4275 0.036 Uiso 1 1 calc R . . C77 C -0.1652(4) 0.3542(5) 0.3826(4) 0.0256(15) Uani 1 1 d . . . C78 C -0.0698(5) 0.4613(5) 0.4088(5) 0.0376(18) Uani 1 1 d . . . H78A H -0.0851 0.4479 0.4714 0.045 Uiso 1 1 calc R . . H78B H -0.1174 0.5220 0.3810 0.045 Uiso 1 1 calc R . . C79 C 0.1615(5) 0.5486(4) 0.2672(4) 0.0299(16) Uani 1 1 d . M . C80 C 0.2393(5) 0.4907(4) 0.3166(4) 0.0287(16) Uani 1 1 d . . . C81 C 0.2129(5) 0.4269(4) 0.3979(4) 0.0291(16) Uani 1 1 d . B . C82 C 0.1119(5) 0.4196(4) 0.4308(4) 0.0248(15) Uani 1 1 d . . . C83 C 0.0370(5) 0.4764(4) 0.3787(4) 0.0275(16) Uani 1 1 d . M . C84 C 0.0611(5) 0.5393(4) 0.2965(4) 0.0291(16) Uani 1 1 d . . . C85 C 0.3473(5) 0.4932(5) 0.2819(4) 0.0384(18) Uani 1 1 d . M . H85A H 0.3538 0.5197 0.2188 0.046 Uiso 1 1 calc R . . H85B H 0.3874 0.4242 0.2976 0.046 Uiso 1 1 calc R . . C86 C 0.3904(5) 0.5587(5) 0.3162(5) 0.052(2) Uani 1 1 d . . . H86A H 0.3593 0.6291 0.2921 0.078 Uiso 1 1 calc R M . H86B H 0.4634 0.5495 0.2995 0.078 Uiso 1 1 calc R . . H86C H 0.3755 0.5388 0.3786 0.078 Uiso 1 1 calc R . . C87 C 0.0870(5) 0.3487(5) 0.5173(4) 0.0380(18) Uani 1 1 d . M . H87A H 0.1404 0.2876 0.5262 0.046 Uiso 1 1 calc R . . H87B H 0.0231 0.3291 0.5189 0.046 Uiso 1 1 calc R . . C88 C 0.0764(6) 0.3903(6) 0.5898(4) 0.058(2) Uani 1 1 d . . . H88A H 0.1388 0.4112 0.5882 0.087 Uiso 1 1 calc R M . H88B H 0.0633 0.3389 0.6443 0.087 Uiso 1 1 calc R . . H88C H 0.0203 0.4480 0.5840 0.087 Uiso 1 1 calc R . . C89 C -0.0215(5) 0.5948(5) 0.2398(4) 0.0398(18) Uani 1 1 d . M . H89A H -0.0726 0.5533 0.2529 0.048 Uiso 1 1 calc R . . H89B H 0.0080 0.6051 0.1793 0.048 Uiso 1 1 calc R . . C90 C -0.0730(6) 0.6964(5) 0.2522(5) 0.060(2) Uani 1 1 d . . . H90A H -0.1010 0.6868 0.3123 0.090 Uiso 1 1 calc R M . H90B H -0.1272 0.7278 0.2164 0.090 Uiso 1 1 calc R . . H90C H -0.0235 0.7395 0.2358 0.090 Uiso 1 1 calc R . . N1 N 0.3370(4) 0.9441(4) 0.8931(3) 0.0265(12) Uani 1 1 d . . . N2 N 0.4645(4) 0.8078(3) 0.9978(3) 0.0264(12) Uani 1 1 d . . . H2 H 0.4747 0.8365 0.9422 0.032 Uiso 1 1 calc R . . N3 N 0.6539(4) 0.8497(4) 0.9173(3) 0.0287(13) Uani 1 1 d . . . N4 N 0.7282(4) 0.9651(3) 0.7637(3) 0.0272(12) Uani 1 1 d . . . H4 H 0.6813 0.9301 0.7739 0.033 Uiso 1 1 calc R . . N5 N 0.5560(4) 1.0861(4) 0.7002(3) 0.0293(13) Uani 1 1 d . . . N6 N 0.3557(4) 1.0876(4) 0.7359(3) 0.0256(12) Uani 1 1 d . . . H6A H 0.4064 1.0363 0.7448 0.031 Uiso 1 1 calc R . . N7 N 0.4869(4) 0.5257(4) 0.9527(3) 0.0335(13) Uani 1 1 d . . . H7 H 0.4618 0.5895 0.9304 0.040 Uiso 1 1 calc R . . N8 N 0.4689(4) 0.5104(4) 0.8273(3) 0.0348(14) Uani 1 1 d . . . H8 H 0.4398 0.5740 0.8145 0.042 Uiso 1 1 calc R . . N9 N 0.8205(4) 0.8243(4) 0.5341(3) 0.0323(13) Uani 1 1 d . . . H9 H 0.7660 0.8675 0.5168 0.039 Uiso 1 1 calc R . . N10 N 0.7398(4) 0.7132(4) 0.5277(4) 0.0455(16) Uani 1 1 d . . . H10 H 0.6886 0.7641 0.5188 0.055 Uiso 1 1 calc R . . N11 N 0.2625(4) 0.9644(4) 0.5559(3) 0.0275(12) Uani 1 1 d . . . H11 H 0.3223 0.9653 0.5653 0.033 Uiso 1 1 calc R . . N12 N 0.3418(4) 0.8228(4) 0.5238(3) 0.0283(13) Uani 1 1 d . . . H12A H 0.3957 0.8344 0.5356 0.034 Uiso 1 1 calc R . . N13 N -0.0298(4) 0.1620(4) 0.0543(3) 0.0281(12) Uani 1 1 d . . . N14 N 0.1108(4) 0.2353(3) -0.0741(3) 0.0267(12) Uani 1 1 d . . . H14 H 0.1079 0.2242 -0.0189 0.032 Uiso 1 1 calc R . . N15 N 0.2868(4) 0.1320(4) -0.0125(3) 0.0280(13) Uani 1 1 d . . . N16 N 0.3397(5) -0.0042(4) 0.1380(3) 0.0399(15) Uani 1 1 d . B . H16 H 0.2808 0.0345 0.1269 0.048 Uiso 1 1 calc R . . N17 N 0.1579(4) -0.0421(4) 0.2361(3) 0.0302(13) Uani 1 1 d . . . N18 N -0.0392(4) 0.0405(4) 0.2244(3) 0.0334(13) Uani 1 1 d . . . H18A H 0.0120 0.0712 0.2075 0.040 Uiso 1 1 calc R . . N19 N 0.2309(5) 0.4991(4) 0.0097(3) 0.0476(16) Uani 1 1 d . M . H19 H 0.2702 0.4457 0.0390 0.057 Uiso 1 1 calc R . . N20 N 0.2226(4) 0.5522(4) 0.1216(3) 0.0444(16) Uani 1 1 d . M . H20 H 0.2621 0.4938 0.1413 0.053 Uiso 1 1 calc R . . N21 N 0.3648(4) 0.1302(4) 0.3725(4) 0.0501(17) Uani 1 1 d D . . H21 H 0.3021 0.1412 0.3632 0.060 Uiso 1 1 calc R B 1 N22 N 0.3014(4) 0.2595(4) 0.4215(3) 0.0353(14) Uani 1 1 d . . . H22 H 0.2437 0.2488 0.4162 0.042 Uiso 1 1 calc R B . N23 N -0.1581(4) 0.2692(4) 0.3646(3) 0.0368(14) Uani 1 1 d . . . H23 H -0.0976 0.2369 0.3503 0.044 Uiso 1 1 calc R . . N24 N -0.0798(4) 0.3753(4) 0.3858(4) 0.0421(15) Uani 1 1 d . . . H24 H -0.0239 0.3349 0.3734 0.051 Uiso 1 1 calc R . . O1 O 0.1710(3) 0.9975(3) 0.9147(2) 0.0234(10) Uani 1 1 d . . . C1A C 0.7231(8) 0.6792(7) 0.7895(6) 0.081(3) Uani 1 1 d . . . H1A1 H 0.7593 0.7101 0.8142 0.122 Uiso 1 1 calc R . . H1A2 H 0.7631 0.6687 0.7370 0.122 Uiso 1 1 calc R . . H1A3 H 0.7119 0.6148 0.8305 0.122 Uiso 1 1 calc R . . N1A N 0.5518(8) 0.7969(8) 0.7558(6) 0.108(3) Uani 1 1 d . . . C2A C 0.6275(10) 0.7439(8) 0.7702(6) 0.081(3) Uani 1 1 d . . . O2 O 0.3434(3) 0.7840(3) 1.1130(3) 0.0300(10) Uani 1 1 d . . . O3 O 0.7064(3) 0.7998(3) 1.0445(3) 0.0373(11) Uani 1 1 d . . . O4 O 0.8600(4) 0.9799(3) 0.8176(3) 0.0465(12) Uani 1 1 d . . . O5 O 0.6391(3) 1.2039(3) 0.6145(2) 0.0279(10) Uani 1 1 d . . . O6 O 0.3134(3) 1.2552(3) 0.6718(2) 0.0300(10) Uani 1 1 d . . . O7 O -0.1793(3) 0.1369(3) 0.0493(3) 0.0363(11) Uani 1 1 d . . . O8 O 0.0238(3) 0.2410(3) -0.1775(3) 0.0415(11) Uani 1 1 d . . . O9 O 0.3827(3) 0.1983(3) -0.1309(2) 0.0279(10) Uani 1 1 d . . . O10 O 0.5052(4) -0.0341(3) 0.0855(3) 0.0432(12) Uani 1 1 d . . . O11 O 0.2324(3) -0.1927(3) 0.3111(2) 0.0269(10) Uani 1 1 d . . . O12 O -0.0898(4) -0.1015(3) 0.3158(3) 0.0423(12) Uani 1 1 d . . . O1W O 0.3601(5) 0.7084(4) 0.8541(4) 0.088(2) Uani 1 1 d D . . O2W O 0.4736(4) 0.8941(4) 0.5920(3) 0.0546(14) Uani 1 1 d D . . O3W O 0.6337(4) 0.9572(3) 0.4657(3) 0.0472(12) Uani 1 1 d D . . O4W O 0.7051(4) 0.9094(4) 0.3209(3) 0.0487(12) Uani 1 1 d D . . O5W O 0.6498(4) 0.0123(4) 0.1558(4) 0.0797(19) Uani 1 1 d D . . O6W O 0.5223(5) 0.2173(5) 0.1353(4) 0.092(2) Uani 1 1 d D . . O7W O 0.5603(4) 0.3153(4) 0.2306(3) 0.0630(15) Uani 1 1 d D . . O8W O 0.6773(4) 0.4563(4) 0.2018(4) 0.0751(17) Uani 1 1 d D . . O9W O 0.7688(5) 0.4315(5) 0.9304(4) 0.0899(19) Uani 1 1 d D . . O10W O 0.1372(5) 0.2182(5) 0.3535(4) 0.083(2) Uani 1 1 d D . . O11W O 0.9026(4) 0.1870(4) 0.5681(3) 0.0630(15) Uani 1 1 d D . . O12W O 0.0013(4) 0.0998(3) 0.4420(3) 0.0467(12) Uani 1 1 d D . . O13W O 0.9658(4) 0.1364(4) 0.7247(3) 0.0531(13) Uani 1 1 d D . . O14W O 0.9090(4) 0.4432(4) 0.7813(4) 0.0817(18) Uani 1 1 d D . . O15W O 0.3171(5) 0.3281(5) 0.1483(4) 0.096(2) Uani 1 1 d D . . O16W O 0.8354(5) 0.4641(6) 0.0604(4) 0.106(2) Uani 1 1 d D . . O17W O 0.0118(7) 0.3375(8) 0.1012(6) 0.107(3) Uani 0.75 1 d P C 9 O18W O 0.1560(7) 0.2059(7) 0.1892(6) 0.103(3) Uani 0.75 1 d P D 9 O19W O 0.1274(14) 0.3384(14) 0.2006(11) 0.072(5) Uiso 0.30 1 d P E 8 O20W O 0.9060(15) 0.6393(15) 0.9303(15) 0.077(6) Uiso 0.30 1 d P F 7 O21W O 0.076(2) 0.803(2) 0.7429(18) 0.102(9) Uiso 0.25 1 d P G 1 O22W O 0.9154(13) 0.6271(13) 0.9880(13) 0.081(5) Uiso 0.35 1 d P H 2 O23W O 0.990(2) 0.620(2) 0.797(2) 0.087(9) Uiso 0.20 1 d P I 3 O24W O 0.009(2) 0.737(2) 0.798(2) 0.082(9) Uiso 0.20 1 d P J 4 O25W O 0.951(2) 0.694(2) 0.842(2) 0.082(9) Uiso 0.20 1 d P K 5 O26W O 0.014(2) 0.369(2) 0.150(2) 0.081(10) Uiso 0.20 1 d P L 6 S1 S 0.55925(18) 0.34532(15) 0.93481(13) 0.0564(6) Uani 1 1 d . . . S2 S 0.91391(15) 0.63556(15) 0.58976(15) 0.0524(5) Uani 1 1 d . . . S3 S 0.14927(14) 0.88174(14) 0.50077(13) 0.0395(5) Uani 1 1 d . . . S4 S 0.1333(5) 0.6876(6) -0.0117(5) 0.0578(14) Uani 0.75 1 d PU M 1 S4A S 0.1637(18) 0.691(2) -0.0072(17) 0.0578(14) Uani 0.25 1 d PU M 2 S5 S 0.49583(14) 0.18726(14) 0.43231(12) 0.0370(4) Uani 1 1 d . . . S6 S -0.27618(14) 0.42978(15) 0.39924(14) 0.0498(5) Uani 1 1 d . . . H1O H 0.4170(17) 0.725(4) 0.828(4) 0.075 Uiso 1 1 d D . . H2O H 0.309(2) 0.754(3) 0.834(4) 0.075 Uiso 1 1 d D . . H3O H 0.525(4) 0.916(6) 0.558(4) 0.075 Uiso 1 1 d D . . H4O H 0.491(6) 0.869(6) 0.643(2) 0.075 Uiso 1 1 d D . . H5O H 0.650(5) 0.942(4) 0.418(2) 0.075 Uiso 1 1 d D . . H6O H 0.597(5) 1.017(2) 0.458(3) 0.075 Uiso 1 1 d D . . H7O H 0.678(5) 0.939(5) 0.274(3) 0.075 Uiso 1 1 d D . . H8O H 0.767(2) 0.912(6) 0.321(5) 0.075 Uiso 1 1 d D . . H9O H 0.608(3) -0.016(3) 0.144(5) 0.075 Uiso 1 1 d D . . H10O H 0.623(4) 0.073(2) 0.155(5) 0.075 Uiso 1 1 d D . . H11O H 0.524(4) 0.246(5) 0.172(3) 0.075 Uiso 1 1 d D . . H12O H 0.581(2) 0.202(6) 0.108(4) 0.075 Uiso 1 1 d D . . H13O H 0.557(6) 0.289(5) 0.2858(7) 0.075 Uiso 1 1 d D . . H14O H 0.597(5) 0.359(4) 0.221(5) 0.075 Uiso 1 1 d D . . H15O H 0.7327(12) 0.422(2) 0.183(3) 0.075 Uiso 1 1 d D . . H16O H 0.680(4) 0.461(6) 0.251(2) 0.075 Uiso 1 1 d D . . H17O H 0.726(5) 0.430(6) 0.900(4) 0.075 Uiso 1 1 d D . . H18O H 0.779(6) 0.405(6) 0.9835(17) 0.075 Uiso 1 1 d D . . H19O H 0.170(6) 0.214(7) 0.304(3) 0.075 Uiso 1 1 d D . . H20O H 0.096(4) 0.178(5) 0.378(5) 0.075 Uiso 1 1 d D . . H21O H 0.897(4) 0.198(5) 0.616(2) 0.075 Uiso 1 1 d D . . H22O H 0.954(3) 0.207(5) 0.533(3) 0.075 Uiso 1 1 d D . . H23O H -0.022(6) 0.134(5) 0.477(4) 0.075 Uiso 1 1 d D . . H24O H 0.039(5) 0.041(2) 0.447(5) 0.075 Uiso 1 1 d D . . H25O H 0.929(5) 0.096(4) 0.761(4) 0.075 Uiso 1 1 d D . . H26O H 1.003(5) 0.152(6) 0.752(4) 0.075 Uiso 1 1 d D . . H27O H 0.947(3) 0.386(2) 0.780(5) 0.075 Uiso 1 1 d D . . H28O H 0.940(4) 0.479(4) 0.795(5) 0.075 Uiso 1 1 d D . . H29O H 0.358(5) 0.277(4) 0.136(5) 0.075 Uiso 1 1 d D . . H30O H 0.2527(13) 0.335(6) 0.165(5) 0.075 Uiso 1 1 d D . . H31O H 0.823(5) 0.468(5) 0.1120(17) 0.075 Uiso 1 1 d D . . H32O H 0.883(4) 0.413(4) 0.056(4) 0.075 Uiso 1 1 d D . . 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 0.018(4) 0.020(4) 0.027(4) -0.008(3) -0.005(3) 0.000(3) C2 0.036(5) 0.017(4) 0.024(4) -0.005(3) -0.004(3) -0.012(3) C3 0.023(4) 0.013(3) 0.019(4) 0.000(3) -0.002(3) -0.001(3) C4 0.028(4) 0.027(4) 0.032(4) -0.007(3) -0.001(3) -0.004(3) C5 0.027(4) 0.021(4) 0.033(5) -0.012(4) -0.004(4) -0.014(3) C6 0.033(4) 0.022(4) 0.023(4) 0.001(3) -0.010(3) 0.001(3) C7 0.033(4) 0.019(4) 0.036(5) -0.008(4) -0.005(4) -0.001(3) C8 0.031(4) 0.041(4) 0.035(4) 0.002(4) -0.003(4) -0.013(4) C9 0.032(4) 0.021(3) 0.025(4) 0.008(3) -0.008(3) -0.010(3) C10 0.058(5) 0.072(5) 0.041(5) 0.003(4) -0.022(4) -0.030(4) C11 0.027(4) 0.025(4) 0.041(5) -0.008(3) -0.003(4) 0.003(3) C12 0.030(4) 0.030(4) 0.025(4) -0.007(3) 0.005(3) -0.015(3) C13 0.025(4) 0.027(4) 0.023(3) -0.008(3) -0.003(3) -0.011(3) C14 0.030(5) 0.026(4) 0.022(4) -0.009(3) 0.002(3) -0.013(3) C15 0.034(5) 0.025(4) 0.024(4) -0.015(3) -0.001(3) -0.007(4) C16 0.030(4) 0.030(4) 0.040(4) -0.014(3) 0.010(3) -0.011(3) C17 0.038(5) 0.023(4) 0.018(4) -0.004(3) -0.010(3) -0.009(4) C18 0.024(4) 0.022(3) 0.025(4) -0.006(3) -0.005(3) 0.002(3) C19 0.036(4) 0.022(4) 0.030(4) 0.003(3) -0.010(3) -0.006(3) C20 0.036(4) 0.030(4) 0.025(4) 0.000(3) -0.004(3) -0.005(3) C21 0.046(4) 0.026(4) 0.032(4) -0.001(3) -0.014(3) -0.005(3) C22 0.037(4) 0.031(4) 0.026(4) -0.005(4) -0.007(3) -0.005(3) C23 0.039(4) 0.035(4) 0.030(4) -0.008(3) -0.011(3) -0.009(3) C24 0.024(4) 0.035(4) 0.029(4) -0.007(3) -0.004(3) -0.012(3) C25 0.023(4) 0.039(4) 0.039(4) -0.009(3) -0.003(3) -0.012(3) C26 0.027(4) 0.036(4) 0.057(5) -0.028(4) 0.000(3) -0.007(3) C27 0.026(4) 0.019(4) 0.024(4) 0.000(3) 0.001(3) -0.003(3) C28 0.030(4) 0.022(4) 0.043(4) -0.013(3) -0.001(3) -0.003(3) C29 0.031(4) 0.016(3) 0.032(4) -0.007(3) -0.009(3) -0.005(3) C30 0.025(4) 0.020(3) 0.028(4) -0.011(3) -0.006(3) 0.001(3) C31 0.028(4) 0.034(4) 0.026(3) -0.012(3) -0.008(3) -0.001(3) C32 0.028(4) 0.030(4) 0.014(3) 0.001(3) -0.003(3) -0.009(3) C33 0.025(4) 0.022(4) 0.030(4) -0.008(3) -0.007(3) -0.005(3) C34 0.040(5) 0.025(4) 0.022(4) -0.010(3) -0.006(3) -0.009(3) C35 0.023(4) 0.026(4) 0.043(5) -0.016(4) -0.012(4) -0.001(3) C36 0.024(4) 0.024(4) 0.033(4) -0.013(3) 0.000(3) -0.010(3) C37 0.039(5) 0.014(3) 0.027(4) -0.009(3) -0.002(4) -0.003(3) C38 0.028(4) 0.020(3) 0.016(4) -0.008(3) 0.006(3) -0.007(3) C39 0.025(4) 0.034(4) 0.027(4) -0.021(3) 0.001(3) -0.009(3) C40 0.038(5) 0.036(4) 0.049(4) -0.018(4) -0.007(4) -0.010(3) C41 0.045(5) 0.036(4) 0.054(5) -0.009(4) -0.018(4) -0.006(4) C42 0.031(4) 0.039(4) 0.028(4) -0.005(3) 0.000(3) -0.015(3) C43 0.064(5) 0.045(5) 0.030(4) -0.012(4) 0.000(4) -0.003(4) C44 0.027(4) 0.036(4) 0.033(4) -0.008(3) -0.003(3) -0.011(3) C45 0.043(5) 0.045(4) 0.035(4) -0.007(3) -0.001(3) -0.018(4) C46 0.033(4) 0.022(4) 0.024(4) -0.007(3) -0.002(4) -0.005(3) C47 0.032(5) 0.036(4) 0.021(4) -0.007(3) -0.002(3) -0.005(3) C48 0.026(4) 0.017(3) 0.023(4) -0.002(3) 0.002(3) -0.005(3) C49 0.044(5) 0.071(5) 0.039(4) -0.025(4) -0.002(4) -0.010(4) C50 0.029(4) 0.020(4) 0.036(5) -0.012(3) -0.008(4) 0.007(3) C51 0.027(4) 0.020(3) 0.027(4) -0.003(3) 0.001(3) -0.005(3) C52 0.028(4) 0.026(4) 0.036(4) -0.016(3) -0.005(3) -0.010(3) C53 0.023(4) 0.029(4) 0.039(4) -0.019(3) -0.005(4) -0.008(3) C54 0.031(5) 0.024(4) 0.036(4) -0.013(3) -0.009(4) -0.013(3) C55 0.046(5) 0.040(4) 0.041(4) -0.015(4) -0.008(4) -0.007(4) C56 0.059(6) 0.033(4) 0.035(5) -0.010(4) -0.012(5) -0.027(4) C57 0.065(6) 0.030(4) 0.047(5) 0.026(4) -0.042(4) -0.032(4) C58 0.048(5) 0.028(4) 0.020(4) -0.005(3) -0.014(3) -0.015(4) C59 0.039(5) 0.022(4) 0.025(4) -0.011(3) -0.003(3) -0.009(3) C60 0.038(5) 0.021(4) 0.017(3) -0.008(3) -0.001(3) -0.005(4) C61 0.045(5) 0.026(4) 0.029(4) -0.004(3) -0.006(3) -0.007(3) C62 0.051(5) 0.023(4) 0.022(4) -0.008(4) -0.009(4) -0.001(4) C63 0.033(4) 0.032(4) 0.021(4) -0.001(3) 0.001(3) -0.006(3) C64 0.038(4) 0.028(4) 0.032(4) -0.002(3) -0.002(3) -0.008(3) C65 0.047(5) 0.032(4) 0.040(4) -0.002(3) -0.011(4) -0.016(3) C66 0.055(5) 0.058(5) 0.030(4) -0.022(4) -0.006(3) -0.018(4) C67 0.049(5) 0.030(4) 0.027(4) -0.009(3) 0.004(3) -0.019(3) C68 0.073(5) 0.036(4) 0.024(4) -0.015(4) 0.000(4) -0.015(4) C69 0.052(8) 0.042(7) 0.063(7) -0.005(5) -0.032(7) -0.019(6) C70 0.040(6) 0.079(7) 0.011(5) -0.014(5) -0.012(5) 0.014(6) C71 0.149(9) 0.026(4) 0.022(5) -0.009(4) -0.015(5) 0.003(5) C69A 0.052(8) 0.042(7) 0.063(7) -0.005(5) -0.032(7) -0.019(6) C70A 0.040(6) 0.079(7) 0.011(5) -0.014(5) -0.012(5) 0.014(6) C71A 0.149(9) 0.026(4) 0.022(5) -0.009(4) -0.015(5) 0.003(5) C72 0.052(5) 0.022(4) 0.020(4) -0.007(3) -0.008(3) -0.015(4) C73 0.029(4) 0.022(4) 0.039(4) -0.013(3) -0.002(3) -0.004(3) C74 0.032(4) 0.024(4) 0.035(4) -0.004(3) 0.002(3) -0.004(3) C75 0.026(4) 0.023(3) 0.031(4) -0.006(3) 0.002(3) -0.007(3) C76 0.028(4) 0.038(4) 0.026(4) -0.009(3) -0.003(3) -0.013(3) C77 0.019(4) 0.030(4) 0.029(4) -0.011(3) -0.004(3) -0.003(3) C78 0.028(4) 0.024(4) 0.059(5) -0.013(4) 0.000(3) -0.007(3) C79 0.045(5) 0.014(3) 0.028(4) -0.005(3) -0.001(4) -0.007(3) C80 0.046(5) 0.020(4) 0.025(4) -0.009(3) 0.002(4) -0.016(3) C81 0.030(4) 0.025(4) 0.033(4) -0.011(3) -0.012(3) 0.002(3) C82 0.024(4) 0.022(4) 0.027(4) -0.006(3) -0.001(3) -0.006(3) C83 0.028(4) 0.020(3) 0.033(4) -0.011(3) 0.002(3) -0.005(3) C84 0.035(5) 0.019(4) 0.036(4) -0.011(3) -0.011(4) 0.000(3) C85 0.023(4) 0.044(4) 0.051(4) -0.024(4) 0.014(3) -0.013(3) C86 0.035(5) 0.048(5) 0.075(6) -0.018(4) -0.001(4) -0.019(4) C87 0.031(4) 0.031(4) 0.040(5) -0.002(4) 0.003(3) -0.006(3) C88 0.060(6) 0.056(5) 0.034(5) 0.003(4) 0.006(4) -0.004(4) C89 0.047(5) 0.038(4) 0.034(4) -0.010(3) -0.014(4) -0.002(4) C90 0.075(6) 0.043(5) 0.052(5) -0.008(4) -0.033(4) 0.013(4) N1 0.027(3) 0.025(3) 0.024(3) -0.006(3) 0.002(3) -0.007(3) N2 0.024(4) 0.023(3) 0.025(3) 0.001(2) -0.004(3) -0.004(3) N3 0.025(3) 0.030(3) 0.026(4) 0.000(3) -0.002(2) -0.009(3) N4 0.027(3) 0.029(3) 0.029(3) -0.009(3) -0.006(3) -0.011(2) N5 0.023(3) 0.032(3) 0.030(3) -0.007(3) -0.004(3) -0.003(3) N6 0.022(3) 0.024(3) 0.026(3) -0.003(3) -0.002(2) -0.005(2) N7 0.047(4) 0.024(3) 0.020(3) 0.001(3) -0.007(3) -0.001(3) N8 0.048(4) 0.027(3) 0.028(3) -0.007(3) -0.011(3) -0.002(3) N9 0.022(3) 0.025(3) 0.049(4) -0.010(3) -0.012(3) -0.001(2) N10 0.029(4) 0.029(3) 0.087(5) -0.023(3) -0.024(3) -0.001(3) N11 0.022(3) 0.034(3) 0.037(3) -0.022(3) -0.013(2) 0.000(2) N12 0.023(3) 0.029(3) 0.037(3) -0.014(3) -0.007(2) -0.005(3) N13 0.032(3) 0.026(3) 0.023(3) -0.005(2) 0.001(3) -0.007(3) N14 0.031(3) 0.027(3) 0.020(3) -0.002(2) -0.004(3) -0.008(3) N15 0.036(4) 0.025(3) 0.024(3) -0.005(3) -0.004(3) -0.010(3) N16 0.048(4) 0.030(3) 0.039(4) 0.010(3) -0.031(3) -0.011(3) N17 0.046(4) 0.026(3) 0.022(3) -0.009(3) -0.015(3) -0.002(3) N18 0.029(3) 0.026(3) 0.035(3) -0.003(3) -0.001(3) 0.001(3) N19 0.073(4) 0.033(3) 0.038(4) -0.020(3) -0.004(3) -0.005(3) N20 0.073(5) 0.027(3) 0.026(3) -0.007(3) -0.007(3) -0.001(3) N21 0.072(5) 0.029(3) 0.058(4) -0.006(3) -0.037(3) -0.014(3) N22 0.018(3) 0.033(3) 0.055(4) -0.007(3) -0.012(3) -0.009(3) N23 0.022(3) 0.036(3) 0.051(4) -0.018(3) -0.002(3) 0.002(3) N24 0.020(4) 0.033(3) 0.076(4) -0.026(3) -0.005(3) 0.002(3) O1 0.025(3) 0.026(2) 0.019(2) -0.006(2) -0.004(2) -0.0042(19) C1A 0.110(8) 0.070(6) 0.057(6) -0.025(5) 0.006(6) -0.015(6) N1A 0.125(8) 0.114(8) 0.080(6) -0.002(6) -0.055(6) -0.022(7) C2A 0.124(11) 0.073(7) 0.048(6) -0.015(5) -0.027(7) -0.019(7) O2 0.036(3) 0.028(2) 0.020(3) 0.001(2) -0.001(2) -0.011(2) O3 0.031(3) 0.045(3) 0.031(3) 0.000(2) -0.013(2) -0.011(2) O4 0.037(3) 0.051(3) 0.047(3) 0.005(2) -0.012(2) -0.027(3) O5 0.030(3) 0.025(3) 0.026(2) -0.004(2) 0.000(2) -0.011(2) O6 0.032(3) 0.019(2) 0.029(2) 0.000(2) -0.004(2) 0.002(2) O7 0.031(3) 0.043(3) 0.035(3) -0.010(2) -0.002(2) -0.011(2) O8 0.048(3) 0.047(3) 0.026(3) -0.004(2) -0.012(2) -0.007(2) O9 0.027(3) 0.027(2) 0.026(2) -0.006(2) 0.000(2) -0.003(2) O10 0.028(3) 0.038(3) 0.064(3) -0.012(2) -0.026(3) 0.004(2) O11 0.037(3) 0.017(2) 0.027(2) -0.002(2) -0.013(2) -0.007(2) O12 0.046(3) 0.032(3) 0.038(3) 0.000(2) 0.004(2) -0.011(3) O1W 0.094(5) 0.051(4) 0.107(5) -0.008(3) -0.041(4) 0.004(3) O2W 0.043(3) 0.068(4) 0.058(4) -0.017(3) -0.013(3) -0.019(3) O3W 0.050(3) 0.034(3) 0.048(3) -0.005(2) -0.021(3) 0.010(2) O4W 0.045(3) 0.042(3) 0.052(3) -0.008(3) -0.004(3) -0.010(3) O5W 0.087(5) 0.094(4) 0.067(4) 0.003(4) -0.025(3) -0.062(4) O6W 0.170(7) 0.065(4) 0.051(4) -0.009(3) -0.011(4) -0.057(5) O7W 0.071(4) 0.071(4) 0.044(3) -0.015(3) -0.018(3) -0.006(3) O8W 0.072(4) 0.068(4) 0.063(4) 0.003(3) -0.023(3) 0.003(3) O9W 0.086(5) 0.104(5) 0.088(5) -0.043(5) -0.002(4) -0.022(4) O10W 0.104(6) 0.096(5) 0.068(4) -0.003(4) -0.030(4) -0.068(4) O11W 0.074(4) 0.068(4) 0.049(3) -0.018(3) 0.015(3) -0.038(3) O12W 0.041(3) 0.043(3) 0.059(3) -0.019(3) -0.023(3) 0.003(2) O13W 0.061(4) 0.065(4) 0.039(3) -0.014(3) 0.006(3) -0.035(3) O14W 0.087(5) 0.064(4) 0.079(4) -0.019(4) -0.010(4) 0.004(3) O15W 0.091(5) 0.078(5) 0.089(5) -0.009(4) -0.015(5) 0.014(4) O16W 0.085(5) 0.117(6) 0.105(6) -0.050(5) -0.011(4) 0.020(4) O17W 0.099(7) 0.134(8) 0.089(7) -0.031(6) -0.022(5) -0.020(6) O18W 0.097(7) 0.111(7) 0.114(7) -0.058(6) -0.014(6) -0.009(6) S1 0.0933(17) 0.0313(10) 0.0375(11) -0.0091(9) -0.0211(11) 0.0074(11) S2 0.0353(12) 0.0336(10) 0.0759(14) 0.0033(10) -0.0195(10) -0.0038(9) S3 0.0309(11) 0.0392(10) 0.0573(12) -0.0236(9) -0.0186(9) -0.0002(8) S4 0.096(5) 0.0393(13) 0.0461(15) -0.0188(11) -0.045(3) 0.009(3) S4A 0.096(5) 0.0393(13) 0.0461(15) -0.0188(11) -0.045(3) 0.009(3) S5 0.0348(11) 0.0344(10) 0.0461(11) -0.0199(9) -0.0116(9) 0.0013(8) S6 0.0218(10) 0.0513(12) 0.0855(15) -0.0414(11) 0.0004(10) -0.0009(9) _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 N1 1.302(7) . ? C1 O1 1.372(7) . ? C1 C18 1.463(8) . ? C2 C3 1.357(8) . ? C2 O1 1.395(7) . ? C2 C4 1.484(8) . ? C3 N1 1.410(7) . ? C3 C5 1.469(8) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 O2 1.228(7) . ? C5 N2 1.344(7) . ? C6 N2 1.446(7) . ? C6 C7 1.517(9) . ? C6 C19 1.553(8) . ? C6 H6 1.0000 . ? C7 N3 1.288(7) . ? C7 O3 1.357(7) . ? C8 C9 1.349(9) . ? C8 O3 1.380(7) . ? C8 C10 1.480(9) . ? C9 N3 1.410(7) . ? C9 C11 1.449(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O4 1.240(7) . ? C11 N4 1.353(8) . ? C12 N4 1.464(7) . ? C12 C13 1.488(9) . ? C12 C24 1.537(8) . ? C12 H12 1.0000 . ? C13 N5 1.291(7) . ? C13 O5 1.354(7) . ? C14 C15 1.344(8) . ? C14 O5 1.390(7) . ? C14 C16 1.500(8) . ? C15 N5 1.425(8) . ? C15 C17 1.468(9) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O6 1.231(7) . ? C17 N6 1.347(7) . ? C18 N6 1.451(7) . ? C18 C29 1.535(8) . ? C18 H18 1.0000 . ? C19 C20 1.501(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.527(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 N7 1.470(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N7 1.331(8) . ? C22 N8 1.339(7) . ? C22 S1 1.697(7) . ? C23 N8 1.473(8) . ? C23 C34 1.536(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.499(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.539(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 N9 1.444(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 N10 1.325(8) . ? C27 N9 1.330(7) . ? C27 S2 1.686(6) . ? C28 N10 1.463(8) . ? C28 C36 1.512(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.515(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.491(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N11 1.460(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N11 1.328(7) . ? C32 N12 1.354(7) . ? C32 S3 1.690(6) . ? C33 N12 1.460(7) . ? C33 C38 1.495(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.404(8) . ? C34 C35 1.415(8) . ? C35 C36 1.409(8) . ? C35 C40 1.497(9) . ? C36 C37 1.400(8) . ? C37 C38 1.392(8) . ? C37 C42 1.522(8) . ? C38 C39 1.402(8) . ? C39 C44 1.527(8) . ? C40 C41 1.547(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.526(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.548(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 N13 1.280(7) . ? C46 O7 1.351(7) . ? C46 C63 1.517(8) . ? C47 C48 1.353(8) . ? C47 O7 1.367(7) . ? C47 C49 1.473(9) . ? C48 N13 1.419(7) . ? C48 C50 1.457(8) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 O8 1.245(7) . ? C50 N14 1.343(8) . ? C51 N14 1.474(7) . ? C51 C52 1.484(8) . ? C51 C64 1.507(8) . ? C51 H51 1.0000 . ? C52 N15 1.280(7) . ? C52 O9 1.360(7) . ? C53 C54 1.325(8) . ? C53 O9 1.399(7) . ? C53 C55 1.466(9) . ? C54 N15 1.400(7) . ? C54 C56 1.497(9) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 O10 1.197(8) . ? C56 N16 1.371(9) . ? C57 N16 1.461(7) . ? C57 C69 1.478(8) . ? C57 C58 1.485(9) . ? C57 C69A 1.576(10) . ? C57 H57 1.0000 . ? C58 N17 1.304(8) . ? C58 O11 1.348(7) . ? C59 C60 1.335(8) . ? C59 O11 1.393(7) . ? C59 C61 1.475(8) . ? C60 N17 1.416(8) . ? C60 C62 1.490(9) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 O12 1.222(7) . ? C62 N18 1.351(8) . ? C63 N18 1.465(8) . ? C63 C74 1.521(8) . ? C63 H63 1.0000 . ? C64 C65 1.462(9) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.562(9) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 N19 1.464(8) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 N19 1.341(8) . ? C67 N20 1.358(8) . ? C67 S4A 1.60(3) . ? C67 S4 1.692(10) . ? C68 N20 1.466(8) . ? C68 C79 1.530(8) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.496(8) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.622(9) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 N21 1.473(8) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C69A C70A 1.547(10) . ? C69A H69C 0.9900 . ? C69A H69D 0.9900 . ? C70A C71A 1.544(11) . ? C70A H70C 0.9900 . ? C70A H70D 0.9900 . ? C71A N21 1.525(11) . ? C71A H71C 0.9900 . ? C71A H71D 0.9900 . ? C72 N22 1.330(8) . ? C72 N21 1.335(8) . ? C72 S5 1.682(7) . ? C73 N22 1.457(8) . ? C73 C81 1.528(8) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.527(8) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.502(8) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 N23 1.475(8) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 N24 1.314(7) . ? C77 N23 1.349(8) . ? C77 S6 1.681(6) . ? C78 N24 1.479(8) . ? C78 C83 1.508(9) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C84 1.401(9) . ? C79 C80 1.410(9) . ? C80 C81 1.398(8) . ? C80 C85 1.494(9) . ? C81 C82 1.411(9) . ? C82 C83 1.403(8) . ? C82 C87 1.497(8) . ? C83 C84 1.397(9) . ? C84 C89 1.523(9) . ? C85 C86 1.556(9) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88 1.508(10) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 C90 1.535(9) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? N2 H2 0.8800 . ? N4 H4 0.8800 . ? N6 H6A 0.8800 . ? N7 H7 0.8800 . ? N8 H8 0.8800 . ? N9 H9 0.8800 . ? N10 H10 0.8800 . ? N11 H11 0.8800 . ? N12 H12A 0.8800 . ? N14 H14 0.8800 . ? N16 H16 0.8800 . ? N18 H18A 0.8800 . ? N19 H19 0.8800 . ? N20 H20 0.8800 . ? N21 H21 0.8800 . ? N22 H22 0.8800 . ? N23 H23 0.8800 . ? N24 H24 0.8800 . ? C1A C2A 1.442(14) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? N1A C2A 1.148(13) . ? O1W H1O 0.87(4) . ? O1W H2O 0.87(4) . ? O2W H3O 0.87(4) . ? O2W H4O 0.87(4) . ? O3W H5O 0.87(4) . ? O3W H6O 0.87(4) . ? O4W H7O 0.87(4) . ? O4W H8O 0.87(4) . ? O5W H9O 0.87(4) . ? O5W H10O 0.87(4) . ? O6W H11O 0.87(4) . ? O6W H12O 0.87(4) . ? O7W H13O 0.870(16) . ? O7W H14O 0.87(7) . ? O8W H15O 0.87(4) . ? O8W H16O 0.87(4) . ? O9W H17O 0.87(4) . ? O9W H18O 0.87(4) . ? O10W H19O 0.87(4) . ? O10W H20O 0.87(4) . ? O11W H21O 0.87(4) . ? O11W H22O 0.87(4) . ? O12W H23O 0.87(4) . ? O12W H24O 0.87(4) . ? O13W H25O 0.87(4) . ? O13W H26O 0.87(4) . ? O14W H27O 0.87(4) . ? O14W H28O 0.87(4) . ? O15W H29O 0.87(4) . ? O15W H30O 0.87(4) . ? O16W H31O 0.87(4) . ? O16W H32O 0.87(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 O1 113.0(5) . . ? N1 C1 C18 127.3(6) . . ? O1 C1 C18 119.6(5) . . ? C3 C2 O1 107.3(5) . . ? C3 C2 C4 135.2(5) . . ? O1 C2 C4 117.5(5) . . ? C2 C3 N1 108.9(5) . . ? C2 C3 C5 130.5(5) . . ? N1 C3 C5 120.5(5) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 N2 124.4(6) . . ? O2 C5 C3 123.6(6) . . ? N2 C5 C3 112.1(6) . . ? N2 C6 C7 106.2(5) . . ? N2 C6 C19 110.5(5) . . ? C7 C6 C19 109.7(5) . . ? N2 C6 H6 110.1 . . ? C7 C6 H6 110.1 . . ? C19 C6 H6 110.1 . . ? N3 C7 O3 114.5(5) . . ? N3 C7 C6 125.4(6) . . ? O3 C7 C6 120.1(6) . . ? C9 C8 O3 108.0(5) . . ? C9 C8 C10 135.6(6) . . ? O3 C8 C10 116.4(6) . . ? C8 C9 N3 108.5(5) . . ? C8 C9 C11 130.6(6) . . ? N3 C9 C11 120.7(6) . . ? 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 . . ? O4 C11 N4 123.9(6) . . ? O4 C11 C9 122.6(6) . . ? N4 C11 C9 113.5(6) . . ? N4 C12 C13 106.9(5) . . ? N4 C12 C24 111.7(5) . . ? C13 C12 C24 110.2(5) . . ? N4 C12 H12 109.3 . . ? C13 C12 H12 109.3 . . ? C24 C12 H12 109.3 . . ? N5 C13 O5 114.6(5) . . ? N5 C13 C12 125.2(5) . . ? O5 C13 C12 120.2(5) . . ? C15 C14 O5 107.8(5) . . ? C15 C14 C16 134.7(6) . . ? O5 C14 C16 117.5(5) . . ? C14 C15 N5 108.7(5) . . ? C14 C15 C17 131.4(6) . . ? N5 C15 C17 119.8(5) . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 N6 123.9(6) . . ? O6 C17 C15 122.9(5) . . ? N6 C17 C15 113.2(6) . . ? N6 C18 C1 107.6(5) . . ? N6 C18 C29 110.9(5) . . ? C1 C18 C29 111.1(5) . . ? N6 C18 H18 109.1 . . ? C1 C18 H18 109.1 . . ? C29 C18 H18 109.1 . . ? C20 C19 C6 112.0(5) . . ? C20 C19 H19A 109.2 . . ? C6 C19 H19A 109.2 . . ? C20 C19 H19B 109.2 . . ? C6 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C19 C20 C21 112.8(5) . . ? C19 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? N7 C21 C20 109.0(5) . . ? N7 C21 H21A 109.9 . . ? C20 C21 H21A 109.9 . . ? N7 C21 H21B 109.9 . . ? C20 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? N7 C22 N8 116.4(5) . . ? N7 C22 S1 122.5(5) . . ? N8 C22 S1 121.1(5) . . ? N8 C23 C34 110.1(5) . . ? N8 C23 H23A 109.6 . . ? C34 C23 H23A 109.6 . . ? N8 C23 H23B 109.6 . . ? C34 C23 H23B 109.6 . . ? H23A C23 H23B 108.2 . . ? C25 C24 C12 114.6(5) . . ? C25 C24 H24A 108.6 . . ? C12 C24 H24A 108.6 . . ? C25 C24 H24B 108.6 . . ? C12 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? C24 C25 C26 112.3(5) . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.9 . . ? N9 C26 C25 112.2(5) . . ? N9 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? N9 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? N10 C27 N9 114.5(5) . . ? N10 C27 S2 123.1(5) . . ? N9 C27 S2 122.4(5) . . ? N10 C28 C36 109.1(5) . . ? N10 C28 H28A 109.9 . . ? C36 C28 H28A 109.9 . . ? N10 C28 H28B 109.9 . . ? C36 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? C30 C29 C18 111.2(4) . . ? C30 C29 H29A 109.4 . . ? C18 C29 H29A 109.4 . . ? C30 C29 H29B 109.4 . . ? C18 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C31 C30 C29 113.8(5) . . ? C31 C30 H30A 108.8 . . ? C29 C30 H30A 108.8 . . ? C31 C30 H30B 108.8 . . ? C29 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? N11 C31 C30 109.7(5) . . ? N11 C31 H31A 109.7 . . ? C30 C31 H31A 109.7 . . ? N11 C31 H31B 109.7 . . ? C30 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? N11 C32 N12 115.0(5) . . ? N11 C32 S3 124.0(5) . . ? N12 C32 S3 120.9(5) . . ? N12 C33 C38 107.0(4) . . ? N12 C33 H33A 110.3 . . ? C38 C33 H33A 110.3 . . ? N12 C33 H33B 110.3 . . ? C38 C33 H33B 110.3 . . ? H33A C33 H33B 108.6 . . ? C39 C34 C35 121.6(5) . . ? C39 C34 C23 120.1(6) . . ? C35 C34 C23 118.2(5) . . ? C36 C35 C34 118.3(5) . . ? C36 C35 C40 120.7(6) . . ? C34 C35 C40 121.0(6) . . ? C37 C36 C35 119.8(5) . . ? C37 C36 C28 120.4(6) . . ? C35 C36 C28 119.6(5) . . ? C38 C37 C36 121.2(5) . . ? C38 C37 C42 119.5(5) . . ? C36 C37 C42 119.3(6) . . ? C37 C38 C39 120.1(5) . . ? C37 C38 C33 120.2(5) . . ? C39 C38 C33 119.2(5) . . ? C38 C39 C34 118.8(5) . . ? C38 C39 C44 119.6(5) . . ? C34 C39 C44 121.5(5) . . ? C35 C40 C41 112.6(5) . . ? C35 C40 H40A 109.1 . . ? C41 C40 H40A 109.1 . . ? C35 C40 H40B 109.1 . . ? C41 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 C43 114.5(5) . . ? C37 C42 H42A 108.6 . . ? C43 C42 H42A 108.6 . . ? C37 C42 H42B 108.6 . . ? C43 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 C45 112.0(5) . . ? C39 C44 H44A 109.2 . . ? C45 C44 H44A 109.2 . . ? C39 C44 H44B 109.2 . . ? C45 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N13 C46 O7 114.8(5) . . ? N13 C46 C63 127.2(6) . . ? O7 C46 C63 118.0(6) . . ? C48 C47 O7 107.1(5) . . ? C48 C47 C49 135.9(6) . . ? O7 C47 C49 117.0(6) . . ? C47 C48 N13 109.0(5) . . ? C47 C48 C50 130.8(6) . . ? N13 C48 C50 120.1(6) . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O8 C50 N14 123.9(6) . . ? O8 C50 C48 122.5(6) . . ? N14 C50 C48 113.6(6) . . ? N14 C51 C52 106.0(5) . . ? N14 C51 C64 111.9(5) . . ? C52 C51 C64 112.7(5) . . ? N14 C51 H51 108.7 . . ? C52 C51 H51 108.7 . . ? C64 C51 H51 108.7 . . ? N15 C52 O9 113.7(5) . . ? N15 C52 C51 127.8(6) . . ? O9 C52 C51 118.2(6) . . ? C54 C53 O9 106.6(5) . . ? C54 C53 C55 136.1(6) . . ? O9 C53 C55 117.3(6) . . ? C53 C54 N15 110.3(5) . . ? C53 C54 C56 127.1(6) . . ? N15 C54 C56 122.5(6) . . ? 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 . . ? O10 C56 N16 123.9(6) . . ? O10 C56 C54 125.9(7) . . ? N16 C56 C54 110.2(7) . . ? N16 C57 C69 115.6(6) . . ? N16 C57 C58 107.3(5) . . ? C69 C57 C58 123.4(7) . . ? N16 C57 C69A 109.5(15) . . ? C58 C57 C69A 96.9(10) . . ? N16 C57 H57 102.5 . . ? C69 C57 H57 102.5 . . ? C58 C57 H57 102.5 . . ? C69A C57 H57 135.4 . . ? N17 C58 O11 113.9(6) . . ? N17 C58 C57 126.4(6) . . ? O11 C58 C57 119.5(6) . . ? C60 C59 O11 106.8(5) . . ? C60 C59 C61 136.6(6) . . ? O11 C59 C61 116.6(5) . . ? C59 C60 N17 110.0(6) . . ? C59 C60 C62 130.8(6) . . ? N17 C60 C62 119.2(5) . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O12 C62 N18 125.5(6) . . ? O12 C62 C60 121.6(6) . . ? N18 C62 C60 112.9(6) . . ? N18 C63 C46 104.9(5) . . ? N18 C63 C74 111.3(5) . . ? C46 C63 C74 112.0(5) . . ? N18 C63 H63 109.5 . . ? C46 C63 H63 109.5 . . ? C74 C63 H63 109.5 . . ? C65 C64 C51 112.2(5) . . ? C65 C64 H64A 109.2 . . ? C51 C64 H64A 109.2 . . ? C65 C64 H64B 109.2 . . ? C51 C64 H64B 109.2 . . ? H64A C64 H64B 107.9 . . ? C64 C65 C66 113.7(5) . . ? C64 C65 H65A 108.8 . . ? C66 C65 H65A 108.8 . . ? C64 C65 H65B 108.8 . . ? C66 C65 H65B 108.8 . . ? H65A C65 H65B 107.7 . . ? N19 C66 C65 106.6(5) . . ? N19 C66 H66A 110.4 . . ? C65 C66 H66A 110.4 . . ? N19 C66 H66B 110.4 . . ? C65 C66 H66B 110.4 . . ? H66A C66 H66B 108.6 . . ? N19 C67 N20 112.6(6) . . ? N19 C67 S4A 128.0(11) . . ? N20 C67 S4A 116.2(9) . . ? N19 C67 S4 122.9(5) . . ? N20 C67 S4 124.5(5) . . ? N20 C68 C79 107.0(5) . . ? N20 C68 H68A 110.3 . . ? C79 C68 H68A 110.3 . . ? N20 C68 H68B 110.3 . . ? C79 C68 H68B 110.3 . . ? H68A C68 H68B 108.6 . . ? C57 C69 C70 103.5(7) . . ? C57 C69 H69A 111.1 . . ? C70 C69 H69A 111.1 . . ? C57 C69 H69B 111.1 . . ? C70 C69 H69B 111.1 . . ? H69A C69 H69B 109.0 . . ? C69 C70 C71 107.2(6) . . ? C69 C70 H70A 110.3 . . ? C71 C70 H70A 110.3 . . ? C69 C70 H70B 110.3 . . ? C71 C70 H70B 110.3 . . ? H70A C70 H70B 108.5 . . ? N21 C71 C70 100.4(7) . . ? N21 C71 H71A 111.7 . . ? C70 C71 H71A 111.7 . . ? N21 C71 H71B 111.7 . . ? C70 C71 H71B 111.7 . . ? H71A C71 H71B 109.5 . . ? C70A C69A C57 114.8(17) . . ? C70A C69A H69C 108.6 . . ? C57 C69A H69C 108.6 . . ? C70A C69A H69D 108.6 . . ? C57 C69A H69D 108.6 . . ? H69C C69A H69D 107.6 . . ? C71A C70A C69A 109.4(10) . . ? C71A C70A H70C 109.8 . . ? C69A C70A H70C 109.8 . . ? C71A C70A H70D 109.8 . . ? C69A C70A H70D 109.8 . . ? H70C C70A H70D 108.2 . . ? N21 C71A C70A 121(2) . . ? N21 C71A H71C 107.1 . . ? C70A C71A H71C 107.1 . . ? N21 C71A H71D 107.1 . . ? C70A C71A H71D 107.1 . . ? H71C C71A H71D 106.8 . . ? N22 C72 N21 113.0(6) . . ? N22 C72 S5 122.9(5) . . ? N21 C72 S5 124.1(5) . . ? N22 C73 C81 105.2(5) . . ? N22 C73 H73A 110.7 . . ? C81 C73 H73A 110.7 . . ? N22 C73 H73B 110.7 . . ? C81 C73 H73B 110.7 . . ? H73A C73 H73B 108.8 . . ? C63 C74 C75 112.7(5) . . ? C63 C74 H74A 109.0 . . ? C75 C74 H74A 109.0 . . ? C63 C74 H74B 109.0 . . ? C75 C74 H74B 109.0 . . ? H74A C74 H74B 107.8 . . ? C76 C75 C74 114.0(5) . . ? C76 C75 H75A 108.8 . . ? C74 C75 H75A 108.8 . . ? C76 C75 H75B 108.8 . . ? C74 C75 H75B 108.8 . . ? H75A C75 H75B 107.6 . . ? N23 C76 C75 109.8(5) . . ? N23 C76 H76A 109.7 . . ? C75 C76 H76A 109.7 . . ? N23 C76 H76B 109.7 . . ? C75 C76 H76B 109.7 . . ? H76A C76 H76B 108.2 . . ? N24 C77 N23 116.0(5) . . ? N24 C77 S6 121.4(5) . . ? N23 C77 S6 122.5(5) . . ? N24 C78 C83 107.8(5) . . ? N24 C78 H78A 110.2 . . ? C83 C78 H78A 110.2 . . ? N24 C78 H78B 110.2 . . ? C83 C78 H78B 110.2 . . ? H78A C78 H78B 108.5 . . ? C84 C79 C80 121.4(5) . . ? C84 C79 C68 120.7(6) . . ? C80 C79 C68 117.7(6) . . ? C81 C80 C79 118.0(6) . . ? C81 C80 C85 120.6(6) . . ? C79 C80 C85 121.4(6) . . ? C80 C81 C82 121.9(6) . . ? C80 C81 C73 118.8(6) . . ? C82 C81 C73 118.1(6) . . ? C83 C82 C81 118.3(5) . . ? C83 C82 C87 121.4(6) . . ? C81 C82 C87 120.2(6) . . ? C84 C83 C82 121.2(6) . . ? C84 C83 C78 119.4(6) . . ? C82 C83 C78 119.1(5) . . ? C83 C84 C79 119.0(6) . . ? C83 C84 C89 119.7(6) . . ? C79 C84 C89 121.3(6) . . ? C80 C85 C86 112.3(5) . . ? C80 C85 H85A 109.1 . . ? C86 C85 H85A 109.1 . . ? C80 C85 H85B 109.1 . . ? C86 C85 H85B 109.1 . . ? H85A C85 H85B 107.9 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C82 C87 C88 114.2(5) . . ? C82 C87 H87A 108.7 . . ? C88 C87 H87A 108.7 . . ? C82 C87 H87B 108.7 . . ? C88 C87 H87B 108.7 . . ? H87A C87 H87B 107.6 . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C84 C89 C90 112.6(5) . . ? C84 C89 H89A 109.1 . . ? C90 C89 H89A 109.1 . . ? C84 C89 H89B 109.1 . . ? C90 C89 H89B 109.1 . . ? H89A C89 H89B 107.8 . . ? C89 C90 H90A 109.5 . . ? C89 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C89 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C1 N1 C3 105.5(5) . . ? C5 N2 C6 125.4(5) . . ? C5 N2 H2 117.3 . . ? C6 N2 H2 117.3 . . ? C7 N3 C9 104.5(5) . . ? C11 N4 C12 124.8(5) . . ? C11 N4 H4 117.6 . . ? C12 N4 H4 117.6 . . ? C13 N5 C15 104.2(5) . . ? C17 N6 C18 125.3(5) . . ? C17 N6 H6A 117.4 . . ? C18 N6 H6A 117.4 . . ? C22 N7 C21 125.1(5) . . ? C22 N7 H7 117.5 . . ? C21 N7 H7 117.5 . . ? C22 N8 C23 125.8(5) . . ? C22 N8 H8 117.1 . . ? C23 N8 H8 117.1 . . ? C27 N9 C26 127.5(5) . . ? C27 N9 H9 116.3 . . ? C26 N9 H9 116.3 . . ? C27 N10 C28 127.5(5) . . ? C27 N10 H10 116.2 . . ? C28 N10 H10 116.2 . . ? C32 N11 C31 125.6(5) . . ? C32 N11 H11 117.2 . . ? C31 N11 H11 117.2 . . ? C32 N12 C33 127.1(5) . . ? C32 N12 H12A 116.4 . . ? C33 N12 H12A 116.4 . . ? C46 N13 C48 103.6(5) . . ? C50 N14 C51 125.3(5) . . ? C50 N14 H14 117.4 . . ? C51 N14 H14 117.4 . . ? C52 N15 C54 104.7(5) . . ? C56 N16 C57 123.7(6) . . ? C56 N16 H16 118.1 . . ? C57 N16 H16 118.1 . . ? C58 N17 C60 103.7(5) . . ? C62 N18 C63 124.3(5) . . ? C62 N18 H18A 117.8 . . ? C63 N18 H18A 117.8 . . ? C67 N19 C66 125.0(6) . . ? C67 N19 H19 117.5 . . ? C66 N19 H19 117.5 . . ? C67 N20 C68 126.1(6) . . ? C67 N20 H20 116.9 . . ? C68 N20 H20 116.9 . . ? C72 N21 C71 131.2(7) . . ? C72 N21 C71A 122.5(8) . . ? C72 N21 H21 114.4 . . ? C71 N21 H21 114.4 . . ? C71A N21 H21 123.0 . . ? C72 N22 C73 128.1(5) . . ? C72 N22 H22 116.0 . . ? C73 N22 H22 116.0 . . ? C77 N23 C76 124.2(5) . . ? C77 N23 H23 117.9 . . ? C76 N23 H23 117.9 . . ? C77 N24 C78 125.3(5) . . ? C77 N24 H24 117.3 . . ? C78 N24 H24 117.3 . . ? C1 O1 C2 105.3(4) . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? N1A C2A C1A 178.3(11) . . ? C7 O3 C8 104.4(5) . . ? C13 O5 C14 104.7(4) . . ? C46 O7 C47 105.4(5) . . ? C52 O9 C53 104.7(4) . . ? C58 O11 C59 105.5(5) . . ? H1O O1W H2O 112(5) . . ? H3O O2W H4O 106(8) . . ? H5O O3W H6O 111(5) . . ? H7O O4W H8O 120(8) . . ? H9O O5W H10O 112(5) . . ? H11O O6W H12O 112(5) . . ? H13O O7W H14O 102(8) . . ? H15O O8W H16O 112(5) . . ? H17O O9W H18O 136(8) . . ? H19O O10W H20O 115(8) . . ? H21O O11W H22O 112(5) . . ? H23O O12W H24O 132(8) . . ? H25O O13W H26O 109(7) . . ? H27O O14W H28O 112(5) . . ? H29O O15W H30O 128(9) . . ? H31O O16W H32O 112(5) . . ? 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 C2 C3 N1 -0.4(6) . . . . ? C4 C2 C3 N1 179.9(6) . . . . ? O1 C2 C3 C5 178.5(5) . . . . ? C4 C2 C3 C5 -1.2(11) . . . . ? C2 C3 C5 O2 -3.3(9) . . . . ? N1 C3 C5 O2 175.6(5) . . . . ? C2 C3 C5 N2 176.2(6) . . . . ? N1 C3 C5 N2 -4.9(7) . . . . ? N2 C6 C7 N3 -38.6(8) . . . . ? C19 C6 C7 N3 80.9(7) . . . . ? N2 C6 C7 O3 144.2(5) . . . . ? C19 C6 C7 O3 -96.3(6) . . . . ? O3 C8 C9 N3 0.5(7) . . . . ? C10 C8 C9 N3 -178.5(8) . . . . ? O3 C8 C9 C11 176.7(6) . . . . ? C10 C8 C9 C11 -2.2(13) . . . . ? C8 C9 C11 O4 3.4(11) . . . . ? N3 C9 C11 O4 179.3(6) . . . . ? C8 C9 C11 N4 -177.0(7) . . . . ? N3 C9 C11 N4 -1.1(8) . . . . ? N4 C12 C13 N5 -29.3(7) . . . . ? C24 C12 C13 N5 92.3(7) . . . . ? N4 C12 C13 O5 152.7(5) . . . . ? C24 C12 C13 O5 -85.6(6) . . . . ? O5 C14 C15 N5 0.0(6) . . . . ? C16 C14 C15 N5 178.5(6) . . . . ? O5 C14 C15 C17 -179.4(5) . . . . ? C16 C14 C15 C17 -0.9(11) . . . . ? C14 C15 C17 O6 -8.2(10) . . . . ? N5 C15 C17 O6 172.5(5) . . . . ? C14 C15 C17 N6 171.7(6) . . . . ? N5 C15 C17 N6 -7.7(7) . . . . ? N1 C1 C18 N6 -23.9(8) . . . . ? O1 C1 C18 N6 160.7(5) . . . . ? N1 C1 C18 C29 97.7(7) . . . . ? O1 C1 C18 C29 -77.7(6) . . . . ? N2 C6 C19 C20 -66.2(6) . . . . ? C7 C6 C19 C20 177.0(5) . . . . ? C6 C19 C20 C21 166.4(5) . . . . ? C19 C20 C21 N7 -70.4(7) . . . . ? N4 C12 C24 C25 -56.6(7) . . . . ? C13 C12 C24 C25 -175.3(5) . . . . ? C12 C24 C25 C26 -178.7(5) . . . . ? C24 C25 C26 N9 -56.1(7) . . . . ? N6 C18 C29 C30 -66.0(6) . . . . ? C1 C18 C29 C30 174.3(5) . . . . ? C18 C29 C30 C31 176.2(5) . . . . ? C29 C30 C31 N11 -66.0(7) . . . . ? N8 C23 C34 C39 -91.1(6) . . . . ? N8 C23 C34 C35 85.8(6) . . . . ? C39 C34 C35 C36 -4.8(8) . . . . ? C23 C34 C35 C36 178.3(5) . . . . ? C39 C34 C35 C40 176.9(5) . . . . ? C23 C34 C35 C40 0.1(8) . . . . ? C34 C35 C36 C37 2.5(8) . . . . ? C40 C35 C36 C37 -179.2(5) . . . . ? C34 C35 C36 C28 178.0(5) . . . . ? C40 C35 C36 C28 -3.7(8) . . . . ? N10 C28 C36 C37 76.3(7) . . . . ? N10 C28 C36 C35 -99.1(6) . . . . ? C35 C36 C37 C38 1.0(8) . . . . ? C28 C36 C37 C38 -174.5(5) . . . . ? C35 C36 C37 C42 179.7(5) . . . . ? C28 C36 C37 C42 4.2(8) . . . . ? C36 C37 C38 C39 -2.3(8) . . . . ? C42 C37 C38 C39 179.0(5) . . . . ? C36 C37 C38 C33 169.7(5) . . . . ? C42 C37 C38 C33 -9.0(8) . . . . ? N12 C33 C38 C37 -81.2(6) . . . . ? N12 C33 C38 C39 90.9(6) . . . . ? C37 C38 C39 C34 0.1(8) . . . . ? C33 C38 C39 C34 -172.0(5) . . . . ? C37 C38 C39 C44 177.2(5) . . . . ? C33 C38 C39 C44 5.1(7) . . . . ? C35 C34 C39 C38 3.5(8) . . . . ? C23 C34 C39 C38 -179.7(5) . . . . ? C35 C34 C39 C44 -173.5(5) . . . . ? C23 C34 C39 C44 3.3(8) . . . . ? C36 C35 C40 C41 -84.6(7) . . . . ? C34 C35 C40 C41 93.6(7) . . . . ? C38 C37 C42 C43 -82.5(7) . . . . ? C36 C37 C42 C43 98.8(7) . . . . ? C38 C39 C44 C45 81.6(7) . . . . ? C34 C39 C44 C45 -101.4(6) . . . . ? O7 C47 C48 N13 -0.3(7) . . . . ? C49 C47 C48 N13 179.2(7) . . . . ? O7 C47 C48 C50 -179.0(5) . . . . ? C49 C47 C48 C50 0.5(12) . . . . ? C47 C48 C50 O8 -5.2(10) . . . . ? N13 C48 C50 O8 176.2(5) . . . . ? C47 C48 C50 N14 175.6(6) . . . . ? N13 C48 C50 N14 -3.0(7) . . . . ? N14 C51 C52 N15 -13.1(8) . . . . ? C64 C51 C52 N15 109.6(7) . . . . ? N14 C51 C52 O9 173.3(4) . . . . ? C64 C51 C52 O9 -63.9(7) . . . . ? O9 C53 C54 N15 0.5(6) . . . . ? C55 C53 C54 N15 -177.7(6) . . . . ? O9 C53 C54 C56 178.1(5) . . . . ? C55 C53 C54 C56 0.0(11) . . . . ? C53 C54 C56 O10 -4.8(10) . . . . ? N15 C54 C56 O10 172.6(6) . . . . ? C53 C54 C56 N16 175.5(6) . . . . ? N15 C54 C56 N16 -7.1(7) . . . . ? N16 C57 C58 N17 -28.7(8) . . . . ? C69 C57 C58 N17 109.6(8) . . . . ? C69A C57 C58 N17 84.2(16) . . . . ? N16 C57 C58 O11 156.2(5) . . . . ? C69 C57 C58 O11 -65.5(9) . . . . ? C69A C57 C58 O11 -90.9(16) . . . . ? O11 C59 C60 N17 -2.0(6) . . . . ? C61 C59 C60 N17 178.2(6) . . . . ? O11 C59 C60 C62 176.3(5) . . . . ? C61 C59 C60 C62 -3.5(12) . . . . ? C59 C60 C62 O12 -1.1(10) . . . . ? N17 C60 C62 O12 177.1(5) . . . . ? C59 C60 C62 N18 178.8(6) . . . . ? N17 C60 C62 N18 -3.0(7) . . . . ? N13 C46 C63 N18 -35.5(8) . . . . ? O7 C46 C63 N18 144.7(5) . . . . ? N13 C46 C63 C74 85.3(7) . . . . ? O7 C46 C63 C74 -94.5(6) . . . . ? N14 C51 C64 C65 69.8(7) . . . . ? C52 C51 C64 C65 -49.6(7) . . . . ? C51 C64 C65 C66 -172.4(5) . . . . ? C64 C65 C66 N19 -176.9(6) . . . . ? N16 C57 C69 C70 67.1(10) . . . . ? C58 C57 C69 C70 -68.0(10) . . . . ? C69A C57 C69 C70 -21(2) . . . . ? C57 C69 C70 C71 -172.8(10) . . . . ? C69 C70 C71 N21 -173.2(10) . . . . ? N16 C57 C69A C70A -65(3) . . . . ? C69 C57 C69A C70A 42.0(18) . . . . ? C58 C57 C69A C70A -176(3) . . . . ? C57 C69A C70A C71A -174(3) . . . . ? C69A C70A C71A N21 -64(5) . . . . ? N18 C63 C74 C75 -66.1(7) . . . . ? C46 C63 C74 C75 176.9(5) . . . . ? C63 C74 C75 C76 172.6(5) . . . . ? C74 C75 C76 N23 -69.1(6) . . . . ? N20 C68 C79 C84 -94.0(7) . . . . ? N20 C68 C79 C80 80.9(7) . . . . ? C84 C79 C80 C81 -3.2(8) . . . . ? C68 C79 C80 C81 -178.1(5) . . . . ? C84 C79 C80 C85 173.8(5) . . . . ? C68 C79 C80 C85 -1.1(8) . . . . ? C79 C80 C81 C82 0.0(8) . . . . ? C85 C80 C81 C82 -177.0(5) . . . . ? C79 C80 C81 C73 167.3(5) . . . . ? C85 C80 C81 C73 -9.6(8) . . . . ? N22 C73 C81 C80 -91.6(6) . . . . ? N22 C73 C81 C82 76.3(6) . . . . ? C80 C81 C82 C83 1.7(8) . . . . ? C73 C81 C82 C83 -165.7(5) . . . . ? C80 C81 C82 C87 178.6(5) . . . . ? C73 C81 C82 C87 11.2(8) . . . . ? C81 C82 C83 C84 -0.3(8) . . . . ? C87 C82 C83 C84 -177.2(5) . . . . ? C81 C82 C83 C78 173.5(5) . . . . ? C87 C82 C83 C78 -3.4(8) . . . . ? N24 C78 C83 C84 89.9(6) . . . . ? N24 C78 C83 C82 -84.0(7) . . . . ? C82 C83 C84 C79 -2.7(8) . . . . ? C78 C83 C84 C79 -176.5(5) . . . . ? C82 C83 C84 C89 176.2(5) . . . . ? C78 C83 C84 C89 2.4(8) . . . . ? C80 C79 C84 C83 4.5(8) . . . . ? C68 C79 C84 C83 179.3(5) . . . . ? C80 C79 C84 C89 -174.4(5) . . . . ? C68 C79 C84 C89 0.4(8) . . . . ? C81 C80 C85 C86 -81.1(7) . . . . ? C79 C80 C85 C86 102.0(7) . . . . ? C83 C82 C87 C88 -98.0(7) . . . . ? C81 C82 C87 C88 85.2(7) . . . . ? C83 C84 C89 C90 88.6(7) . . . . ? C79 C84 C89 C90 -92.5(7) . . . . ? O1 C1 N1 C3 -1.4(6) . . . . ? C18 C1 N1 C3 -177.1(5) . . . . ? C2 C3 N1 C1 1.1(6) . . . . ? C5 C3 N1 C1 -177.9(5) . . . . ? O2 C5 N2 C6 -5.0(9) . . . . ? C3 C5 N2 C6 175.6(5) . . . . ? C7 C6 N2 C5 -140.1(5) . . . . ? C19 C6 N2 C5 100.9(6) . . . . ? O3 C7 N3 C9 -0.6(7) . . . . ? C6 C7 N3 C9 -178.0(5) . . . . ? C8 C9 N3 C7 0.1(7) . . . . ? C11 C9 N3 C7 -176.6(5) . . . . ? O4 C11 N4 C12 -11.1(9) . . . . ? C9 C11 N4 C12 169.3(5) . . . . ? C13 C12 N4 C11 -122.3(6) . . . . ? C24 C12 N4 C11 117.0(6) . . . . ? O5 C13 N5 C15 0.2(6) . . . . ? C12 C13 N5 C15 -177.9(5) . . . . ? C14 C15 N5 C13 -0.1(6) . . . . ? C17 C15 N5 C13 179.4(5) . . . . ? O6 C17 N6 C18 -2.5(9) . . . . ? C15 C17 N6 C18 177.6(5) . . . . ? C1 C18 N6 C17 -132.9(5) . . . . ? C29 C18 N6 C17 105.4(6) . . . . ? N8 C22 N7 C21 175.9(6) . . . . ? S1 C22 N7 C21 -6.4(9) . . . . ? C20 C21 N7 C22 172.0(6) . . . . ? N7 C22 N8 C23 178.6(5) . . . . ? S1 C22 N8 C23 0.8(9) . . . . ? C34 C23 N8 C22 -144.0(6) . . . . ? N10 C27 N9 C26 -176.3(6) . . . . ? S2 C27 N9 C26 6.2(9) . . . . ? C25 C26 N9 C27 -113.1(7) . . . . ? N9 C27 N10 C28 167.2(6) . . . . ? S2 C27 N10 C28 -15.4(9) . . . . ? C36 C28 N10 C27 141.3(6) . . . . ? N12 C32 N11 C31 -175.3(5) . . . . ? S3 C32 N11 C31 4.0(8) . . . . ? C30 C31 N11 C32 161.2(5) . . . . ? N11 C32 N12 C33 175.3(5) . . . . ? S3 C32 N12 C33 -4.1(8) . . . . ? C38 C33 N12 C32 -152.2(5) . . . . ? O7 C46 N13 C48 -1.3(6) . . . . ? C63 C46 N13 C48 178.9(6) . . . . ? C47 C48 N13 C46 0.9(6) . . . . ? C50 C48 N13 C46 179.8(5) . . . . ? O8 C50 N14 C51 -3.4(9) . . . . ? C48 C50 N14 C51 175.8(5) . . . . ? C52 C51 N14 C50 -131.8(5) . . . . ? C64 C51 N14 C50 105.0(6) . . . . ? O9 C52 N15 C54 -0.3(6) . . . . ? C51 C52 N15 C54 -174.1(5) . . . . ? C53 C54 N15 C52 -0.1(6) . . . . ? C56 C54 N15 C52 -177.9(5) . . . . ? O10 C56 N16 C57 -3.5(9) . . . . ? C54 C56 N16 C57 176.2(5) . . . . ? C69 C57 N16 C56 61.8(9) . . . . ? C58 C57 N16 C56 -156.3(6) . . . . ? C69A C57 N16 C56 99.7(13) . . . . ? O11 C58 N17 C60 -2.2(6) . . . . ? C57 C58 N17 C60 -177.6(6) . . . . ? C59 C60 N17 C58 2.6(6) . . . . ? C62 C60 N17 C58 -176.0(5) . . . . ? O12 C62 N18 C63 -11.1(9) . . . . ? C60 C62 N18 C63 169.0(5) . . . . ? C46 C63 N18 C62 -126.8(6) . . . . ? C74 C63 N18 C62 111.9(6) . . . . ? N20 C67 N19 C66 174.8(6) . . . . ? S4A C67 N19 C66 -26.5(14) . . . . ? S4 C67 N19 C66 -8.2(10) . . . . ? C65 C66 N19 C67 -154.6(6) . . . . ? N19 C67 N20 C68 -175.5(6) . . . . ? S4A C67 N20 C68 23.2(14) . . . . ? S4 C67 N20 C68 7.6(10) . . . . ? C79 C68 N20 C67 135.9(7) . . . . ? N22 C72 N21 C71 -179.8(12) . . . . ? S5 C72 N21 C71 -0.5(14) . . . . ? N22 C72 N21 C71A -177(3) . . . . ? S5 C72 N21 C71A 2(3) . . . . ? C70 C71 N21 C72 -171.4(7) . . . . ? C70 C71 N21 C71A 175(21) . . . . ? C70A C71A N21 C72 -148(2) . . . . ? C70A C71A N21 C71 20(16) . . . . ? N21 C72 N22 C73 -168.6(6) . . . . ? S5 C72 N22 C73 12.1(9) . . . . ? C81 C73 N22 C72 143.3(6) . . . . ? N24 C77 N23 C76 172.9(5) . . . . ? S6 C77 N23 C76 -7.5(8) . . . . ? C75 C76 N23 C77 168.6(5) . . . . ? N23 C77 N24 C78 -176.6(6) . . . . ? S6 C77 N24 C78 3.8(9) . . . . ? C83 C78 N24 C77 -162.6(6) . . . . ? N1 C1 O1 C2 1.2(6) . . . . ? C18 C1 O1 C2 177.2(5) . . . . ? C3 C2 O1 C1 -0.4(5) . . . . ? C4 C2 O1 C1 179.4(5) . . . . ? N3 C7 O3 C8 0.9(7) . . . . ? C6 C7 O3 C8 178.5(5) . . . . ? C9 C8 O3 C7 -0.8(7) . . . . ? C10 C8 O3 C7 178.4(6) . . . . ? N5 C13 O5 C14 -0.2(6) . . . . ? C12 C13 O5 C14 178.0(5) . . . . ? C15 C14 O5 C13 0.1(6) . . . . ? C16 C14 O5 C13 -178.7(5) . . . . ? N13 C46 O7 C47 1.1(7) . . . . ? C63 C46 O7 C47 -179.0(5) . . . . ? C48 C47 O7 C46 -0.4(6) . . . . ? C49 C47 O7 C46 179.9(6) . . . . ? N15 C52 O9 C53 0.6(6) . . . . ? C51 C52 O9 C53 175.1(5) . . . . ? C54 C53 O9 C52 -0.7(6) . . . . ? C55 C53 O9 C52 177.9(5) . . . . ? N17 C58 O11 C59 1.1(6) . . . . ? C57 C58 O11 C59 176.8(5) . . . . ? C60 C59 O11 C58 0.6(6) . . . . ? C61 C59 O11 C58 -179.5(5) . . . . ? 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 N2 H2 N1 0.88 2.24 2.693(7) 111.8 . N6 H6A N5 0.88 2.27 2.712(7) 111.3 . N7 H7 O1W 0.88 2.15 2.949(7) 151.5 . N8 H8 O1W 0.88 2.24 3.033(8) 150.7 . N9 H9 O3W 0.88 2.11 2.986(6) 171.7 . N10 H10 O3W 0.88 2.60 3.360(7) 145.7 . N11 H11 O2W 0.88 2.15 2.959(7) 152.2 . N12 H12A O2W 0.88 2.08 2.899(7) 155.5 . N14 H14 N13 0.88 2.26 2.706(7) 111.0 . N16 H16 N15 0.88 2.28 2.729(7) 111.4 . N19 H19 O15W 0.88 2.12 2.949(9) 156.7 . N20 H20 O15W 0.88 2.31 3.102(9) 150.0 . N21 H21 O10W 0.88 2.29 3.126(9) 159.5 . N22 H22 O10W 0.88 2.19 3.020(7) 156.5 . N23 H23 O12W 0.88 2.37 2.976(7) 126.5 . N24 H24 O10W 0.88 2.48 3.353(9) 174.0 . O1W H1O N1A 0.87(4) 2.29(5) 3.148(12) 170(6) . O2W H3O O3W 0.87(4) 1.97(6) 2.831(7) 169(8) . O2W H4O N1A 0.87(4) 2.06(5) 2.925(10) 171(8) . O3W H5O O4W 0.87(4) 1.82(4) 2.690(7) 171(7) . O3W H6O S5 0.87(4) 2.46(4) 3.328(5) 178(5) 1_565 O4W H7O O5W 0.87(4) 1.97(5) 2.824(7) 166(7) 1_565 O4W H8O O12 0.87(4) 1.93(4) 2.792(7) 170(8) 1_665 O5W H9O O10 0.87(4) 2.01(6) 2.848(7) 160(6) . O5W H10O O6W 0.87(4) 2.17(4) 3.002(9) 163(5) . O6W H11O O7W 0.87(4) 1.85(6) 2.688(8) 164(6) . O6W H12O O5W 0.87(4) 2.58(8) 3.002(9) 111(7) . O7W H13O S5 0.870(16) 2.49(3) 3.318(5) 158(7) . O7W H14O O8W 0.87(4) 1.92(7) 2.789(8) 180(9) . O8W H15O O16W 0.87(4) 2.24(4) 2.873(10) 130(4) . O8W H16O S6 0.87(4) 2.55(4) 3.390(6) 165(5) 1_655 O9W H17O S1 0.87(4) 2.76(6) 3.426(7) 134(7) . O9W H18O O16W 0.87(4) 2.14(7) 2.768(10) 129(7) 1_556 O10W H19O O18W 0.87(4) 2.03(5) 2.788(11) 145(8) . O10W H19O O19W 0.87(4) 2.09(8) 2.572(19) 114(7) . O10W H20O O12W 0.87(4) 1.87(7) 2.731(8) 172(8) . O11W H21O O13W 0.87(4) 2.04(5) 2.748(7) 137(6) . O12W H23O O11W 0.87(4) 1.95(7) 2.788(7) 165(8) 1_455 O12W H24O S3 0.87(4) 2.42(5) 3.259(5) 163(7) 1_545 O13W H25O O4 0.87(4) 2.00(7) 2.843(6) 161(7) 1_545 O13W H26O O8 0.87(4) 2.14(4) 2.933(7) 151(7) 1_656 O14W H27O O8 0.87(4) 2.05(3) 2.888(7) 160(7) 1_656 O14W H28O O23W 0.87(4) 2.34(4) 3.17(3) 160(6) . O15W H29O O6W 0.87(4) 2.22(6) 2.895(10) 134(7) . O15W H30O O19W 0.87(4) 1.71(2) 2.58(2) 175(9) . O15W H30O O18W 0.87(4) 2.46(7) 3.028(12) 123(7) . O16W H31O O8W 0.87(4) 2.26(6) 2.873(10) 128(6) . O16W H32O O17W 0.87(4) 1.99(4) 2.714(11) 140(6) 1_655 O16W H32O O26W 0.87(4) 2.46(7) 2.94(3) 115(5) 1_655 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 20.91 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.628 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.052