Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal SOciety of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_section_title ;Supramolecular chainlike aggregate and polymeric capsules constructed by p-sulfonatocalix[4, 6]arenes with (8-hydroxy)quinoline guests ; _publ_contact_author_name 'Prof. Yu Liu' _publ_contact_author_email YULIU@NANKAI.EDU.CN loop_ _publ_author_name 'Yu Liu' 'Kun Chen' 'Dong-Sheng Guo' 'Qiang Li' # Attachment 'complex_3.cif' data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 657145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H115 N6 O42.50 S6' _chemical_formula_sum 'C96 H115 N6 O42.50 S6' _chemical_formula_weight 2225.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0638(11) _cell_length_b 12.9848(11) _cell_length_c 19.8264(8) _cell_angle_alpha 73.838(15) _cell_angle_beta 73.607(11) _cell_angle_gamma 87.276(18) _cell_volume 2623.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6025 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1169 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9651 _exptl_absorpt_correction_T_max 0.9737 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21257 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _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 1.63 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10069 _reflns_number_gt 8298 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.1028P)^2^+6.0428P] 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 SHELXL _refine_ls_extinction_coef 0.025(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10069 _refine_ls_number_parameters 732 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.2366 _refine_ls_wR_factor_gt 0.2268 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.080 _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 S1 S 0.88005(9) 0.34486(8) 0.33999(5) 0.0329(3) Uani 1 1 d . . . S2 S 0.78161(10) 0.26629(9) 0.76156(6) 0.0374(3) Uani 1 1 d . . . S3 S 0.68732(13) -0.29882(12) 0.85493(7) 0.0545(4) Uani 1 1 d . . . O1 O 0.3533(2) 0.2636(2) 0.52375(14) 0.0295(6) Uani 1 1 d . . . H1 H 0.3096 0.3171 0.5130 0.044 Uiso 1 1 calc R . . O2 O 0.3615(2) 0.1718(2) 0.65560(15) 0.0322(6) Uani 1 1 d . . . H2 H 0.3650 0.2120 0.6137 0.048 Uiso 1 1 calc R . . O3 O 0.4355(3) -0.0341(2) 0.64251(14) 0.0336(6) Uani 1 1 d . . . H3 H 0.4057 0.0212 0.6541 0.050 Uiso 1 1 calc R . . O4 O 0.9019(3) 0.2771(3) 0.29076(15) 0.0436(7) Uani 1 1 d . . . O5 O 0.8939(3) 0.4585(3) 0.30250(18) 0.0512(9) Uani 1 1 d . . . O6 O 0.9576(2) 0.3141(2) 0.39153(15) 0.0347(6) Uani 1 1 d . . . O7 O 0.8936(3) 0.2342(3) 0.7129(2) 0.0519(8) Uani 1 1 d . . . O8 O 0.7863(3) 0.3805(3) 0.7532(2) 0.0541(9) Uani 1 1 d . . . O9 O 0.7567(4) 0.2025(4) 0.8363(2) 0.0814(14) Uani 1 1 d . . . O10 O 0.7244(8) -0.2265(5) 0.8896(4) 0.153(3) Uani 1 1 d . . . O11 O 0.6002(5) -0.3755(5) 0.9078(3) 0.113(2) Uani 1 1 d . . . O12 O 0.7923(5) -0.3396(5) 0.8116(2) 0.120(2) Uani 1 1 d . . . O13 O 0.2256(3) 0.4261(2) 0.49005(18) 0.0432(7) Uani 1 1 d . . . O14 O 0.1845(3) 0.4309(3) 0.3610(2) 0.0550(9) Uani 1 1 d . . . O15 O 0.9082(4) 0.9017(3) 0.2730(2) 0.0701(11) Uani 1 1 d . . . O16 O 0.9192(4) 0.6104(4) 0.3726(3) 0.0933(16) Uani 1 1 d . . . O17 O 0.4277(5) 0.6853(5) 0.0249(2) 0.0985(17) Uani 1 1 d . . . N1 N 0.0874(3) 0.1323(3) 0.37426(18) 0.0331(7) Uani 1 1 d . . . H1A H 0.0431 0.1902 0.3753 0.040 Uiso 1 1 calc R . . N2 N 0.4840(4) 0.3782(3) 0.8574(2) 0.0512(10) Uani 1 1 d . . . H2A H 0.5191 0.3546 0.8933 0.061 Uiso 1 1 calc R . . N3 N 1.0178(8) 0.4726(6) 0.1441(3) 0.100(3) Uani 1 1 d . . . H3B H 1.0288 0.4137 0.1766 0.120 Uiso 1 1 calc R . . C1 C 0.4760(3) 0.2850(3) 0.47999(19) 0.0248(7) Uani 1 1 d . . . C2 C 0.5118(3) 0.2515(3) 0.41602(19) 0.0258(7) Uani 1 1 d . . . C3 C 0.6369(3) 0.2702(3) 0.37276(19) 0.0272(8) Uani 1 1 d . . . H3A H 0.6638 0.2491 0.3288 0.033 Uiso 1 1 calc R . . C4 C 0.7217(3) 0.3202(3) 0.3948(2) 0.0273(8) Uani 1 1 d . . . C5 C 0.6852(3) 0.3536(3) 0.4585(2) 0.0273(8) Uani 1 1 d . . . H5 H 0.7449 0.3879 0.4722 0.033 Uiso 1 1 calc R . . C6 C 0.5603(3) 0.3362(3) 0.50229(19) 0.0262(7) Uani 1 1 d . . . C7 C 0.5164(4) 0.3718(3) 0.5721(2) 0.0292(8) Uani 1 1 d . . . H7A H 0.4254 0.3863 0.5814 0.035 Uiso 1 1 calc R . . H7B H 0.5616 0.4400 0.5644 0.035 Uiso 1 1 calc R . . C8 C 0.4596(3) 0.1979(3) 0.6779(2) 0.0278(8) Uani 1 1 d . . . C9 C 0.5373(3) 0.2907(3) 0.63986(19) 0.0267(8) Uani 1 1 d . . . C10 C 0.6345(4) 0.3100(3) 0.6669(2) 0.0300(8) Uani 1 1 d . . . H10 H 0.6888 0.3715 0.6416 0.036 Uiso 1 1 calc R . . C11 C 0.6538(4) 0.2407(3) 0.7306(2) 0.0304(8) Uani 1 1 d . . . C12 C 0.5759(4) 0.1504(3) 0.7678(2) 0.0301(8) Uani 1 1 d . . . H12 H 0.5886 0.1041 0.8115 0.036 Uiso 1 1 calc R . . C13 C 0.4790(3) 0.1268(3) 0.7415(2) 0.0288(8) Uani 1 1 d . . . C14 C 0.3994(4) 0.0232(3) 0.7813(2) 0.0308(8) Uani 1 1 d . . . H14A H 0.3771 0.0133 0.8347 0.037 Uiso 1 1 calc R . . H14B H 0.3203 0.0285 0.7668 0.037 Uiso 1 1 calc R . . C15 C 0.4872(3) -0.0945(3) 0.6950(2) 0.0275(8) Uani 1 1 d . . . C16 C 0.4713(3) -0.0733(3) 0.7629(2) 0.0280(8) Uani 1 1 d . . . C17 C 0.5314(4) -0.1377(3) 0.8113(2) 0.0312(8) Uani 1 1 d . . . H17 H 0.5218 -0.1244 0.8573 0.037 Uiso 1 1 calc R . . C18 C 0.6055(4) -0.2214(3) 0.7940(2) 0.0347(9) Uani 1 1 d . . . C19 C 0.6204(4) -0.2415(3) 0.7266(2) 0.0320(8) Uani 1 1 d . . . H19 H 0.6716 -0.2982 0.7146 0.038 Uiso 1 1 calc R . . C20 C 0.5611(3) -0.1795(3) 0.6771(2) 0.0288(8) Uani 1 1 d . . . C21 C 0.5879(3) -0.1961(3) 0.6013(2) 0.0292(8) Uani 1 1 d . . . H21A H 0.6070 -0.1247 0.5652 0.035 Uiso 1 1 calc R . . H21B H 0.6655 -0.2376 0.5931 0.035 Uiso 1 1 calc R . . C22 C 0.1126(4) 0.0991(4) 0.3143(2) 0.0385(9) Uani 1 1 d . . . H22 H 0.0839 0.1381 0.2739 0.046 Uiso 1 1 calc R . . C23 C 0.1813(4) 0.0069(4) 0.3107(2) 0.0399(10) Uani 1 1 d . . . H23 H 0.1986 -0.0177 0.2681 0.048 Uiso 1 1 calc R . . C24 C 0.2236(4) -0.0481(3) 0.3690(2) 0.0377(9) Uani 1 1 d . . . H24 H 0.2703 -0.1109 0.3668 0.045 Uiso 1 1 calc R . . C25 C 0.1983(4) -0.0119(3) 0.4322(2) 0.0342(9) Uani 1 1 d . . . C26 C 0.1262(3) 0.0816(3) 0.4341(2) 0.0298(8) Uani 1 1 d . . . C27 C 0.0964(4) 0.1219(3) 0.4960(2) 0.0344(9) Uani 1 1 d . . . H27 H 0.0481 0.1843 0.4968 0.041 Uiso 1 1 calc R . . C28 C 0.1384(4) 0.0691(4) 0.5551(2) 0.0415(10) Uani 1 1 d . . . H28 H 0.1187 0.0952 0.5971 0.050 Uiso 1 1 calc R . . C29 C 0.2107(4) -0.0239(4) 0.5542(2) 0.0415(10) Uani 1 1 d . . . H29 H 0.2390 -0.0593 0.5956 0.050 Uiso 1 1 calc R . . C30 C 0.2404(4) -0.0632(3) 0.4943(2) 0.0380(9) Uani 1 1 d . . . H30 H 0.2894 -0.1253 0.4944 0.046 Uiso 1 1 calc R . . C31 C 0.5275(5) 0.4688(4) 0.8071(3) 0.0571(13) Uani 1 1 d . . . H31 H 0.5960 0.5069 0.8103 0.069 Uiso 1 1 calc R . . C32 C 0.4751(5) 0.5094(4) 0.7495(3) 0.0563(13) Uani 1 1 d . . . H32 H 0.5077 0.5745 0.7134 0.068 Uiso 1 1 calc R . . C33 C 0.3769(5) 0.4553(4) 0.7453(3) 0.0511(12) Uani 1 1 d . . . H33 H 0.3403 0.4832 0.7062 0.061 Uiso 1 1 calc R . . C34 C 0.3282(5) 0.3575(4) 0.7985(3) 0.0462(11) Uani 1 1 d . . . C35 C 0.3862(5) 0.3201(4) 0.8554(2) 0.0469(12) Uani 1 1 d . . . C36 C 0.3426(5) 0.2235(4) 0.9110(3) 0.0557(13) Uani 1 1 d . . . H36 H 0.3814 0.1985 0.9494 0.067 Uiso 1 1 calc R . . C37 C 0.2449(6) 0.1674(4) 0.9084(3) 0.0604(15) Uani 1 1 d . . . H37 H 0.2152 0.1023 0.9453 0.072 Uiso 1 1 calc R . . C38 C 0.1857(5) 0.2044(4) 0.8513(3) 0.0605(14) Uani 1 1 d . . . H38 H 0.1167 0.1643 0.8505 0.073 Uiso 1 1 calc R . . C39 C 0.2277(5) 0.2976(4) 0.7974(3) 0.0535(13) Uani 1 1 d . . . H39 H 0.1884 0.3215 0.7592 0.064 Uiso 1 1 calc R . . C40 C 1.0920(7) 0.5526(8) 0.1292(4) 0.082(2) Uani 1 1 d . . . H40 H 1.1548 0.5462 0.1542 0.098 Uiso 1 1 calc R . . C41 C 1.0855(7) 0.6506(7) 0.0772(4) 0.093(3) Uani 1 1 d . . . H41 H 1.1410 0.7100 0.0670 0.112 Uiso 1 1 calc R . . C42 C 0.9911(6) 0.6547(6) 0.0411(3) 0.0699(19) Uani 1 1 d . . . H42 H 0.9836 0.7177 0.0043 0.084 Uiso 1 1 calc R . . C43 C 0.9103(5) 0.5682(5) 0.0590(3) 0.0548(14) Uani 1 1 d . . . C44 C 0.9230(6) 0.4715(6) 0.1137(3) 0.073(2) Uani 1 1 d . . . C45 C 0.8380(9) 0.3819(6) 0.1330(4) 0.092(3) Uani 1 1 d . . . H45 H 0.8448 0.3182 0.1694 0.110 Uiso 1 1 calc R . . C46 C 0.7493(9) 0.3901(7) 0.0987(4) 0.097(3) Uani 1 1 d . . . H46 H 0.6929 0.3305 0.1109 0.117 Uiso 1 1 calc R . . C47 C 0.7355(7) 0.4812(6) 0.0462(4) 0.079(2) Uani 1 1 d . . . H47 H 0.6696 0.4829 0.0239 0.095 Uiso 1 1 calc R . . C48 C 0.8142(6) 0.5690(6) 0.0255(3) 0.0643(17) Uani 1 1 d . . . H48 H 0.8040 0.6306 -0.0116 0.077 Uiso 1 1 calc R . . O18 O 0.1310(8) 0.8902(6) 0.7771(5) 0.0618(19) Uani 0.50 1 d PU . . O19 O 0.6963(14) 0.9872(11) 0.9215(6) 0.118(4) Uani 0.50 1 d PU . . O20 O 0.3184(17) 0.8697(13) 0.9861(9) 0.156(5) Uani 0.50 1 d PU . . O21 O -0.0924(16) 0.8652(12) 0.9016(8) 0.137(4) Uani 0.50 1 d PU . . O22 O 0.4444(18) 0.9357(14) 0.9753(8) 0.159(5) Uani 0.50 1 d PU . . O23 O 0.0000 1.0000 1.0000 0.186(7) Uani 0.50 2 d SPU . . O24 O 0.067(2) 0.9216(17) 0.9670(12) 0.189(6) Uani 0.50 1 d PU . . O25 O 0.1482(19) 0.8797(15) 0.9277(11) 0.182(6) Uani 0.50 1 d PU . . O26 O 0.016(2) 0.8849(18) 0.8455(13) 0.101(5) Uani 0.25 1 d PU . . O27 O 0.786(3) 1.033(2) 0.9334(13) 0.114(6) Uani 0.25 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0246(5) 0.0363(5) 0.0328(5) -0.0029(4) -0.0070(4) 0.0023(4) S2 0.0357(6) 0.0429(6) 0.0373(5) -0.0107(4) -0.0156(4) -0.0030(4) S3 0.0607(8) 0.0686(9) 0.0414(6) -0.0158(6) -0.0296(6) 0.0304(7) O1 0.0222(13) 0.0322(14) 0.0333(13) -0.0100(11) -0.0064(10) 0.0043(10) O2 0.0301(14) 0.0319(14) 0.0349(14) -0.0056(11) -0.0130(11) -0.0002(11) O3 0.0428(16) 0.0281(14) 0.0340(14) -0.0078(11) -0.0192(12) 0.0069(12) O4 0.0297(15) 0.068(2) 0.0342(15) -0.0186(14) -0.0074(12) 0.0064(14) O5 0.0359(17) 0.0403(17) 0.059(2) 0.0125(15) -0.0090(14) -0.0038(13) O6 0.0277(14) 0.0380(15) 0.0386(15) -0.0095(12) -0.0112(12) 0.0029(11) O7 0.0351(17) 0.052(2) 0.077(2) -0.0251(17) -0.0229(16) 0.0073(14) O8 0.0493(19) 0.056(2) 0.074(2) -0.0352(18) -0.0274(17) 0.0020(16) O9 0.076(3) 0.119(4) 0.044(2) 0.011(2) -0.035(2) -0.044(3) O10 0.231(8) 0.141(5) 0.199(7) -0.101(5) -0.199(7) 0.098(5) O11 0.111(4) 0.128(5) 0.071(3) 0.038(3) -0.043(3) 0.004(3) O12 0.096(4) 0.184(6) 0.055(2) -0.008(3) -0.023(2) 0.106(4) O13 0.0332(16) 0.0365(16) 0.0592(19) -0.0111(14) -0.0146(14) 0.0058(12) O14 0.050(2) 0.0462(19) 0.086(3) -0.0237(18) -0.0401(19) 0.0060(15) O15 0.058(2) 0.077(3) 0.084(3) -0.032(2) -0.029(2) 0.022(2) O16 0.075(3) 0.075(3) 0.105(4) -0.041(3) 0.033(3) -0.020(2) O17 0.072(3) 0.160(5) 0.062(3) -0.025(3) -0.026(2) 0.020(3) N1 0.0276(16) 0.0335(17) 0.0396(18) -0.0111(14) -0.0106(14) 0.0009(13) N2 0.051(2) 0.052(2) 0.050(2) -0.0148(19) -0.0127(19) 0.0151(19) N3 0.145(6) 0.126(6) 0.070(4) -0.064(4) -0.072(4) 0.090(5) C1 0.0214(17) 0.0220(17) 0.0291(17) -0.0045(14) -0.0070(14) 0.0019(13) C2 0.0259(18) 0.0226(17) 0.0290(17) -0.0054(14) -0.0098(14) 0.0013(14) C3 0.0289(19) 0.0255(18) 0.0267(17) -0.0064(14) -0.0089(14) 0.0058(14) C4 0.0248(18) 0.0234(17) 0.0311(18) -0.0024(14) -0.0089(14) 0.0024(14) C5 0.0270(18) 0.0224(17) 0.0326(18) -0.0039(14) -0.0115(15) -0.0019(14) C6 0.0276(18) 0.0215(17) 0.0295(18) -0.0058(14) -0.0095(15) 0.0039(14) C7 0.0316(19) 0.0234(18) 0.0355(19) -0.0109(15) -0.0114(16) 0.0034(14) C8 0.0260(18) 0.0272(18) 0.0327(18) -0.0127(15) -0.0081(15) 0.0037(14) C9 0.0284(18) 0.0238(17) 0.0290(17) -0.0106(14) -0.0073(14) 0.0044(14) C10 0.032(2) 0.0269(18) 0.0327(19) -0.0114(15) -0.0079(15) 0.0008(15) C11 0.032(2) 0.033(2) 0.0312(18) -0.0161(16) -0.0092(15) 0.0032(15) C12 0.032(2) 0.0307(19) 0.0277(18) -0.0109(15) -0.0066(15) 0.0051(15) C13 0.0281(19) 0.0270(18) 0.0309(18) -0.0105(15) -0.0057(15) 0.0035(15) C14 0.0304(19) 0.0287(19) 0.0314(19) -0.0087(15) -0.0054(15) 0.0023(15) C15 0.0264(18) 0.0274(18) 0.0299(18) -0.0065(15) -0.0109(15) 0.0003(14) C16 0.0274(18) 0.0267(18) 0.0304(18) -0.0084(15) -0.0080(15) -0.0012(14) C17 0.033(2) 0.035(2) 0.0266(18) -0.0085(15) -0.0088(15) 0.0001(16) C18 0.034(2) 0.037(2) 0.034(2) -0.0064(17) -0.0151(17) 0.0050(17) C19 0.0301(19) 0.031(2) 0.036(2) -0.0098(16) -0.0114(16) 0.0045(15) C20 0.0279(19) 0.0299(19) 0.0296(18) -0.0088(15) -0.0085(15) -0.0021(15) C21 0.0270(18) 0.0306(19) 0.0312(18) -0.0093(15) -0.0086(15) -0.0021(15) C22 0.033(2) 0.044(2) 0.040(2) -0.0121(18) -0.0106(17) 0.0002(18) C23 0.034(2) 0.042(2) 0.046(2) -0.0179(19) -0.0099(18) -0.0004(18) C24 0.0260(19) 0.035(2) 0.047(2) -0.0122(18) -0.0003(17) -0.0021(16) C25 0.0260(19) 0.031(2) 0.041(2) -0.0055(16) -0.0063(16) -0.0022(15) C26 0.0191(17) 0.0279(19) 0.043(2) -0.0091(16) -0.0098(15) -0.0021(14) C27 0.0252(19) 0.037(2) 0.040(2) -0.0090(17) -0.0075(16) -0.0060(16) C28 0.035(2) 0.049(3) 0.038(2) -0.0099(19) -0.0083(18) -0.0091(19) C29 0.032(2) 0.042(2) 0.045(2) 0.0026(19) -0.0157(18) -0.0058(18) C30 0.026(2) 0.032(2) 0.050(2) -0.0022(18) -0.0113(18) -0.0016(16) C31 0.056(3) 0.045(3) 0.067(3) -0.016(2) -0.014(3) 0.014(2) C32 0.057(3) 0.038(3) 0.069(3) -0.009(2) -0.017(3) 0.012(2) C33 0.058(3) 0.040(3) 0.051(3) -0.011(2) -0.015(2) 0.024(2) C34 0.048(3) 0.041(2) 0.048(2) -0.019(2) -0.007(2) 0.018(2) C35 0.050(3) 0.048(3) 0.038(2) -0.016(2) -0.004(2) 0.022(2) C36 0.058(3) 0.055(3) 0.048(3) -0.017(2) -0.006(2) 0.019(3) C37 0.068(4) 0.051(3) 0.049(3) -0.014(2) 0.003(3) 0.015(3) C38 0.056(3) 0.055(3) 0.066(3) -0.029(3) 0.001(3) 0.007(2) C39 0.054(3) 0.054(3) 0.052(3) -0.023(2) -0.008(2) 0.019(2) C40 0.085(5) 0.127(6) 0.074(4) -0.065(5) -0.060(4) 0.072(5) C41 0.070(4) 0.142(7) 0.103(5) -0.085(5) -0.037(4) 0.051(4) C42 0.068(4) 0.101(5) 0.054(3) -0.040(3) -0.027(3) 0.052(4) C43 0.061(3) 0.076(4) 0.039(2) -0.032(2) -0.023(2) 0.039(3) C44 0.096(5) 0.110(5) 0.033(2) -0.042(3) -0.039(3) 0.069(4) C45 0.157(8) 0.062(4) 0.054(4) -0.019(3) -0.027(4) 0.029(5) C46 0.135(7) 0.101(6) 0.066(4) -0.039(4) -0.033(5) 0.028(5) C47 0.096(5) 0.089(5) 0.064(4) -0.041(4) -0.029(4) 0.042(4) C48 0.081(4) 0.085(4) 0.042(3) -0.036(3) -0.032(3) 0.056(4) O18 0.071(4) 0.043(4) 0.086(5) -0.014(3) -0.048(4) -0.001(3) O19 0.142(8) 0.121(7) 0.072(5) 0.009(5) -0.033(5) 0.013(6) O20 0.160(9) 0.146(8) 0.160(8) -0.056(7) -0.031(7) 0.031(7) O21 0.164(8) 0.133(7) 0.119(7) -0.050(6) -0.030(6) -0.019(7) O22 0.187(9) 0.160(8) 0.121(7) -0.028(6) -0.048(7) 0.062(7) O23 0.176(10) 0.177(10) 0.193(9) -0.050(7) -0.034(7) -0.002(8) O24 0.184(9) 0.173(8) 0.196(9) -0.045(7) -0.035(7) -0.001(7) O25 0.176(9) 0.154(9) 0.180(9) -0.040(7) -0.003(7) 0.018(7) O26 0.104(8) 0.091(8) 0.108(8) -0.018(7) -0.038(7) 0.000(7) O27 0.120(10) 0.111(9) 0.090(9) -0.003(7) -0.022(8) 0.030(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 S1 O5 1.449(3) . ? S1 O4 1.452(3) . ? S1 O6 1.475(3) . ? S1 C4 1.771(4) . ? S2 O9 1.437(4) . ? S2 O8 1.447(4) . ? S2 O7 1.462(3) . ? S2 C11 1.771(4) . ? S3 O11 1.399(5) . ? S3 O12 1.414(4) . ? S3 O10 1.441(5) . ? S3 C18 1.773(4) . ? O1 C1 1.382(4) . ? O1 H1 0.8400 . ? O2 C8 1.370(5) . ? O2 H2 0.8400 . ? O3 C15 1.365(4) . ? O3 H3 0.8400 . ? N1 C22 1.327(5) . ? N1 C26 1.361(5) . ? N1 H1A 0.8800 . ? N2 C31 1.319(7) . ? N2 C35 1.364(7) . ? N2 H2A 0.8800 . ? N3 C40 1.270(10) . ? N3 C44 1.352(9) . ? N3 H3B 0.8800 . ? C1 C2 1.401(5) . ? C1 C6 1.401(5) . ? C2 C3 1.399(5) . ? C2 C21 1.510(5) 2_656 ? C3 C4 1.392(5) . ? C3 H3A 0.9500 . ? C4 C5 1.396(5) . ? C5 C6 1.399(5) . ? C5 H5 0.9500 . ? C6 C7 1.523(5) . ? C7 C9 1.527(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.405(5) . ? C8 C9 1.409(5) . ? C9 C10 1.390(5) . ? C10 C11 1.396(5) . ? C10 H10 0.9500 . ? C11 C12 1.385(6) . ? C12 C13 1.397(6) . ? C12 H12 0.9500 . ? C13 C14 1.529(5) . ? C14 C16 1.527(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.408(5) . ? C15 C16 1.410(5) . ? C16 C17 1.387(5) . ? C17 C18 1.391(5) . ? C17 H17 0.9500 . ? C18 C19 1.395(6) . ? C19 C20 1.384(5) . ? C19 H19 0.9500 . ? C20 C21 1.521(5) . ? C21 C2 1.510(5) 2_656 ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.395(6) . ? C22 H22 0.9500 . ? C23 C24 1.371(6) . ? C23 H23 0.9500 . ? C24 C25 1.409(6) . ? C24 H24 0.9500 . ? C25 C30 1.418(6) . ? C25 C26 1.425(5) . ? C26 C27 1.415(6) . ? C27 C28 1.374(6) . ? C27 H27 0.9500 . ? C28 C29 1.418(6) . ? C28 H28 0.9500 . ? C29 C30 1.373(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.388(8) . ? C31 H31 0.9500 . ? C32 C33 1.355(8) . ? C32 H32 0.9500 . ? C33 C34 1.420(7) . ? C33 H33 0.9500 . ? C34 C39 1.395(8) . ? C34 C35 1.413(7) . ? C35 C36 1.418(7) . ? C36 C37 1.353(8) . ? C36 H36 0.9500 . ? C37 C38 1.424(8) . ? C37 H37 0.9500 . ? C38 C39 1.369(8) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.411(11) . ? C40 H40 0.9500 . ? C41 C42 1.414(9) . ? C41 H41 0.9500 . ? C42 C43 1.372(9) . ? C42 H42 0.9500 . ? C43 C48 1.402(8) . ? C43 C44 1.442(8) . ? C44 C45 1.427(11) . ? C45 C46 1.329(11) . ? C45 H45 0.9500 . ? C46 C47 1.375(10) . ? C46 H46 0.9500 . ? C47 C48 1.364(10) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? O18 O26 1.56(3) . ? O19 O27 1.29(3) . ? O20 O22 1.60(2) . ? O21 O26 1.36(3) . ? O23 O24 1.43(2) 2_577 ? O23 O24 1.43(2) . ? O24 O25 1.22(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 S1 O4 113.4(2) . . ? O5 S1 O6 111.81(19) . . ? O4 S1 O6 111.57(17) . . ? O5 S1 C4 106.90(18) . . ? O4 S1 C4 107.09(18) . . ? O6 S1 C4 105.51(17) . . ? O9 S2 O8 113.4(3) . . ? O9 S2 O7 113.1(3) . . ? O8 S2 O7 111.0(2) . . ? O9 S2 C11 106.6(2) . . ? O8 S2 C11 106.90(19) . . ? O7 S2 C11 105.30(18) . . ? O11 S3 O12 115.8(4) . . ? O11 S3 O10 108.9(5) . . ? O12 S3 O10 112.2(5) . . ? O11 S3 C18 106.6(3) . . ? O12 S3 C18 106.4(2) . . ? O10 S3 C18 106.3(3) . . ? C1 O1 H1 109.5 . . ? C8 O2 H2 109.5 . . ? C15 O3 H3 109.5 . . ? C22 N1 C26 123.6(3) . . ? C22 N1 H1A 118.2 . . ? C26 N1 H1A 118.2 . . ? C31 N2 C35 121.9(5) . . ? C31 N2 H2A 119.1 . . ? C35 N2 H2A 119.1 . . ? C40 N3 C44 124.5(7) . . ? C40 N3 H3B 117.7 . . ? C44 N3 H3B 117.7 . . ? O1 C1 C2 118.3(3) . . ? O1 C1 C6 118.9(3) . . ? C2 C1 C6 122.7(3) . . ? C3 C2 C1 118.4(3) . . ? C3 C2 C21 124.2(3) . 2_656 ? C1 C2 C21 117.4(3) . 2_656 ? C4 C3 C2 119.3(3) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 121.9(3) . . ? C3 C4 S1 119.5(3) . . ? C5 C4 S1 118.5(3) . . ? C4 C5 C6 119.6(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C1 118.0(3) . . ? C5 C6 C7 121.3(3) . . ? C1 C6 C7 120.7(3) . . ? C6 C7 C9 114.5(3) . . ? C6 C7 H7A 108.6 . . ? C9 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C9 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? O2 C8 C13 116.3(3) . . ? O2 C8 C9 122.5(3) . . ? C13 C8 C9 121.3(3) . . ? C10 C9 C8 118.0(3) . . ? C10 C9 C7 119.1(3) . . ? C8 C9 C7 122.8(3) . . ? C9 C10 C11 121.2(4) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C12 C11 C10 120.1(4) . . ? C12 C11 S2 120.2(3) . . ? C10 C11 S2 119.7(3) . . ? C11 C12 C13 120.5(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 118.9(3) . . ? C12 C13 C14 119.3(3) . . ? C8 C13 C14 121.8(3) . . ? C16 C14 C13 110.8(3) . . ? C16 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C16 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O3 C15 C20 116.0(3) . . ? O3 C15 C16 123.1(3) . . ? C20 C15 C16 120.9(3) . . ? C17 C16 C15 118.2(3) . . ? C17 C16 C14 119.9(3) . . ? C15 C16 C14 121.7(3) . . ? C16 C17 C18 121.4(4) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C19 119.8(4) . . ? C17 C18 S3 120.6(3) . . ? C19 C18 S3 119.6(3) . . ? C20 C19 C18 120.6(4) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C15 119.2(3) . . ? C19 C20 C21 119.7(3) . . ? C15 C20 C21 120.8(3) . . ? C2 C21 C20 118.8(3) 2_656 . ? C2 C21 H21A 107.6 2_656 . ? C20 C21 H21A 107.6 . . ? C2 C21 H21B 107.6 2_656 . ? C20 C21 H21B 107.6 . . ? H21A C21 H21B 107.1 . . ? N1 C22 C23 120.1(4) . . ? N1 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 119.4(4) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 120.5(4) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C30 123.9(4) . . ? C24 C25 C26 118.2(4) . . ? C30 C25 C26 117.9(4) . . ? N1 C26 C27 120.6(3) . . ? N1 C26 C25 118.2(4) . . ? C27 C26 C25 121.3(4) . . ? C28 C27 C26 118.8(4) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C27 C28 C29 120.8(4) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 120.7(4) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C25 120.5(4) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? N2 C31 C32 121.2(5) . . ? N2 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C33 C32 C31 119.4(5) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 120.8(5) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C39 C34 C35 119.1(5) . . ? C39 C34 C33 123.9(5) . . ? C35 C34 C33 117.0(5) . . ? N2 C35 C34 119.7(4) . . ? N2 C35 C36 119.7(5) . . ? C34 C35 C36 120.6(5) . . ? C37 C36 C35 118.9(5) . . ? C37 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C36 C37 C38 121.0(5) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C39 C38 C37 120.3(6) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C34 120.1(5) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? N3 C40 C41 123.1(6) . . ? N3 C40 H40 118.4 . . ? C41 C40 H40 118.4 . . ? C40 C41 C42 115.8(8) . . ? C40 C41 H41 122.1 . . ? C42 C41 H41 122.1 . . ? C43 C42 C41 120.3(7) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C48 122.3(6) . . ? C42 C43 C44 120.1(6) . . ? C48 C43 C44 117.6(7) . . ? N3 C44 C45 123.6(7) . . ? N3 C44 C43 116.2(8) . . ? C45 C44 C43 120.2(6) . . ? C46 C45 C44 118.1(7) . . ? C46 C45 H45 120.9 . . ? C44 C45 H45 120.9 . . ? C45 C46 C47 122.8(9) . . ? C45 C46 H46 118.6 . . ? C47 C46 H46 118.6 . . ? C48 C47 C46 121.5(8) . . ? C48 C47 H47 119.2 . . ? C46 C47 H47 119.2 . . ? C47 C48 C43 119.7(6) . . ? C47 C48 H48 120.1 . . ? C43 C48 H48 120.1 . . ? O24 O23 O24 179.998(9) 2_577 . ? O25 O24 O23 161(2) . . ? O21 O26 O18 169.4(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -178.1(3) . . . . ? C6 C1 C2 C3 -0.1(5) . . . . ? O1 C1 C2 C21 1.2(5) . . . 2_656 ? C6 C1 C2 C21 179.3(3) . . . 2_656 ? C1 C2 C3 C4 0.7(5) . . . . ? C21 C2 C3 C4 -178.7(3) 2_656 . . . ? C2 C3 C4 C5 -0.8(5) . . . . ? C2 C3 C4 S1 -179.6(3) . . . . ? O5 S1 C4 C3 104.6(3) . . . . ? O4 S1 C4 C3 -17.2(3) . . . . ? O6 S1 C4 C3 -136.2(3) . . . . ? O5 S1 C4 C5 -74.2(3) . . . . ? O4 S1 C4 C5 163.9(3) . . . . ? O6 S1 C4 C5 45.0(3) . . . . ? C3 C4 C5 C6 0.4(5) . . . . ? S1 C4 C5 C6 179.2(3) . . . . ? C4 C5 C6 C1 0.2(5) . . . . ? C4 C5 C6 C7 -179.7(3) . . . . ? O1 C1 C6 C5 177.7(3) . . . . ? C2 C1 C6 C5 -0.3(5) . . . . ? O1 C1 C6 C7 -2.4(5) . . . . ? C2 C1 C6 C7 179.6(3) . . . . ? C5 C6 C7 C9 -86.0(4) . . . . ? C1 C6 C7 C9 94.1(4) . . . . ? O2 C8 C9 C10 -179.9(3) . . . . ? C13 C8 C9 C10 0.2(5) . . . . ? O2 C8 C9 C7 2.0(5) . . . . ? C13 C8 C9 C7 -177.9(3) . . . . ? C6 C7 C9 C10 105.1(4) . . . . ? C6 C7 C9 C8 -76.8(4) . . . . ? C8 C9 C10 C11 -1.0(5) . . . . ? C7 C9 C10 C11 177.1(3) . . . . ? C9 C10 C11 C12 0.4(5) . . . . ? C9 C10 C11 S2 178.1(3) . . . . ? O9 S2 C11 C12 -18.4(4) . . . . ? O8 S2 C11 C12 -139.9(3) . . . . ? O7 S2 C11 C12 102.0(3) . . . . ? O9 S2 C11 C10 163.9(3) . . . . ? O8 S2 C11 C10 42.4(3) . . . . ? O7 S2 C11 C10 -75.7(3) . . . . ? C10 C11 C12 C13 1.0(5) . . . . ? S2 C11 C12 C13 -176.7(3) . . . . ? C11 C12 C13 C8 -1.8(5) . . . . ? C11 C12 C13 C14 176.5(3) . . . . ? O2 C8 C13 C12 -178.7(3) . . . . ? C9 C8 C13 C12 1.2(5) . . . . ? O2 C8 C13 C14 3.0(5) . . . . ? C9 C8 C13 C14 -177.1(3) . . . . ? C12 C13 C14 C16 -77.0(4) . . . . ? C8 C13 C14 C16 101.3(4) . . . . ? O3 C15 C16 C17 -178.0(3) . . . . ? C20 C15 C16 C17 0.6(5) . . . . ? O3 C15 C16 C14 -3.0(6) . . . . ? C20 C15 C16 C14 175.6(3) . . . . ? C13 C14 C16 C17 99.4(4) . . . . ? C13 C14 C16 C15 -75.5(4) . . . . ? C15 C16 C17 C18 -0.1(6) . . . . ? C14 C16 C17 C18 -175.1(4) . . . . ? C16 C17 C18 C19 0.0(6) . . . . ? C16 C17 C18 S3 177.1(3) . . . . ? O11 S3 C18 C17 81.9(5) . . . . ? O12 S3 C18 C17 -154.0(5) . . . . ? O10 S3 C18 C17 -34.2(5) . . . . ? O11 S3 C18 C19 -101.1(5) . . . . ? O12 S3 C18 C19 23.1(5) . . . . ? O10 S3 C18 C19 142.8(5) . . . . ? C17 C18 C19 C20 -0.6(6) . . . . ? S3 C18 C19 C20 -177.6(3) . . . . ? C18 C19 C20 C15 1.1(6) . . . . ? C18 C19 C20 C21 174.4(4) . . . . ? O3 C15 C20 C19 177.5(3) . . . . ? C16 C15 C20 C19 -1.1(6) . . . . ? O3 C15 C20 C21 4.3(5) . . . . ? C16 C15 C20 C21 -174.4(3) . . . . ? C19 C20 C21 C2 106.5(4) . . . 2_656 ? C15 C20 C21 C2 -80.3(5) . . . 2_656 ? C26 N1 C22 C23 0.8(6) . . . . ? N1 C22 C23 C24 -0.8(6) . . . . ? C22 C23 C24 C25 -0.1(6) . . . . ? C23 C24 C25 C30 -179.0(4) . . . . ? C23 C24 C25 C26 1.0(6) . . . . ? C22 N1 C26 C27 179.7(4) . . . . ? C22 N1 C26 C25 0.2(6) . . . . ? C24 C25 C26 N1 -1.1(5) . . . . ? C30 C25 C26 N1 178.9(3) . . . . ? C24 C25 C26 C27 179.4(3) . . . . ? C30 C25 C26 C27 -0.5(5) . . . . ? N1 C26 C27 C28 -179.4(4) . . . . ? C25 C26 C27 C28 0.1(6) . . . . ? C26 C27 C28 C29 0.2(6) . . . . ? C27 C28 C29 C30 0.0(6) . . . . ? C28 C29 C30 C25 -0.4(6) . . . . ? C24 C25 C30 C29 -179.3(4) . . . . ? C26 C25 C30 C29 0.7(6) . . . . ? C35 N2 C31 C32 0.2(7) . . . . ? N2 C31 C32 C33 0.4(7) . . . . ? C31 C32 C33 C34 -0.6(7) . . . . ? C32 C33 C34 C39 -179.8(4) . . . . ? C32 C33 C34 C35 0.2(6) . . . . ? C31 N2 C35 C34 -0.6(6) . . . . ? C31 N2 C35 C36 -179.8(4) . . . . ? C39 C34 C35 N2 -179.6(4) . . . . ? C33 C34 C35 N2 0.4(6) . . . . ? C39 C34 C35 C36 -0.4(6) . . . . ? C33 C34 C35 C36 179.6(4) . . . . ? N2 C35 C36 C37 179.5(4) . . . . ? C34 C35 C36 C37 0.3(6) . . . . ? C35 C36 C37 C38 -0.3(7) . . . . ? C36 C37 C38 C39 0.5(7) . . . . ? C37 C38 C39 C34 -0.6(7) . . . . ? C35 C34 C39 C38 0.6(6) . . . . ? C33 C34 C39 C38 -179.4(4) . . . . ? C44 N3 C40 C41 -1.3(10) . . . . ? N3 C40 C41 C42 -0.8(9) . . . . ? C40 C41 C42 C43 2.0(8) . . . . ? C41 C42 C43 C48 179.1(5) . . . . ? C41 C42 C43 C44 -1.4(7) . . . . ? C40 N3 C44 C45 -177.9(6) . . . . ? C40 N3 C44 C43 2.0(8) . . . . ? C42 C43 C44 N3 -0.6(7) . . . . ? C48 C43 C44 N3 178.9(4) . . . . ? C42 C43 C44 C45 179.2(5) . . . . ? C48 C43 C44 C45 -1.3(7) . . . . ? N3 C44 C45 C46 -179.3(6) . . . . ? C43 C44 C45 C46 0.9(9) . . . . ? C44 C45 C46 C47 -0.6(10) . . . . ? C45 C46 C47 C48 0.8(10) . . . . ? C46 C47 C48 C43 -1.2(8) . . . . ? C42 C43 C48 C47 -179.1(5) . . . . ? C44 C43 C48 C47 1.4(7) . . . . ? O24 O23 O24 O25 20(100) 2_577 . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.871 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.099 # Attachment 'complex_4.cif' data_shelxl4 _database_code_depnum_ccdc_archive 'CCDC 657146' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H120 N6 O51 S6' _chemical_formula_sum 'C96 H120 N6 O51 S6' _chemical_formula_weight 2366.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.131(2) _cell_length_b 12.741(2) _cell_length_c 17.734(3) _cell_angle_alpha 102.191(3) _cell_angle_beta 103.227(4) _cell_angle_gamma 90.240(2) _cell_volume 2604.1(8) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7572 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1242 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9283 _exptl_absorpt_correction_T_max 0.9677 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24594 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.88 _reflns_number_total 12178 _reflns_number_gt 9198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0677P)^2^+1.9796P] 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 SHELXL _refine_ls_extinction_coef 0.0063(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12178 _refine_ls_number_parameters 870 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.094 _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 S1 S 0.83709(6) 1.01040(5) 0.83089(4) 0.03059(17) Uani 1 1 d D . . S2 S 0.77816(5) 0.95801(4) 0.43294(3) 0.01775(14) Uani 1 1 d . . . S3 S 0.59781(5) 0.47151(5) 0.17306(3) 0.02099(14) Uani 1 1 d . . . O1 O 0.57307(14) 0.63906(13) 0.60336(10) 0.0224(4) Uani 1 1 d . . . H1 H 0.5975 0.5815 0.6149 0.034 Uiso 1 1 calc R . . O2 O 0.33028(13) 0.79229(13) 0.44388(9) 0.0190(3) Uani 1 1 d . A . H2 H 0.3098 0.8275 0.4835 0.028 Uiso 1 1 calc R . . O3 O 0.21335(13) 0.61777(13) 0.31239(10) 0.0206(4) Uani 1 1 d . A . H3 H 0.2007 0.6827 0.3130 0.031 Uiso 1 1 calc R . . O4 O 0.9053(5) 1.0451(8) 0.7797(4) 0.0244(12) Uani 0.671(11) 1 d PDU A 1 O5 O 0.9183(4) 0.9658(2) 0.89235(19) 0.0251(11) Uani 0.671(11) 1 d PD A 1 O6 O 0.7658(6) 1.0892(5) 0.8580(4) 0.0290(11) Uani 0.671(11) 1 d PDU A 1 O4' O 0.9246(9) 1.0410(16) 0.7980(9) 0.025(3) Uani 0.329(11) 1 d PDU A 2 O5' O 0.8597(8) 0.9906(5) 0.9112(4) 0.030(3) Uani 0.329(11) 1 d PD A 2 O6' O 0.7523(11) 1.0975(11) 0.8351(7) 0.036(3) Uani 0.329(11) 1 d PDU A 2 O7 O 0.79060(15) 0.91520(14) 0.35195(10) 0.0257(4) Uani 1 1 d . . . O8 O 0.86540(14) 0.92473(15) 0.49269(11) 0.0264(4) Uani 1 1 d . . . O9 O 0.76958(13) 1.07459(13) 0.44765(10) 0.0208(4) Uani 1 1 d . . . O10 O 0.65113(15) 0.56580(15) 0.15888(11) 0.0274(4) Uani 1 1 d . . . O11 O 0.54514(17) 0.39626(19) 0.09858(13) 0.0453(6) Uani 1 1 d . . . O12 O 0.67323(17) 0.41940(17) 0.22718(12) 0.0357(5) Uani 1 1 d . . . O13 O 0.21987(16) 0.67616(14) 0.55347(11) 0.0281(4) Uani 1 1 d . . . H13 H 0.2554 0.6987 0.6009 0.042 Uiso 1 1 calc R . . O15 O 0.6431(2) 0.22308(17) 1.03694(13) 0.0439(5) Uani 1 1 d . . . H15 H 0.6122 0.2792 1.0539 0.066 Uiso 1 1 calc R . . O16 O 0.04156(15) 0.79984(15) 0.45364(12) 0.0282(4) Uani 1 1 d D . . H16A H 0.096(2) 0.839(2) 0.4877(15) 0.042 Uiso 1 1 d D . . H16B H -0.0204(17) 0.827(3) 0.4611(19) 0.042 Uiso 1 1 d D . . O17 O 0.94451(17) 0.90048(16) 0.64908(12) 0.0321(4) Uani 1 1 d D . . H17A H 0.918(3) 0.922(3) 0.6068(13) 0.048 Uiso 1 1 d D . . H17B H 0.926(3) 0.936(3) 0.6902(13) 0.048 Uiso 1 1 d D . . O18 O 0.83192(16) 0.08297(16) 0.27670(11) 0.0289(4) Uani 1 1 d D . . H18A H 0.805(3) 0.0312(19) 0.2917(19) 0.043 Uiso 1 1 d D . . H18B H 0.9007(12) 0.094(3) 0.3023(18) 0.043 Uiso 1 1 d D . . O19 O 0.68166(17) 0.24344(17) 0.29870(12) 0.0324(4) Uani 1 1 d D . . H19A H 0.729(2) 0.197(2) 0.289(2) 0.049 Uiso 1 1 d D . . H19B H 0.679(3) 0.291(2) 0.2712(18) 0.049 Uiso 1 1 d D . . O20 O 0.09606(18) 0.79682(18) 0.30905(13) 0.0379(5) Uani 1 1 d D . . H20A H 0.100(3) 0.853(2) 0.290(2) 0.057 Uiso 1 1 d D . . H20B H 0.075(3) 0.809(3) 0.3540(12) 0.057 Uiso 1 1 d D . . O21 O 0.4280(2) 0.5828(2) 0.45225(15) 0.0493(6) Uani 1 1 d D . . H21A H 0.456(3) 0.601(4) 0.5011(8) 0.074 Uiso 1 1 d D . . H21B H 0.377(3) 0.627(3) 0.444(3) 0.074 Uiso 1 1 d D . . O22 O 0.1223(2) 0.1664(2) 0.8565(2) 0.0690(9) Uani 1 1 d D . . H22A H 0.134(5) 0.173(5) 0.8118(18) 0.103 Uiso 1 1 d D . . H22B H 0.059(2) 0.130(4) 0.840(3) 0.103 Uiso 1 1 d D . . O23 O 0.8492(3) 0.0914(3) 0.12466(15) 0.0682(9) Uani 1 1 d D . . H23A H 0.854(4) 0.083(4) 0.1718(13) 0.102 Uiso 1 1 d D . . H23B H 0.800(4) 0.138(4) 0.130(3) 0.102 Uiso 1 1 d D . . O24 O 0.1768(2) 0.2826(2) 0.7464(2) 0.0725(10) Uani 1 1 d D . . H24A H 0.189(5) 0.246(4) 0.7036(18) 0.109 Uiso 1 1 d D . . H24B H 0.231(3) 0.328(3) 0.769(3) 0.109 Uiso 1 1 d D . . N1 N 0.05497(17) 0.58072(17) 0.42928(12) 0.0230(4) Uani 1 1 d . . . H1A H 0.0635 0.6511 0.4459 0.028 Uiso 1 1 calc R . . N3 N 0.67473(19) 0.01257(19) 0.99968(13) 0.0297(5) Uani 1 1 d . . . H3C H 0.7170 0.0558 1.0419 0.036 Uiso 1 1 calc R . . C1 C 0.63224(19) 0.72455(18) 0.65796(13) 0.0162(4) Uani 1 1 d . . . C2 C 0.72562(19) 0.70657(18) 0.71585(14) 0.0178(5) Uani 1 1 d . A . C3 C 0.7865(2) 0.79433(19) 0.76977(14) 0.0223(5) Uani 1 1 d . . . H3A H 0.8505 0.7833 0.8090 0.027 Uiso 1 1 calc R A . C4 C 0.7544(2) 0.89845(19) 0.76667(14) 0.0228(5) Uani 1 1 d . A . C5 C 0.6592(2) 0.91478(18) 0.71006(14) 0.0205(5) Uani 1 1 d . . . H5 H 0.6365 0.9859 0.7092 0.025 Uiso 1 1 calc R A . C6 C 0.59712(19) 0.82882(18) 0.65506(13) 0.0169(4) Uani 1 1 d . A . C7 C 0.76180(19) 0.59388(18) 0.71764(14) 0.0182(5) Uani 1 1 d . . . H7A H 0.8352 0.5985 0.7569 0.022 Uiso 1 1 calc R A . H7B H 0.7750 0.5604 0.6650 0.022 Uiso 1 1 calc R . . C8 C 0.49481(19) 0.84734(18) 0.59349(13) 0.0168(4) Uani 1 1 d . . . H8A H 0.4601 0.9135 0.6156 0.020 Uiso 1 1 calc R A . H8B H 0.4383 0.7865 0.5827 0.020 Uiso 1 1 calc R . . C9 C 0.43680(18) 0.82920(17) 0.44435(13) 0.0150(4) Uani 1 1 d . . . C10 C 0.52088(18) 0.85843(17) 0.51544(13) 0.0149(4) Uani 1 1 d . A . C11 C 0.62663(18) 0.89655(17) 0.51149(13) 0.0163(4) Uani 1 1 d . . . H11 H 0.6846 0.9184 0.5587 0.020 Uiso 1 1 calc R A . C12 C 0.64763(18) 0.90268(17) 0.43841(13) 0.0161(4) Uani 1 1 d . A . C13 C 0.56519(19) 0.86847(17) 0.36859(13) 0.0168(4) Uani 1 1 d . . . H13A H 0.5818 0.8708 0.3191 0.020 Uiso 1 1 calc R A . C14 C 0.45878(19) 0.83089(17) 0.37058(13) 0.0158(4) Uani 1 1 d . A . C15 C 0.37140(19) 0.78656(17) 0.29376(13) 0.0165(4) Uani 1 1 d . . . H15A H 0.3848 0.8216 0.2516 0.020 Uiso 1 1 calc R A . H15B H 0.2944 0.8027 0.3014 0.020 Uiso 1 1 calc R . . C16 C 0.30382(18) 0.59125(18) 0.28053(13) 0.0150(4) Uani 1 1 d . . . C17 C 0.37893(18) 0.66570(17) 0.26837(13) 0.0155(4) Uani 1 1 d . A . C18 C 0.46832(19) 0.62730(18) 0.23487(13) 0.0171(4) Uani 1 1 d . . . H18 H 0.5191 0.6768 0.2249 0.021 Uiso 1 1 calc R A . C19 C 0.48440(19) 0.51811(18) 0.21586(13) 0.0175(4) Uani 1 1 d . A . C20 C 0.41046(19) 0.44446(18) 0.23032(13) 0.0169(4) Uani 1 1 d . . . H20 H 0.4224 0.3697 0.2181 0.020 Uiso 1 1 calc R A . C21 C 0.31997(18) 0.47977(17) 0.26238(13) 0.0151(4) Uani 1 1 d . . . C22 C 0.2154(2) 0.5669(2) 0.53544(15) 0.0239(5) Uani 1 1 d . . . C23 C 0.2873(2) 0.5028(2) 0.57412(15) 0.0264(5) Uani 1 1 d . . . H23 H 0.3464 0.5346 0.6185 0.032 Uiso 1 1 calc R . . C24 C 0.2749(2) 0.3893(2) 0.54872(16) 0.0283(6) Uani 1 1 d . . . H24 H 0.3262 0.3463 0.5762 0.034 Uiso 1 1 calc R . . C25 C 0.1905(2) 0.3405(2) 0.48555(15) 0.0251(5) Uani 1 1 d . . . H25 H 0.1829 0.2643 0.4696 0.030 Uiso 1 1 calc R . . C26 C 0.1145(2) 0.40446(19) 0.44400(15) 0.0214(5) Uani 1 1 d . . . C27 C 0.1284(2) 0.51783(19) 0.46954(14) 0.0205(5) Uani 1 1 d . . . C28 C -0.0274(2) 0.5400(2) 0.36702(15) 0.0255(5) Uani 1 1 d . . . H28 H -0.0751 0.5867 0.3406 0.031 Uiso 1 1 calc R . . C29 C -0.0451(2) 0.4288(2) 0.33961(16) 0.0266(5) Uani 1 1 d . . . H29 H -0.1049 0.3995 0.2949 0.032 Uiso 1 1 calc R . . C30 C 0.0248(2) 0.3620(2) 0.37789(15) 0.0238(5) Uani 1 1 d . . . H30 H 0.0126 0.2863 0.3596 0.029 Uiso 1 1 calc R . . C40 C 0.5735(3) 0.1660(2) 0.96947(16) 0.0319(6) Uani 1 1 d . . . C41 C 0.4892(3) 0.2067(2) 0.91962(18) 0.0373(7) Uani 1 1 d . . . H41 H 0.4764 0.2813 0.9312 0.045 Uiso 1 1 calc R . . C42 C 0.4218(3) 0.1388(2) 0.85151(17) 0.0347(6) Uani 1 1 d . . . H42 H 0.3633 0.1685 0.8181 0.042 Uiso 1 1 calc R . . C43 C 0.4380(2) 0.0312(2) 0.83214(16) 0.0292(6) Uani 1 1 d . . . H43 H 0.3919 -0.0131 0.7856 0.035 Uiso 1 1 calc R . . C44 C 0.5247(2) -0.0137(2) 0.88244(15) 0.0241(5) Uani 1 1 d . . . C45 C 0.5916(2) 0.0553(2) 0.95058(14) 0.0245(5) Uani 1 1 d . . . C46 C 0.6941(2) -0.0900(2) 0.98652(17) 0.0337(6) Uani 1 1 d . . . H46 H 0.7528 -0.1156 1.0224 0.040 Uiso 1 1 calc R . . C47 C 0.6298(2) -0.1620(2) 0.92069(17) 0.0351(6) Uani 1 1 d . . . H47 H 0.6437 -0.2364 0.9119 0.042 Uiso 1 1 calc R . . C48 C 0.5466(2) -0.1239(2) 0.86903(16) 0.0293(6) Uani 1 1 d . . . H48 H 0.5029 -0.1722 0.8235 0.035 Uiso 1 1 calc R . . O14 O 0.1666(2) 0.3126(2) -0.00343(17) 0.0335(7) Uani 0.667(3) 1 d P B 1 H14A H 0.1366 0.2671 -0.0450 0.050 Uiso 0.667(3) 1 calc PR B 1 C31 C 0.08598(18) 0.34435(13) 0.03972(12) 0.0262(10) Uani 0.667(3) 1 d PG B 1 C32 C 0.0016(2) 0.27784(13) 0.04946(14) 0.0305(9) Uani 0.667(3) 1 d PG B 1 H32A H -0.0037 0.2032 0.0260 0.037 Uiso 0.667(3) 1 calc PR B 1 C33 C -0.07515(18) 0.32057(17) 0.09358(15) 0.0301(10) Uani 0.667(3) 1 d PG B 1 H33A H -0.1328 0.2751 0.1002 0.036 Uiso 0.667(3) 1 calc PR B 1 C34 C -0.06743(16) 0.42981(17) 0.12797(14) 0.0285(13) Uani 0.667(3) 1 d PG B 1 H34A H -0.1199 0.4590 0.1581 0.034 Uiso 0.667(3) 1 calc PR B 1 C35 C 0.01698(13) 0.49632(13) 0.11823(10) 0.0224(8) Uani 0.667(3) 1 d PG B 1 C36 C 0.09369(13) 0.45359(13) 0.07411(9) 0.0209(9) Uani 0.667(3) 1 d PGU B 1 N2 N 0.17811(15) 0.52009(16) 0.06437(13) 0.0215(8) Uani 0.667(3) 1 d PG B 1 H2A H 0.2267 0.4930 0.0364 0.026 Uiso 0.667(3) 1 calc PR B 1 C37 C 0.18583(18) 0.62933(16) 0.09876(14) 0.0266(9) Uani 0.667(3) 1 d PG B 1 H37A H 0.2435 0.6748 0.0921 0.032 Uiso 0.667(3) 1 calc PR B 1 C38 C 0.1091(2) 0.67206(13) 0.14289(15) 0.0285(10) Uani 0.667(3) 1 d PGU B 1 H38A H 0.1144 0.7467 0.1664 0.034 Uiso 0.667(3) 1 calc PR B 1 C39 C 0.02470(19) 0.60556(14) 0.15262(13) 0.0265(9) Uani 0.667(3) 1 d PG B 1 H39A H -0.0277 0.6348 0.1828 0.032 Uiso 0.667(3) 1 calc PR B 1 O25 O 0.3602(2) 0.4909(3) 0.00890(17) 0.0389(8) Uani 0.667(3) 1 d P B 1 O14' O 0.0786(6) 0.2909(5) 0.0260(4) 0.0284(15) Uani 0.333(3) 1 d P B 2 H14B H 0.0436 0.2350 0.0282 0.043 Uiso 0.333(3) 1 calc PR B 2 C31' C 0.0422(3) 0.3782(2) 0.0708(3) 0.0246(17) Uani 0.333(3) 1 d PG B 2 C32' C -0.0488(3) 0.3775(3) 0.1062(3) 0.0238(19) Uani 0.333(3) 1 d PG B 2 H32B H -0.0892 0.3117 0.1020 0.029 Uiso 0.333(3) 1 calc PR B 2 C33' C -0.0807(3) 0.4731(4) 0.1477(3) 0.030(2) Uani 0.333(3) 1 d PG B 2 H33B H -0.1429 0.4727 0.1719 0.036 Uiso 0.333(3) 1 calc PR B 2 C34' C -0.0216(3) 0.5694(3) 0.1538(3) 0.032(2) Uani 0.333(3) 1 d PG B 2 H34B H -0.0434 0.6348 0.1822 0.038 Uiso 0.333(3) 1 calc PR B 2 C35' C 0.0694(3) 0.5701(2) 0.11846(19) 0.0234(16) Uani 0.333(3) 1 d PG B 2 C36' C 0.1013(3) 0.4745(2) 0.07694(18) 0.0222(18) Uani 0.333(3) 1 d PGU B 2 N2' N 0.1923(3) 0.4752(3) 0.0416(3) 0.0291(18) Uani 0.333(3) 1 d PG B 2 H2'A H 0.2125 0.4146 0.0153 0.035 Uiso 0.333(3) 1 calc PR B 2 C37' C 0.2514(3) 0.5715(3) 0.0477(3) 0.0265(17) Uani 0.333(3) 1 d PG B 2 H37B H 0.3136 0.5719 0.0235 0.032 Uiso 0.333(3) 1 calc PR B 2 C38' C 0.2195(4) 0.6671(3) 0.0892(3) 0.0287(19) Uani 0.333(3) 1 d PG B 2 H38B H 0.2599 0.7329 0.0934 0.034 Uiso 0.333(3) 1 calc PR B 2 C39' C 0.1285(4) 0.6664(2) 0.1246(3) 0.0150(15) Uani 0.333(3) 1 d PGU B 2 H39B H 0.1067 0.7318 0.1530 0.018 Uiso 0.333(3) 1 calc PR B 2 O25' O 0.2654(5) 0.3270(4) -0.0574(3) 0.0274(13) Uani 0.333(3) 1 d P B 2 O25" O -0.0294(5) 0.1134(4) 0.0315(3) 0.0640(14) Uani 0.50 1 d P C 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 S1 0.0454(4) 0.0184(3) 0.0223(3) 0.0063(2) -0.0050(3) -0.0142(3) S2 0.0158(3) 0.0133(3) 0.0245(3) 0.0030(2) 0.0065(2) -0.0001(2) S3 0.0239(3) 0.0182(3) 0.0205(3) -0.0013(2) 0.0096(2) -0.0011(2) O1 0.0280(9) 0.0153(8) 0.0206(8) 0.0007(6) 0.0023(7) -0.0060(7) O2 0.0164(8) 0.0208(8) 0.0186(8) 0.0012(6) 0.0047(6) -0.0023(6) O3 0.0184(8) 0.0167(8) 0.0297(9) 0.0087(7) 0.0084(7) 0.0030(6) O4 0.019(2) 0.0202(17) 0.027(3) -0.002(2) -0.004(2) -0.007(2) O5 0.022(2) 0.0217(15) 0.0276(16) 0.0057(12) -0.0031(13) 0.0009(13) O6 0.041(2) 0.0311(18) 0.013(3) -0.0085(19) 0.013(2) -0.0159(14) O4' 0.009(3) 0.023(4) 0.031(6) -0.004(4) -0.012(4) -0.003(3) O5' 0.033(5) 0.024(3) 0.026(3) 0.008(3) -0.010(3) -0.003(3) O6' 0.054(5) 0.042(4) 0.005(5) -0.012(3) 0.011(4) -0.025(3) O7 0.0283(9) 0.0232(9) 0.0266(9) 0.0005(7) 0.0129(8) -0.0035(7) O8 0.0172(8) 0.0284(10) 0.0352(10) 0.0121(8) 0.0045(7) 0.0031(7) O9 0.0179(8) 0.0137(8) 0.0308(9) 0.0029(7) 0.0075(7) -0.0008(6) O10 0.0285(9) 0.0282(10) 0.0300(10) 0.0082(8) 0.0142(8) -0.0014(8) O11 0.0345(11) 0.0501(14) 0.0376(12) -0.0247(10) 0.0124(9) -0.0041(10) O12 0.0368(11) 0.0358(11) 0.0447(12) 0.0182(9) 0.0213(9) 0.0166(9) O13 0.0335(10) 0.0199(9) 0.0283(10) 0.0038(7) 0.0036(8) -0.0011(7) O15 0.0582(14) 0.0276(11) 0.0350(12) -0.0120(9) 0.0064(10) -0.0022(10) O16 0.0203(9) 0.0224(10) 0.0388(11) 0.0026(8) 0.0043(8) 0.0022(7) O17 0.0344(11) 0.0261(10) 0.0304(11) 0.0019(8) 0.0005(9) 0.0015(8) O18 0.0285(10) 0.0294(10) 0.0305(10) 0.0130(8) 0.0041(8) -0.0001(8) O19 0.0334(11) 0.0278(11) 0.0353(11) 0.0090(8) 0.0046(9) 0.0022(8) O20 0.0374(11) 0.0406(13) 0.0394(12) 0.0141(10) 0.0115(10) 0.0128(10) O21 0.0465(13) 0.0640(16) 0.0548(14) 0.0432(13) 0.0186(12) 0.0283(12) O22 0.0286(12) 0.0331(14) 0.116(2) -0.0110(15) -0.0167(15) 0.0013(10) O23 0.080(2) 0.084(2) 0.0306(13) 0.0189(14) -0.0128(14) -0.0474(16) O24 0.0261(12) 0.0377(15) 0.128(3) -0.0292(15) 0.0086(15) -0.0004(10) N1 0.0264(11) 0.0175(10) 0.0300(11) 0.0070(8) 0.0148(9) 0.0012(8) N3 0.0295(12) 0.0330(13) 0.0211(11) -0.0016(9) 0.0017(9) -0.0051(10) C1 0.0178(11) 0.0144(11) 0.0167(11) 0.0046(8) 0.0038(9) -0.0025(8) C2 0.0181(11) 0.0147(11) 0.0215(11) 0.0073(9) 0.0038(9) -0.0022(8) C3 0.0230(12) 0.0199(12) 0.0225(12) 0.0105(10) -0.0030(10) -0.0064(9) C4 0.0310(13) 0.0159(11) 0.0199(12) 0.0059(9) 0.0010(10) -0.0074(10) C5 0.0285(12) 0.0133(11) 0.0194(11) 0.0056(9) 0.0034(10) -0.0020(9) C6 0.0202(11) 0.0143(11) 0.0173(11) 0.0061(8) 0.0042(9) -0.0003(8) C7 0.0163(11) 0.0154(11) 0.0236(12) 0.0091(9) 0.0020(9) -0.0021(8) C8 0.0187(11) 0.0141(10) 0.0174(11) 0.0035(8) 0.0038(9) 0.0018(8) C9 0.0161(10) 0.0090(10) 0.0203(11) 0.0026(8) 0.0057(9) 0.0006(8) C10 0.0162(10) 0.0098(10) 0.0186(11) 0.0038(8) 0.0030(9) 0.0021(8) C11 0.0166(11) 0.0112(10) 0.0206(11) 0.0036(8) 0.0032(9) 0.0019(8) C12 0.0173(11) 0.0097(10) 0.0218(11) 0.0026(8) 0.0060(9) 0.0014(8) C13 0.0212(11) 0.0113(10) 0.0192(11) 0.0031(8) 0.0078(9) 0.0018(8) C14 0.0189(11) 0.0079(9) 0.0199(11) 0.0032(8) 0.0030(9) 0.0022(8) C15 0.0212(11) 0.0111(10) 0.0160(11) 0.0037(8) 0.0018(9) -0.0002(8) C16 0.0151(10) 0.0155(11) 0.0144(10) 0.0054(8) 0.0016(8) 0.0010(8) C17 0.0178(11) 0.0134(10) 0.0139(10) 0.0043(8) -0.0003(8) -0.0012(8) C18 0.0199(11) 0.0167(11) 0.0141(10) 0.0035(8) 0.0024(9) -0.0034(9) C19 0.0216(11) 0.0155(11) 0.0147(10) 0.0008(8) 0.0053(9) -0.0023(9) C20 0.0222(11) 0.0121(10) 0.0151(11) 0.0023(8) 0.0024(9) -0.0020(8) C21 0.0175(11) 0.0131(10) 0.0138(10) 0.0047(8) 0.0003(8) -0.0026(8) C22 0.0254(12) 0.0211(12) 0.0277(13) 0.0028(10) 0.0133(10) -0.0014(10) C23 0.0254(13) 0.0284(14) 0.0252(13) 0.0024(10) 0.0087(11) -0.0032(10) C24 0.0280(13) 0.0290(14) 0.0329(14) 0.0117(11) 0.0127(11) 0.0073(11) C25 0.0281(13) 0.0186(12) 0.0322(14) 0.0049(10) 0.0151(11) 0.0048(10) C26 0.0242(12) 0.0177(12) 0.0264(12) 0.0043(9) 0.0148(10) 0.0016(9) C27 0.0208(11) 0.0198(12) 0.0244(12) 0.0041(9) 0.0128(10) 0.0018(9) C28 0.0231(12) 0.0281(13) 0.0280(13) 0.0085(11) 0.0095(11) 0.0028(10) C29 0.0257(13) 0.0272(14) 0.0277(13) 0.0042(10) 0.0094(11) -0.0022(10) C30 0.0256(12) 0.0204(12) 0.0282(13) 0.0031(10) 0.0140(11) -0.0012(10) C40 0.0418(16) 0.0259(14) 0.0263(14) -0.0025(11) 0.0124(12) -0.0018(12) C41 0.0541(19) 0.0266(15) 0.0349(16) 0.0053(12) 0.0190(14) 0.0072(13) C42 0.0397(16) 0.0393(17) 0.0298(15) 0.0125(12) 0.0129(13) 0.0113(13) C43 0.0288(13) 0.0342(15) 0.0238(13) 0.0051(11) 0.0060(11) -0.0001(11) C44 0.0223(12) 0.0270(13) 0.0222(12) 0.0005(10) 0.0084(10) -0.0021(10) C45 0.0256(12) 0.0270(13) 0.0203(12) -0.0003(10) 0.0093(10) -0.0025(10) C46 0.0306(14) 0.0367(16) 0.0301(14) 0.0031(12) 0.0034(12) 0.0063(12) C47 0.0402(16) 0.0275(15) 0.0317(15) -0.0037(11) 0.0059(12) 0.0077(12) C48 0.0308(14) 0.0270(14) 0.0242(13) -0.0048(10) 0.0043(11) -0.0019(11) O14 0.0281(15) 0.0342(17) 0.0302(16) -0.0084(12) 0.0052(12) 0.0056(12) C31 0.028(2) 0.025(2) 0.020(2) 0.004(2) -0.0061(17) 0.001(2) C32 0.034(2) 0.023(2) 0.031(2) 0.0099(16) -0.0024(18) -0.0017(17) C33 0.028(2) 0.032(2) 0.032(2) 0.017(2) 0.0020(18) -0.0058(19) C34 0.025(2) 0.038(3) 0.028(3) 0.016(2) 0.0100(19) 0.010(2) C35 0.0217(18) 0.026(2) 0.0198(18) 0.0095(15) 0.0016(14) 0.0041(15) C36 0.0209(19) 0.0275(19) 0.0157(18) 0.0090(14) 0.0031(16) 0.0037(16) N2 0.0168(16) 0.026(2) 0.0221(18) 0.0122(15) -0.0004(13) 0.0014(15) C37 0.025(2) 0.033(2) 0.023(2) 0.0171(18) -0.0021(17) -0.0062(18) C38 0.033(2) 0.026(2) 0.022(2) 0.0007(15) 0.0015(18) 0.0044(16) C39 0.025(2) 0.030(2) 0.022(2) 0.0068(18) -0.0009(18) 0.0059(18) O25 0.0324(16) 0.062(2) 0.0252(15) 0.0103(14) 0.0119(13) -0.0012(15) O14' 0.039(4) 0.017(3) 0.027(3) -0.001(3) 0.007(3) 0.000(3) C31' 0.033(4) 0.027(4) 0.016(4) 0.000(3) 0.012(3) 0.010(3) C32' 0.019(4) 0.022(5) 0.030(5) 0.015(4) -0.003(3) -0.006(4) C33' 0.011(4) 0.058(7) 0.024(5) 0.013(5) 0.009(3) 0.017(4) C34' 0.024(5) 0.027(5) 0.040(5) 0.004(4) 0.001(4) -0.006(3) C35' 0.024(4) 0.022(4) 0.021(4) 0.006(3) -0.002(3) 0.002(3) C36' 0.023(3) 0.021(3) 0.013(3) -0.004(2) -0.008(3) 0.004(3) N2' 0.030(4) 0.011(4) 0.046(5) 0.011(3) 0.005(3) 0.010(3) C37' 0.025(4) 0.027(4) 0.026(4) 0.003(3) 0.004(3) 0.001(3) C38' 0.039(5) 0.029(5) 0.021(4) 0.010(3) 0.008(4) -0.007(4) C39' 0.023(3) 0.017(3) 0.005(3) 0.000(2) 0.005(2) 0.003(2) O25' 0.030(3) 0.024(3) 0.028(3) 0.003(2) 0.008(2) 0.003(2) O25" 0.074(4) 0.050(3) 0.065(4) 0.011(3) 0.012(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O6 1.407(4) . ? S1 O4' 1.412(8) . ? S1 O5' 1.464(5) . ? S1 O4 1.488(4) . ? S1 O5 1.502(3) . ? S1 O6' 1.518(8) . ? S1 C4 1.765(2) . ? S2 O8 1.4501(18) . ? S2 O9 1.4613(17) . ? S2 O7 1.4671(18) . ? S2 C12 1.762(2) . ? S3 O12 1.439(2) . ? S3 O10 1.4561(18) . ? S3 O11 1.465(2) . ? S3 C19 1.765(2) . ? O1 C1 1.367(3) . ? O1 H1 0.8400 . ? O2 C9 1.371(3) . ? O2 H2 0.8400 . ? O3 C16 1.358(3) . ? O3 H3 0.8400 . ? O13 C22 1.359(3) . ? O13 H13 0.8400 . ? O15 C40 1.356(3) . ? O15 H15 0.8400 . ? O16 H16A 0.857(10) . ? O16 H16B 0.857(10) . ? O17 H17A 0.847(10) . ? O17 H17B 0.848(10) . ? O18 H18A 0.849(10) . ? O18 H18B 0.848(10) . ? O19 H19A 0.849(10) . ? O19 H19B 0.851(10) . ? O20 H20A 0.865(10) . ? O20 H20B 0.874(10) . ? O21 H21A 0.836(10) . ? O21 H21B 0.848(10) . ? O22 H22A 0.856(10) . ? O22 H22B 0.852(11) . ? O23 H23A 0.854(10) . ? O23 H23B 0.850(10) . ? O24 H24A 0.845(10) . ? O24 H24B 0.847(11) . ? N1 C28 1.318(3) . ? N1 C27 1.379(3) . ? N1 H1A 0.8800 . ? N3 C46 1.310(4) . ? N3 C45 1.369(3) . ? N3 H3C 0.8800 . ? C1 C2 1.400(3) . ? C1 C6 1.404(3) . ? C2 C3 1.389(3) . ? C2 C7 1.508(3) . ? C3 C4 1.393(3) . ? C3 H3A 0.9500 . ? C4 C5 1.394(3) . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 C8 1.510(3) . ? C7 C21 1.511(3) 2_666 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.523(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.398(3) . ? C9 C10 1.407(3) . ? C10 C11 1.392(3) . ? C11 C12 1.394(3) . ? C11 H11 0.9500 . ? C12 C13 1.387(3) . ? C13 C14 1.385(3) . ? C13 H13A 0.9500 . ? C14 C15 1.519(3) . ? C15 C17 1.520(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.395(3) . ? C16 C21 1.413(3) . ? C17 C18 1.395(3) . ? C18 C19 1.386(3) . ? C18 H18 0.9500 . ? C19 C20 1.397(3) . ? C20 C21 1.383(3) . ? C20 H20 0.9500 . ? C21 C7 1.511(3) 2_666 ? C22 C23 1.367(4) . ? C22 C27 1.411(4) . ? C23 C24 1.417(4) . ? C23 H23 0.9500 . ? C24 C25 1.365(4) . ? C24 H24 0.9500 . ? C25 C26 1.417(3) . ? C25 H25 0.9500 . ? C26 C30 1.413(4) . ? C26 C27 1.417(3) . ? C28 C29 1.397(4) . ? C28 H28 0.9500 . ? C29 C30 1.375(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C40 C41 1.371(4) . ? C40 C45 1.410(4) . ? C41 C42 1.406(4) . ? C41 H41 0.9500 . ? C42 C43 1.369(4) . ? C42 H42 0.9500 . ? C43 C44 1.421(4) . ? C43 H43 0.9500 . ? C44 C48 1.410(4) . ? C44 C45 1.410(4) . ? C46 C47 1.392(4) . ? C46 H46 0.9500 . ? C47 C48 1.365(4) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? O14 C31 1.386(3) . ? O14 H14A 0.8400 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C32 H32A 0.9500 . ? C33 C34 1.3900 . ? C33 H33A 0.9500 . ? C34 C35 1.3900 . ? C34 H34A 0.9500 . ? C35 C36 1.3900 . ? C35 C39 1.3900 . ? C36 N2 1.3900 . ? N2 C37 1.3900 . ? N2 H2A 0.8800 . ? C37 C38 1.3900 . ? C37 H37A 0.9500 . ? C38 C39 1.3900 . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? O14' C31' 1.362(7) . ? O14' H14B 0.8400 . ? C31' C32' 1.3900 . ? C31' C36' 1.3900 . ? C32' C33' 1.3900 . ? C32' H32B 0.9500 . ? C33' C34' 1.3900 . ? C33' H33B 0.9500 . ? C34' C35' 1.3900 . ? C34' H34B 0.9500 . ? C35' C36' 1.3900 . ? C35' C39' 1.3900 . ? C36' N2' 1.3900 . ? N2' C37' 1.3900 . ? N2' H2'A 0.8800 . ? C37' C38' 1.3900 . ? C37' H37B 0.9500 . ? C38' C39' 1.3900 . ? C38' H38B 0.9500 . ? C39' H39B 0.9500 . ? 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 O6 S1 O4' 118.8(9) . . ? O6 S1 O5' 85.3(4) . . ? O4' S1 O5' 122.0(5) . . ? O6 S1 O4 113.4(4) . . ? O4' S1 O4 14.3(7) . . ? O5' S1 O4 136.2(4) . . ? O6 S1 O5 117.3(2) . . ? O4' S1 O5 92.8(5) . . ? O5' S1 O5 34.7(3) . . ? O4 S1 O5 106.6(3) . . ? O6 S1 O6' 16.6(5) . . ? O4' S1 O6' 109.9(8) . . ? O5' S1 O6' 101.9(4) . . ? O4 S1 O6' 101.6(7) . . ? O5 S1 O6' 133.7(4) . . ? O6 S1 C4 109.8(3) . . ? O4' S1 C4 110.9(8) . . ? O5' S1 C4 107.3(2) . . ? O4 S1 C4 102.8(4) . . ? O5 S1 C4 105.70(14) . . ? O6' S1 C4 102.9(6) . . ? O8 S2 O9 112.68(11) . . ? O8 S2 O7 112.77(11) . . ? O9 S2 O7 110.89(10) . . ? O8 S2 C12 107.01(10) . . ? O9 S2 C12 106.76(10) . . ? O7 S2 C12 106.26(11) . . ? O12 S3 O10 112.98(12) . . ? O12 S3 O11 111.95(14) . . ? O10 S3 O11 111.57(13) . . ? O12 S3 C19 108.38(11) . . ? O10 S3 C19 106.14(11) . . ? O11 S3 C19 105.29(11) . . ? C1 O1 H1 109.5 . . ? C9 O2 H2 109.5 . . ? C16 O3 H3 109.5 . . ? C22 O13 H13 109.5 . . ? C40 O15 H15 109.5 . . ? H16A O16 H16B 107(3) . . ? H17A O17 H17B 115(4) . . ? H18A O18 H18B 106(3) . . ? H19A O19 H19B 112(3) . . ? H20A O20 H20B 114(4) . . ? H21A O21 H21B 103(4) . . ? H22A O22 H22B 99(5) . . ? H23A O23 H23B 91(5) . . ? H24A O24 H24B 110(5) . . ? C28 N1 C27 122.8(2) . . ? C28 N1 H1A 118.6 . . ? C27 N1 H1A 118.6 . . ? C46 N3 C45 122.8(2) . . ? C46 N3 H3C 118.6 . . ? C45 N3 H3C 118.6 . . ? O1 C1 C2 119.6(2) . . ? O1 C1 C6 119.05(19) . . ? C2 C1 C6 121.4(2) . . ? C3 C2 C1 118.9(2) . . ? C3 C2 C7 120.7(2) . . ? C1 C2 C7 120.4(2) . . ? C2 C3 C4 120.5(2) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C3 C4 C5 119.9(2) . . ? C3 C4 S1 120.48(19) . . ? C5 C4 S1 119.58(18) . . ? C6 C5 C4 121.0(2) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 118.3(2) . . ? C5 C6 C8 120.6(2) . . ? C1 C6 C8 121.0(2) . . ? C2 C7 C21 116.15(19) . 2_666 ? C2 C7 H7A 108.3 . . ? C21 C7 H7A 108.3 2_666 . ? C2 C7 H7B 108.3 . . ? C21 C7 H7B 108.3 2_666 . ? H7A C7 H7B 107.4 . . ? C6 C8 C10 114.13(18) . . ? C6 C8 H8A 108.7 . . ? C10 C8 H8A 108.7 . . ? C6 C8 H8B 108.7 . . ? C10 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? O2 C9 C14 116.63(19) . . ? O2 C9 C10 121.21(19) . . ? C14 C9 C10 122.1(2) . . ? C11 C10 C9 118.0(2) . . ? C11 C10 C8 122.1(2) . . ? C9 C10 C8 119.90(19) . . ? C10 C11 C12 120.1(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.9(2) . . ? C13 C12 S2 118.41(17) . . ? C11 C12 S2 120.66(17) . . ? C14 C13 C12 120.4(2) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C9 118.4(2) . . ? C13 C14 C15 120.2(2) . . ? C9 C14 C15 121.3(2) . . ? C14 C15 C17 110.33(17) . . ? C14 C15 H15A 109.6 . . ? C17 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C17 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? O3 C16 C17 124.3(2) . . ? O3 C16 C21 114.55(19) . . ? C17 C16 C21 121.1(2) . . ? C18 C17 C16 118.3(2) . . ? C18 C17 C15 118.5(2) . . ? C16 C17 C15 123.1(2) . . ? C19 C18 C17 121.1(2) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 120.0(2) . . ? C18 C19 S3 120.27(17) . . ? C20 C19 S3 119.74(18) . . ? C21 C20 C19 120.3(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C16 119.1(2) . . ? C20 C21 C7 123.8(2) . 2_666 ? C16 C21 C7 117.1(2) . 2_666 ? O13 C22 C23 126.1(2) . . ? O13 C22 C27 115.2(2) . . ? C23 C22 C27 118.6(2) . . ? C22 C23 C24 120.8(2) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 121.3(2) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 119.4(2) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C30 C26 C27 117.4(2) . . ? C30 C26 C25 123.9(2) . . ? C27 C26 C25 118.7(2) . . ? N1 C27 C22 119.8(2) . . ? N1 C27 C26 119.1(2) . . ? C22 C27 C26 121.1(2) . . ? N1 C28 C29 120.4(2) . . ? N1 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 119.4(2) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C26 120.9(2) . . ? C29 C30 H30 119.6 . . ? C26 C30 H30 119.6 . . ? O15 C40 C41 125.8(3) . . ? O15 C40 C45 115.5(3) . . ? C41 C40 C45 118.6(3) . . ? C40 C41 C42 120.5(3) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C43 C42 C41 121.8(3) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C42 C43 C44 119.3(3) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C48 C44 C45 117.9(2) . . ? C48 C44 C43 123.8(2) . . ? C45 C44 C43 118.3(2) . . ? N3 C45 C40 119.8(2) . . ? N3 C45 C44 118.7(2) . . ? C40 C45 C44 121.5(2) . . ? N3 C46 C47 121.0(3) . . ? N3 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C48 C47 C46 118.9(3) . . ? C48 C47 H47 120.5 . . ? C46 C47 H47 120.5 . . ? C47 C48 C44 120.8(2) . . ? C47 C48 H48 119.6 . . ? C44 C48 H48 119.6 . . ? C31 O14 H14A 109.5 . . ? O14 C31 C32 125.88(17) . . ? O14 C31 C36 114.12(17) . . ? C32 C31 C36 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 C39 120.0 . . ? C34 C35 C39 120.0 . . ? C35 C36 N2 120.0 . . ? C35 C36 C31 120.0 . . ? N2 C36 C31 120.0 . . ? C36 N2 C37 120.0 . . ? C36 N2 H2A 120.0 . . ? C37 N2 H2A 120.0 . . ? C38 C37 N2 120.0 . . ? C38 C37 H37A 120.0 . . ? N2 C37 H37A 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C38 C39 C35 120.0 . . ? C38 C39 H39A 120.0 . . ? C35 C39 H39A 120.0 . . ? C31' O14' H14B 109.5 . . ? O14' C31' C32' 125.5(3) . . ? O14' C31' C36' 114.4(3) . . ? C32' C31' C36' 120.0 . . ? C33' C32' C31' 120.0 . . ? C33' C32' H32B 120.0 . . ? C31' C32' H32B 120.0 . . ? C32' C33' C34' 120.0 . . ? C32' C33' H33B 120.0 . . ? C34' C33' H33B 120.0 . . ? C33' C34' C35' 120.0 . . ? C33' C34' H34B 120.0 . . ? C35' C34' H34B 120.0 . . ? C34' C35' C36' 120.0 . . ? C34' C35' C39' 120.0 . . ? C36' C35' C39' 120.0 . . ? C35' C36' N2' 120.0 . . ? C35' C36' C31' 120.0 . . ? N2' C36' C31' 120.0 . . ? C37' N2' C36' 120.0 . . ? C37' N2' H2'A 120.0 . . ? C36' N2' H2'A 120.0 . . ? C38' C37' N2' 120.0 . . ? C38' C37' H37B 120.0 . . ? N2' C37' H37B 120.0 . . ? C37' C38' C39' 120.0 . . ? C37' C38' H38B 120.0 . . ? C39' C38' H38B 120.0 . . ? C38' C39' C35' 120.0 . . ? C38' C39' H39B 120.0 . . ? C35' C39' H39B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 178.5(2) . . . . ? C6 C1 C2 C3 -2.1(3) . . . . ? O1 C1 C2 C7 0.7(3) . . . . ? C6 C1 C2 C7 -179.9(2) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C7 C2 C3 C4 178.4(2) . . . . ? C2 C3 C4 C5 1.2(4) . . . . ? C2 C3 C4 S1 -175.80(19) . . . . ? O6 S1 C4 C3 -140.2(3) . . . . ? O4' S1 C4 C3 86.5(7) . . . . ? O5' S1 C4 C3 -49.0(5) . . . . ? O4 S1 C4 C3 98.8(4) . . . . ? O5 S1 C4 C3 -12.7(3) . . . . ? O6' S1 C4 C3 -156.0(5) . . . . ? O6 S1 C4 C5 42.7(3) . . . . ? O4' S1 C4 C5 -90.5(7) . . . . ? O5' S1 C4 C5 134.0(5) . . . . ? O4 S1 C4 C5 -78.2(4) . . . . ? O5 S1 C4 C5 170.2(3) . . . . ? O6' S1 C4 C5 27.0(5) . . . . ? C3 C4 C5 C6 -1.7(4) . . . . ? S1 C4 C5 C6 175.37(18) . . . . ? C4 C5 C6 C1 0.3(3) . . . . ? C4 C5 C6 C8 -179.4(2) . . . . ? O1 C1 C6 C5 -179.0(2) . . . . ? C2 C1 C6 C5 1.6(3) . . . . ? O1 C1 C6 C8 0.8(3) . . . . ? C2 C1 C6 C8 -178.7(2) . . . . ? C3 C2 C7 C21 115.6(2) . . . 2_666 ? C1 C2 C7 C21 -66.6(3) . . . 2_666 ? C5 C6 C8 C10 92.1(3) . . . . ? C1 C6 C8 C10 -87.6(3) . . . . ? O2 C9 C10 C11 -179.18(19) . . . . ? C14 C9 C10 C11 4.2(3) . . . . ? O2 C9 C10 C8 1.1(3) . . . . ? C14 C9 C10 C8 -175.53(19) . . . . ? C6 C8 C10 C11 -27.6(3) . . . . ? C6 C8 C10 C9 152.1(2) . . . . ? C9 C10 C11 C12 -1.4(3) . . . . ? C8 C10 C11 C12 178.30(19) . . . . ? C10 C11 C12 C13 -1.7(3) . . . . ? C10 C11 C12 S2 176.28(16) . . . . ? O8 S2 C12 C13 -144.43(18) . . . . ? O9 S2 C12 C13 94.69(19) . . . . ? O7 S2 C12 C13 -23.7(2) . . . . ? O8 S2 C12 C11 37.5(2) . . . . ? O9 S2 C12 C11 -83.38(19) . . . . ? O7 S2 C12 C11 158.22(17) . . . . ? C11 C12 C13 C14 2.2(3) . . . . ? S2 C12 C13 C14 -175.83(16) . . . . ? C12 C13 C14 C9 0.5(3) . . . . ? C12 C13 C14 C15 -175.90(19) . . . . ? O2 C9 C14 C13 179.49(18) . . . . ? C10 C9 C14 C13 -3.7(3) . . . . ? O2 C9 C14 C15 -4.2(3) . . . . ? C10 C9 C14 C15 172.61(19) . . . . ? C13 C14 C15 C17 92.0(2) . . . . ? C9 C14 C15 C17 -84.3(2) . . . . ? O3 C16 C17 C18 -179.9(2) . . . . ? C21 C16 C17 C18 2.5(3) . . . . ? O3 C16 C17 C15 3.4(3) . . . . ? C21 C16 C17 C15 -174.32(19) . . . . ? C14 C15 C17 C18 -75.7(2) . . . . ? C14 C15 C17 C16 101.1(2) . . . . ? C16 C17 C18 C19 -1.6(3) . . . . ? C15 C17 C18 C19 175.3(2) . . . . ? C17 C18 C19 C20 -0.1(3) . . . . ? C17 C18 C19 S3 179.70(17) . . . . ? O12 S3 C19 C18 116.5(2) . . . . ? O10 S3 C19 C18 -5.1(2) . . . . ? O11 S3 C19 C18 -123.5(2) . . . . ? O12 S3 C19 C20 -63.7(2) . . . . ? O10 S3 C19 C20 174.66(18) . . . . ? O11 S3 C19 C20 56.2(2) . . . . ? C18 C19 C20 C21 1.1(3) . . . . ? S3 C19 C20 C21 -178.73(17) . . . . ? C19 C20 C21 C16 -0.3(3) . . . . ? C19 C20 C21 C7 -178.0(2) . . . 2_666 ? O3 C16 C21 C20 -179.43(19) . . . . ? C17 C16 C21 C20 -1.5(3) . . . . ? O3 C16 C21 C7 -1.6(3) . . . 2_666 ? C17 C16 C21 C7 176.32(19) . . . 2_666 ? O13 C22 C23 C24 -179.0(2) . . . . ? C27 C22 C23 C24 -0.1(4) . . . . ? C22 C23 C24 C25 -0.5(4) . . . . ? C23 C24 C25 C26 0.6(4) . . . . ? C24 C25 C26 C30 179.8(2) . . . . ? C24 C25 C26 C27 -0.1(3) . . . . ? C28 N1 C27 C22 179.5(2) . . . . ? C28 N1 C27 C26 -0.8(3) . . . . ? O13 C22 C27 N1 -0.7(3) . . . . ? C23 C22 C27 N1 -179.8(2) . . . . ? O13 C22 C27 C26 179.6(2) . . . . ? C23 C22 C27 C26 0.6(3) . . . . ? C30 C26 C27 N1 -0.1(3) . . . . ? C25 C26 C27 N1 179.8(2) . . . . ? C30 C26 C27 C22 179.5(2) . . . . ? C25 C26 C27 C22 -0.5(3) . . . . ? C27 N1 C28 C29 1.1(4) . . . . ? N1 C28 C29 C30 -0.4(4) . . . . ? C28 C29 C30 C26 -0.5(4) . . . . ? C27 C26 C30 C29 0.8(3) . . . . ? C25 C26 C30 C29 -179.2(2) . . . . ? O15 C40 C41 C42 -179.4(3) . . . . ? C45 C40 C41 C42 0.6(4) . . . . ? C40 C41 C42 C43 -0.6(4) . . . . ? C41 C42 C43 C44 0.6(4) . . . . ? C42 C43 C44 C48 178.4(3) . . . . ? C42 C43 C44 C45 -0.5(4) . . . . ? C46 N3 C45 C40 178.3(3) . . . . ? C46 N3 C45 C44 -0.7(4) . . . . ? O15 C40 C45 N3 0.5(4) . . . . ? C41 C40 C45 N3 -179.6(2) . . . . ? O15 C40 C45 C44 179.5(2) . . . . ? C41 C40 C45 C44 -0.5(4) . . . . ? C48 C44 C45 N3 0.6(4) . . . . ? C43 C44 C45 N3 179.5(2) . . . . ? C48 C44 C45 C40 -178.4(2) . . . . ? C43 C44 C45 C40 0.5(4) . . . . ? C45 N3 C46 C47 0.0(4) . . . . ? N3 C46 C47 C48 0.8(4) . . . . ? C46 C47 C48 C44 -0.9(4) . . . . ? C45 C44 C48 C47 0.2(4) . . . . ? C43 C44 C48 C47 -178.7(3) . . . . ? O14 C31 C32 C33 -179.1(2) . . . . ? C36 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C33 C34 C35 C39 180.0 . . . . ? C34 C35 C36 N2 180.0 . . . . ? C39 C35 C36 N2 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C39 C35 C36 C31 180.0 . . . . ? O14 C31 C36 C35 179.2(2) . . . . ? C32 C31 C36 C35 0.0 . . . . ? O14 C31 C36 N2 -0.8(2) . . . . ? C32 C31 C36 N2 180.0 . . . . ? C35 C36 N2 C37 0.0 . . . . ? C31 C36 N2 C37 180.0 . . . . ? C36 N2 C37 C38 0.0 . . . . ? N2 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C35 0.0 . . . . ? C36 C35 C39 C38 0.0 . . . . ? C34 C35 C39 C38 180.0 . . . . ? O14' C31' C32' C33' -177.1(5) . . . . ? C36' C31' C32' C33' 0.0 . . . . ? C31' C32' C33' C34' 0.0 . . . . ? C32' C33' C34' C35' 0.0 . . . . ? C33' C34' C35' C36' 0.0 . . . . ? C33' C34' C35' C39' 180.0 . . . . ? C34' C35' C36' N2' 180.0 . . . . ? C39' C35' C36' N2' 0.0 . . . . ? C34' C35' C36' C31' 0.0 . . . . ? C39' C35' C36' C31' 180.0 . . . . ? O14' C31' C36' C35' 177.4(4) . . . . ? C32' C31' C36' C35' 0.0 . . . . ? O14' C31' C36' N2' -2.6(4) . . . . ? C32' C31' C36' N2' 180.0 . . . . ? C35' C36' N2' C37' 0.0 . . . . ? C31' C36' N2' C37' 180.0 . . . . ? C36' N2' C37' C38' 0.0 . . . . ? N2' C37' C38' C39' 0.0 . . . . ? C37' C38' C39' C35' 0.0 . . . . ? C34' C35' C39' C38' 180.0 . . . . ? C36' C35' C39' C38' 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.962 _refine_diff_density_min -1.060 _refine_diff_density_rms 0.071 # Attachment 'complex_1.cif' data_shelxl1 _database_code_depnum_ccdc_archive 'CCDC 666758' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H63 N3 O25 S4' _chemical_formula_weight 1294.32 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9696(16) _cell_length_b 23.274(3) _cell_length_c 20.884(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.405(2) _cell_angle_gamma 90.00 _cell_volume 6132.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 7991 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 26.10 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 0.239 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.737134 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 30840 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10805 _reflns_number_gt 6543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1475P)^2^+6.4622P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10805 _refine_ls_number_parameters 980 _refine_ls_number_restraints 234 _refine_ls_R_factor_all 0.1223 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2642 _refine_ls_wR_factor_gt 0.2049 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.081 _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 S1 S 1.04145(10) 0.26821(5) 1.11763(6) 0.0420(3) Uani 1 1 d . . . S2 S 0.80598(14) -0.01083(6) 0.90489(8) 0.0662(5) Uani 1 1 d D . . S3 S 0.46351(12) 0.22548(8) 0.79967(8) 0.0678(5) Uani 1 1 d D . . S4 S 0.77990(12) 0.50934(6) 0.92538(7) 0.0587(4) Uani 1 1 d D . . O1 O 1.1360(3) 0.25002(13) 0.85576(16) 0.0432(8) Uani 1 1 d . . . H1 H 1.1392 0.2815 0.8387 0.065 Uiso 1 1 calc R . . O2 O 0.9790(3) 0.18636(14) 0.78474(16) 0.0485(8) Uani 1 1 d . A . H2 H 1.0363 0.1976 0.8066 0.073 Uiso 1 1 calc R . . O3 O 0.8378(3) 0.26798(13) 0.69061(15) 0.0424(8) Uani 1 1 d . A . H3 H 0.8603 0.2384 0.6773 0.064 Uiso 1 1 calc R . . O4 O 0.9640(3) 0.32851(14) 0.78702(16) 0.0475(8) Uani 1 1 d . A . H4 H 0.9225 0.3168 0.7538 0.071 Uiso 1 1 calc R . . O5 O 1.1273(3) 0.30595(16) 1.15022(17) 0.0576(10) Uani 1 1 d . . . O6 O 1.0506(3) 0.21072(15) 1.14608(17) 0.0567(9) Uani 1 1 d . . . O7 O 0.9379(3) 0.29399(15) 1.11418(17) 0.0542(9) Uani 1 1 d . . . O8 O 0.8921(7) -0.0457(4) 0.9398(5) 0.076(3) Uani 0.50 1 d PU A 1 O9 O 0.7358(10) 0.0118(5) 0.9437(6) 0.096(3) Uani 0.50 1 d PU A 1 O10 O 0.7367(9) -0.0418(4) 0.8490(4) 0.079(3) Uani 0.50 1 d PU A 1 O8' O 0.8545(13) -0.0600(4) 0.8844(9) 0.136(4) Uani 0.50 1 d PDU A 2 O9' O 0.8274(11) -0.0023(5) 0.9752(5) 0.105(3) Uani 0.50 1 d PU A 2 O10' O 0.6952(7) -0.0093(7) 0.8776(8) 0.137(5) Uani 0.50 1 d PDU A 2 O11 O 0.4974(8) 0.1985(5) 0.8635(5) 0.068(3) Uani 0.50 1 d PU B 1 O12 O 0.3987(7) 0.1878(5) 0.7505(5) 0.076(3) Uani 0.50 1 d PU B 1 O13 O 0.4248(16) 0.2795(8) 0.8140(10) 0.131(7) Uani 0.50 1 d PU B 1 O11' O 0.4306(15) 0.1682(8) 0.7825(10) 0.153(6) Uani 0.50 1 d PU B 2 O12' O 0.3985(9) 0.2758(6) 0.7827(8) 0.094(4) Uani 0.50 1 d PDU B 2 O13' O 0.4936(15) 0.2323(9) 0.8692(5) 0.145(6) Uani 0.50 1 d PDU B 2 O14 O 0.7270(9) 0.4806(5) 0.9698(6) 0.089(3) Uani 0.50 1 d PDU C 1 O15 O 0.6733(9) 0.5248(5) 0.8860(5) 0.110(4) Uani 0.50 1 d PDU C 1 O16 O 0.8478(11) 0.5576(5) 0.9334(7) 0.097(5) Uani 0.50 1 d PDU C 1 O14' O 0.7855(13) 0.4872(7) 0.9913(5) 0.118(5) Uani 0.50 1 d PDU C 2 O15' O 0.7271(9) 0.5485(4) 0.8725(5) 0.077(3) Uani 0.50 1 d PU C 2 O16' O 0.8706(10) 0.5426(5) 0.9609(6) 0.079(4) Uani 0.50 1 d PU C 2 C1 C 1.0872(3) 0.36777(18) 0.9032(2) 0.0366(10) Uani 1 1 d . . . H1A H 1.1277 0.3955 0.9336 0.044 Uiso 1 1 calc R . . H1B H 1.1226 0.3624 0.8675 0.044 Uiso 1 1 calc R . . C2 C 1.0845(3) 0.31096(18) 0.9387(2) 0.0335(9) Uani 1 1 d . . . C3 C 1.0620(3) 0.31195(18) 1.0005(2) 0.0362(10) Uani 1 1 d . . . H3A H 1.0503 0.3471 1.0189 0.043 Uiso 1 1 calc R . . C4 C 1.0567(4) 0.26165(18) 1.0357(2) 0.0361(10) Uani 1 1 d . . . C5 C 1.0683(3) 0.20858(18) 1.0079(2) 0.0364(10) Uani 1 1 d . . . H5A H 1.0615 0.1751 1.0308 0.044 Uiso 1 1 calc R . . C6 C 1.0901(3) 0.20532(18) 0.9459(2) 0.0346(9) Uani 1 1 d . . . C7 C 1.1029(3) 0.25691(18) 0.9134(2) 0.0335(9) Uani 1 1 d . . . C8 C 1.1029(4) 0.14666(18) 0.9156(2) 0.0407(11) Uani 1 1 d . . . H8A H 1.1501 0.1506 0.8861 0.049 Uiso 1 1 calc R . . H8B H 1.1359 0.1205 0.9505 0.049 Uiso 1 1 calc R . . C9 C 0.9991(4) 0.12059(18) 0.8779(2) 0.0382(10) Uani 1 1 d . A . C10 C 0.9556(4) 0.07350(19) 0.9042(2) 0.0455(12) Uani 1 1 d . . . H10A H 0.9911 0.0582 0.9445 0.055 Uiso 1 1 calc R A . C11 C 0.8606(4) 0.04939(19) 0.8711(2) 0.0455(12) Uani 1 1 d . A . C12 C 0.8060(4) 0.07201(19) 0.8109(2) 0.0450(11) Uani 1 1 d . . . H12A H 0.7418 0.0559 0.7893 0.054 Uiso 1 1 calc R A . C13 C 0.8469(4) 0.11837(17) 0.7830(2) 0.0385(10) Uani 1 1 d . A . C14 C 0.9439(4) 0.14172(18) 0.8164(2) 0.0386(10) Uani 1 1 d . . . C15 C 0.7871(4) 0.14512(18) 0.7187(2) 0.0401(11) Uani 1 1 d . . . H15A H 0.7373 0.1174 0.6942 0.048 Uiso 1 1 calc R A . H15B H 0.8367 0.1552 0.6922 0.048 Uiso 1 1 calc R . . C16 C 0.7269(4) 0.19894(19) 0.7315(2) 0.0378(10) Uani 1 1 d . A . C17 C 0.6368(4) 0.1915(2) 0.7565(2) 0.0448(11) Uani 1 1 d . . . H17A H 0.6151 0.1545 0.7641 0.054 Uiso 1 1 calc R A . C18 C 0.5788(4) 0.2383(2) 0.7704(2) 0.0474(12) Uani 1 1 d . A . C19 C 0.6120(4) 0.2942(2) 0.7606(2) 0.0450(11) Uani 1 1 d . . . H19A H 0.5739 0.3255 0.7704 0.054 Uiso 1 1 calc R A . C20 C 0.7017(4) 0.30288(19) 0.7363(2) 0.0390(10) Uani 1 1 d . A . C21 C 0.7559(4) 0.25485(19) 0.7191(2) 0.0364(10) Uani 1 1 d . . . C22 C 0.7415(4) 0.36366(19) 0.7277(2) 0.0440(11) Uani 1 1 d . . . H22A H 0.7818 0.3630 0.6939 0.053 Uiso 1 1 calc R A . H22B H 0.6810 0.3887 0.7126 0.053 Uiso 1 1 calc R . . C23 C 0.8105(4) 0.38823(18) 0.7904(2) 0.0382(10) Uani 1 1 d . A . C24 C 0.7718(4) 0.43145(19) 0.8251(2) 0.0432(11) Uani 1 1 d . . . H24A H 0.7035 0.4453 0.8086 0.052 Uiso 1 1 calc R A . C25 C 0.8321(4) 0.45439(19) 0.8833(2) 0.0426(11) Uani 1 1 d . A . C26 C 0.9346(4) 0.43391(18) 0.9086(2) 0.0399(11) Uani 1 1 d . . . H26A H 0.9751 0.4490 0.9476 0.048 Uiso 1 1 calc R A . C27 C 0.9766(3) 0.39105(17) 0.8757(2) 0.0350(10) Uani 1 1 d . A . C28 C 0.9154(4) 0.36909(17) 0.8167(2) 0.0352(10) Uani 1 1 d . . . N2 N 0.3830(4) 0.2232(3) 0.4523(3) 0.0826(16) Uani 1 1 d . . . H2A H 0.4007 0.2389 0.4191 0.099 Uiso 1 1 calc R . . C38 C 0.3381(5) 0.2323(3) 0.5565(3) 0.0689(17) Uani 1 1 d . . . C39 C 0.3220(6) 0.2666(4) 0.6074(4) 0.092(2) Uani 1 1 d . . . H39A H 0.3046 0.2502 0.6441 0.110 Uiso 1 1 calc R . . C40 C 0.3317(6) 0.3234(5) 0.6033(5) 0.105(3) Uani 1 1 d . . . H40A H 0.3214 0.3456 0.6383 0.126 Uiso 1 1 calc R . . C41 C 0.3562(6) 0.3512(4) 0.5502(6) 0.109(3) Uani 1 1 d . . . H41A H 0.3611 0.3911 0.5495 0.130 Uiso 1 1 calc R . . C42 C 0.3736(6) 0.3179(3) 0.4970(4) 0.086(2) Uani 1 1 d . . . H42A H 0.3906 0.3348 0.4604 0.103 Uiso 1 1 calc R . . C43 C 0.3640(4) 0.2582(2) 0.5023(3) 0.0567(14) Uani 1 1 d . . . C44 C 0.3750(6) 0.1663(4) 0.4537(5) 0.099(3) Uani 1 1 d . . . H44A H 0.3871 0.1439 0.4193 0.119 Uiso 1 1 calc R . . C45 C 0.3477(6) 0.1409(3) 0.5085(6) 0.103(3) Uani 1 1 d . . . H45A H 0.3431 0.1011 0.5103 0.124 Uiso 1 1 calc R . . C46 C 0.3282(5) 0.1715(3) 0.5575(5) 0.090(2) Uani 1 1 d . . . H46A H 0.3081 0.1534 0.5924 0.108 Uiso 1 1 calc R . . N3 N 0.2582(4) 0.6950(2) 0.5240(2) 0.0617(12) Uani 1 1 d . . . H3B H 0.2677 0.6614 0.5093 0.074 Uiso 1 1 calc R . . C47 C 0.2976(4) 0.7418(2) 0.4968(2) 0.0513(13) Uani 1 1 d . . . C48 C 0.3545(5) 0.7345(3) 0.4478(3) 0.0708(17) Uani 1 1 d . . . H48A H 0.3668 0.6980 0.4331 0.085 Uiso 1 1 calc R . . C49 C 0.3907(5) 0.7812(5) 0.4226(3) 0.086(2) Uani 1 1 d . . . H49A H 0.4292 0.7768 0.3905 0.103 Uiso 1 1 calc R . . C50 C 0.3718(6) 0.8364(4) 0.4437(4) 0.097(3) Uani 1 1 d . . . H50A H 0.3972 0.8681 0.4250 0.117 Uiso 1 1 calc R . . C51 C 0.3164(6) 0.8445(3) 0.4916(4) 0.086(2) Uani 1 1 d . . . H51A H 0.3044 0.8815 0.5051 0.103 Uiso 1 1 calc R . . C52 C 0.2776(4) 0.7964(2) 0.5203(3) 0.0560(13) Uani 1 1 d . . . C53 C 0.2206(5) 0.7993(3) 0.5702(3) 0.0657(16) Uani 1 1 d . . . H53A H 0.2057 0.8351 0.5857 0.079 Uiso 1 1 calc R . . C54 C 0.1871(5) 0.7512(3) 0.5961(3) 0.0637(16) Uani 1 1 d . . . H54A H 0.1515 0.7537 0.6299 0.076 Uiso 1 1 calc R . . C55 C 0.2069(5) 0.6991(3) 0.5713(3) 0.0632(15) Uani 1 1 d . . . H55A H 0.1836 0.6659 0.5881 0.076 Uiso 1 1 calc R . . C29 C 0.9288(11) 0.5223(5) 0.7375(5) 0.093(11) Uani 0.50 1 d PGD D 1 C30 C 1.0225(11) 0.4953(4) 0.7687(7) 0.107(12) Uani 0.50 1 d PG D 1 H30A H 1.0459 0.4632 0.7496 0.129 Uiso 0.50 1 calc PR D 1 C31 C 1.0811(8) 0.5161(5) 0.8285(7) 0.104(7) Uani 0.50 1 d PG D 1 H31A H 1.1439 0.4980 0.8494 0.125 Uiso 0.50 1 calc PR D 1 C32 C 1.0461(10) 0.5640(5) 0.8571(5) 0.106(19) Uani 0.50 1 d PG D 1 H32A H 1.0853 0.5780 0.8971 0.128 Uiso 0.50 1 calc PR D 1 C33 C 0.9523(10) 0.5911(4) 0.8258(6) 0.049(3) Uani 0.50 1 d PG D 1 H33A H 0.9289 0.6232 0.8450 0.058 Uiso 0.50 1 calc PR D 1 C34 C 0.8937(8) 0.5703(5) 0.7661(6) 0.071(6) Uani 0.50 1 d PGD D 1 N1 N 0.7987(17) 0.5952(13) 0.7371(13) 0.173(15) Uani 0.50 1 d PD D 1 H1C H 0.7776 0.6240 0.7565 0.207 Uiso 0.50 1 calc PR D 1 C35 C 0.7348(15) 0.5767(7) 0.6781(8) 0.090(5) Uani 0.50 1 d PD D 1 H35A H 0.6708 0.5946 0.6595 0.107 Uiso 0.50 1 calc PR D 1 C36 C 0.7707(14) 0.5302(7) 0.6484(10) 0.116(8) Uani 0.50 1 d PD D 1 H36A H 0.7298 0.5157 0.6091 0.139 Uiso 0.50 1 calc PR D 1 C37 C 0.8674(19) 0.5051(11) 0.6769(9) 0.108(12) Uani 0.50 1 d PD D 1 H37A H 0.8922 0.4756 0.6545 0.129 Uiso 0.50 1 calc PR D 1 C29' C 0.9696(7) 0.5546(4) 0.8019(5) 0.068(4) Uani 0.50 1 d PGD E 2 C30' C 1.0517(9) 0.5617(4) 0.8574(5) 0.075(12) Uani 0.50 1 d PGU E 2 H30B H 1.0481 0.5906 0.8875 0.089 Uiso 0.50 1 calc PR E 2 C31' C 1.1393(8) 0.5255(5) 0.8679(5) 0.088(5) Uani 0.50 1 d PG E 2 H31B H 1.1942 0.5302 0.9051 0.105 Uiso 0.50 1 calc PR E 2 C32' C 1.1447(7) 0.4822(4) 0.8230(6) 0.095(5) Uani 0.50 1 d PG E 2 H32B H 1.2033 0.4580 0.8300 0.114 Uiso 0.50 1 calc PR E 2 C33' C 1.0626(10) 0.4751(4) 0.7675(5) 0.081(5) Uani 0.50 1 d PG E 2 H33B H 1.0663 0.4462 0.7374 0.097 Uiso 0.50 1 calc PR E 2 C34' C 0.9751(8) 0.5113(4) 0.7569(4) 0.052(6) Uani 0.50 1 d PGD E 2 C35' C 0.8851(14) 0.5068(12) 0.7058(10) 0.094(9) Uani 0.50 1 d PD E 2 H35B H 0.8807 0.4758 0.6772 0.113 Uiso 0.50 1 calc PR E 2 C36' C 0.8015(15) 0.5456(6) 0.6945(8) 0.088(5) Uani 0.50 1 d PD E 2 H36B H 0.7455 0.5416 0.6578 0.105 Uiso 0.50 1 calc PR E 2 C37' C 0.8021(14) 0.5908(8) 0.7389(9) 0.054(5) Uani 0.50 1 d PDU E 2 H37B H 0.7482 0.6180 0.7331 0.064 Uiso 0.50 1 calc PR E 2 N1' N 0.8883(8) 0.5918(5) 0.7918(7) 0.073(4) Uani 0.50 1 d PD E 2 H1'A H 0.8902 0.6184 0.8206 0.087 Uiso 0.50 1 calc PR E 2 O19 O 0.7605(5) 0.0900(2) 0.0402(3) 0.1063(17) Uani 1 1 d . . . O20 O 0.9568(5) 0.1067(2) 0.1128(3) 0.1168(19) Uani 1 1 d . . . O21 O 0.5728(8) 0.4371(6) 0.5749(6) 0.116(4) Uani 0.50 1 d P . . O22 O 0.6052(8) 0.0173(4) 0.6614(4) 0.187(3) Uani 1 1 d . . . O23 O 0.4870(8) 0.9675(6) 0.8148(7) 0.132(5) Uani 0.50 1 d P . . O24 O 0.2007(3) 0.31744(18) 0.76626(19) 0.0677(11) Uani 1 1 d . . . O25 O 0.5483(5) 0.5654(4) 0.7781(5) 0.170(3) Uani 1 1 d . . . O26 O 0.5225(10) 0.4797(6) 0.9516(9) 0.176(6) Uani 0.60 1 d P F 1 O26' O 0.408(2) 0.5064(10) 0.9648(10) 0.192(10) Uani 0.40 1 d P G 2 O27 O 0.5628(11) 0.0956(5) 0.9105(7) 0.140(5) Uani 0.50 1 d P . . O28 O 0.2626(13) 0.4286(6) 0.7688(7) 0.137(5) Uani 0.50 1 d PU H 1 O28' O 0.3563(17) 0.4174(8) 0.7592(9) 0.176(6) Uani 0.50 1 d PU I 2 O29 O 0.4755(18) 0.0403(10) 0.9730(12) 0.110(7) Uani 0.25 1 d PU . . O29' O 0.506(3) 0.0999(13) 0.353(2) 0.193(16) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0518(7) 0.0441(6) 0.0344(6) 0.0012(5) 0.0191(5) 0.0020(5) S2 0.0866(12) 0.0501(8) 0.0597(9) 0.0085(7) 0.0128(8) -0.0182(8) S3 0.0497(9) 0.0927(12) 0.0682(10) -0.0052(9) 0.0285(8) -0.0047(8) S4 0.0709(10) 0.0459(7) 0.0599(9) -0.0138(6) 0.0166(7) 0.0142(7) O1 0.053(2) 0.0429(18) 0.0390(18) -0.0013(14) 0.0223(16) 0.0010(15) O2 0.058(2) 0.0462(19) 0.0408(19) 0.0042(15) 0.0097(16) -0.0080(16) O3 0.052(2) 0.0396(17) 0.0404(18) -0.0036(14) 0.0215(16) 0.0000(15) O4 0.048(2) 0.0497(19) 0.0442(19) -0.0154(15) 0.0104(16) 0.0064(16) O5 0.063(2) 0.067(2) 0.045(2) -0.0196(17) 0.0163(18) -0.0107(18) O6 0.081(3) 0.050(2) 0.0423(19) 0.0129(16) 0.0202(19) 0.0091(18) O7 0.056(2) 0.066(2) 0.051(2) 0.0100(17) 0.0319(18) 0.0129(18) O8 0.083(5) 0.056(4) 0.072(5) 0.042(4) -0.014(4) -0.014(4) O9 0.105(7) 0.097(6) 0.107(7) -0.003(5) 0.063(6) -0.026(5) O10 0.108(6) 0.055(5) 0.064(5) 0.005(4) 0.000(5) -0.042(4) O8' 0.169(9) 0.083(6) 0.174(9) 0.000(7) 0.078(8) 0.000(6) O9' 0.135(8) 0.097(6) 0.081(6) 0.024(5) 0.021(6) -0.027(6) O10' 0.110(8) 0.147(9) 0.149(9) 0.052(7) 0.018(7) -0.039(7) O11 0.065(5) 0.091(6) 0.058(5) 0.015(4) 0.034(4) -0.003(5) O12 0.043(5) 0.120(7) 0.064(5) 0.003(5) 0.008(4) -0.033(5) O13 0.117(10) 0.136(9) 0.155(11) -0.021(8) 0.060(8) 0.004(7) O11' 0.145(10) 0.137(9) 0.203(11) -0.022(8) 0.091(8) -0.042(7) O12' 0.040(5) 0.141(8) 0.111(8) 0.042(7) 0.036(5) 0.033(5) O13' 0.127(9) 0.202(11) 0.117(9) -0.009(8) 0.051(7) -0.012(9) O14 0.099(7) 0.070(5) 0.129(8) -0.015(5) 0.094(6) 0.001(5) O15 0.080(6) 0.123(8) 0.119(7) -0.062(6) 0.005(6) 0.048(6) O16 0.128(9) 0.062(6) 0.113(9) -0.021(6) 0.056(7) -0.016(6) O14' 0.143(9) 0.116(8) 0.115(8) -0.011(6) 0.068(7) 0.007(7) O15' 0.085(6) 0.066(5) 0.084(6) 0.010(4) 0.025(5) 0.035(5) O16' 0.077(6) 0.064(6) 0.082(7) -0.042(5) -0.009(5) 0.013(5) C1 0.042(3) 0.031(2) 0.038(2) -0.0011(18) 0.013(2) -0.0045(18) C2 0.033(2) 0.034(2) 0.034(2) 0.0003(17) 0.0088(19) -0.0052(17) C3 0.041(3) 0.036(2) 0.034(2) -0.0061(18) 0.012(2) -0.0005(19) C4 0.038(2) 0.036(2) 0.036(2) -0.0009(18) 0.012(2) -0.0008(18) C5 0.040(3) 0.034(2) 0.037(2) 0.0019(18) 0.011(2) -0.0005(18) C6 0.037(2) 0.033(2) 0.034(2) 0.0009(18) 0.0080(19) 0.0035(18) C7 0.031(2) 0.040(2) 0.030(2) 0.0008(18) 0.0070(18) 0.0010(18) C8 0.050(3) 0.033(2) 0.040(2) -0.0008(19) 0.011(2) 0.009(2) C9 0.049(3) 0.029(2) 0.038(2) -0.0033(18) 0.012(2) 0.0057(19) C10 0.062(3) 0.035(2) 0.038(3) 0.001(2) 0.010(2) 0.007(2) C11 0.058(3) 0.035(2) 0.044(3) 0.000(2) 0.013(2) -0.003(2) C12 0.055(3) 0.036(2) 0.044(3) -0.006(2) 0.013(2) -0.002(2) C13 0.053(3) 0.027(2) 0.036(2) -0.0031(18) 0.012(2) 0.0021(19) C14 0.052(3) 0.030(2) 0.036(2) -0.0038(18) 0.015(2) 0.003(2) C15 0.052(3) 0.036(2) 0.031(2) -0.0067(18) 0.008(2) -0.001(2) C16 0.043(3) 0.042(2) 0.027(2) -0.0015(18) 0.005(2) 0.002(2) C17 0.048(3) 0.048(3) 0.037(3) 0.001(2) 0.008(2) -0.002(2) C18 0.040(3) 0.063(3) 0.039(3) -0.001(2) 0.008(2) 0.000(2) C19 0.046(3) 0.051(3) 0.037(3) -0.004(2) 0.007(2) 0.009(2) C20 0.043(3) 0.043(2) 0.029(2) -0.0036(19) 0.005(2) 0.004(2) C21 0.042(3) 0.045(3) 0.022(2) -0.0036(18) 0.0052(19) -0.0004(19) C22 0.050(3) 0.042(3) 0.038(3) 0.002(2) 0.006(2) 0.009(2) C23 0.047(3) 0.030(2) 0.039(2) 0.0003(18) 0.011(2) 0.0016(19) C24 0.047(3) 0.034(2) 0.049(3) 0.004(2) 0.014(2) 0.009(2) C25 0.055(3) 0.032(2) 0.041(3) -0.0030(19) 0.013(2) 0.004(2) C26 0.054(3) 0.030(2) 0.038(2) -0.0007(19) 0.014(2) -0.003(2) C27 0.044(3) 0.026(2) 0.037(2) 0.0021(17) 0.014(2) -0.0032(18) C28 0.044(3) 0.028(2) 0.036(2) 0.0014(18) 0.015(2) 0.0019(18) N2 0.069(4) 0.104(5) 0.071(4) -0.001(3) 0.009(3) 0.010(3) C38 0.042(3) 0.090(5) 0.075(4) 0.013(4) 0.014(3) 0.001(3) C39 0.067(5) 0.134(7) 0.077(5) -0.004(5) 0.021(4) -0.003(5) C40 0.082(6) 0.125(8) 0.108(7) -0.041(6) 0.022(5) -0.010(5) C41 0.077(5) 0.068(5) 0.176(10) -0.008(6) 0.019(6) 0.006(4) C42 0.073(5) 0.071(4) 0.111(6) 0.018(4) 0.018(4) 0.001(4) C43 0.048(3) 0.066(4) 0.055(3) 0.002(3) 0.010(3) 0.004(3) C44 0.074(5) 0.088(6) 0.129(7) -0.035(5) 0.013(5) 0.008(4) C45 0.060(5) 0.070(5) 0.180(10) 0.011(6) 0.029(5) -0.002(4) C46 0.057(4) 0.084(5) 0.135(7) 0.023(5) 0.033(5) -0.005(4) N3 0.070(3) 0.055(3) 0.064(3) -0.011(2) 0.024(3) -0.004(2) C47 0.042(3) 0.070(4) 0.039(3) -0.003(2) 0.002(2) -0.001(2) C48 0.055(4) 0.112(5) 0.044(3) -0.006(3) 0.009(3) 0.001(3) C49 0.051(4) 0.158(8) 0.045(4) 0.016(5) 0.004(3) -0.012(5) C50 0.066(5) 0.139(8) 0.077(5) 0.049(5) -0.004(4) -0.028(5) C51 0.081(5) 0.076(4) 0.090(5) 0.021(4) -0.001(4) -0.005(4) C52 0.055(3) 0.059(3) 0.048(3) 0.002(3) -0.001(3) -0.001(3) C53 0.068(4) 0.067(4) 0.062(4) -0.015(3) 0.013(3) 0.010(3) C54 0.059(4) 0.085(4) 0.051(3) -0.006(3) 0.019(3) 0.001(3) C55 0.059(4) 0.068(4) 0.066(4) 0.004(3) 0.022(3) -0.011(3) C29 0.08(2) 0.049(10) 0.17(3) -0.022(14) 0.068(18) -0.028(12) C30 0.13(2) 0.036(11) 0.20(3) 0.010(12) 0.13(2) 0.008(12) C31 0.107(17) 0.062(11) 0.17(2) 0.037(13) 0.083(17) 0.005(11) C32 0.18(4) 0.059(15) 0.12(3) -0.018(14) 0.11(3) -0.058(17) C33 0.050(8) 0.035(6) 0.068(9) -0.008(6) 0.030(6) 0.005(6) C34 0.106(15) 0.039(8) 0.097(13) -0.011(8) 0.079(13) -0.011(8) N1 0.22(3) 0.15(2) 0.20(3) -0.057(18) 0.16(2) -0.088(18) C35 0.108(14) 0.088(12) 0.083(11) -0.034(9) 0.044(10) -0.036(9) C36 0.152(18) 0.116(15) 0.103(14) -0.056(12) 0.075(15) -0.090(14) C37 0.18(3) 0.049(13) 0.14(2) -0.046(16) 0.11(2) -0.044(14) C29' 0.080(10) 0.060(8) 0.073(9) 0.020(7) 0.038(8) -0.014(7) C30' 0.080(13) 0.070(14) 0.072(14) 0.015(9) 0.016(9) -0.006(9) C31' 0.100(14) 0.078(11) 0.094(13) 0.008(10) 0.039(10) -0.017(10) C32' 0.081(11) 0.083(11) 0.131(15) 0.048(11) 0.045(11) -0.002(9) C33' 0.108(14) 0.058(10) 0.097(12) 0.011(9) 0.066(11) -0.004(9) C34' 0.078(16) 0.044(10) 0.050(8) -0.009(7) 0.046(9) -0.004(10) C35' 0.111(19) 0.08(2) 0.11(2) 0.035(17) 0.067(17) -0.013(17) C36' 0.116(16) 0.074(11) 0.076(11) -0.006(10) 0.028(11) -0.021(11) C37' 0.054(5) 0.054(5) 0.053(5) -0.0003(11) 0.0126(15) -0.0004(11) N1' 0.084(11) 0.056(8) 0.094(12) -0.005(8) 0.053(9) -0.009(7) O19 0.141(5) 0.083(3) 0.094(4) 0.021(3) 0.027(3) 0.006(3) O20 0.134(5) 0.086(4) 0.130(5) 0.021(3) 0.030(4) -0.029(3) O21 0.067(6) 0.163(11) 0.122(9) 0.020(8) 0.027(6) -0.002(7) O22 0.192(8) 0.227(10) 0.142(6) -0.013(6) 0.039(6) -0.008(7) O23 0.066(7) 0.171(12) 0.163(12) 0.066(10) 0.034(7) -0.004(7) O24 0.067(3) 0.081(3) 0.056(2) 0.007(2) 0.015(2) -0.003(2) O25 0.106(5) 0.179(7) 0.213(8) 0.071(6) 0.010(5) 0.018(5) O26 0.124(10) 0.178(12) 0.245(18) 0.039(12) 0.084(11) 0.003(9) O26' 0.26(3) 0.24(2) 0.124(15) 0.041(15) 0.138(17) 0.064(19) O27 0.151(11) 0.100(9) 0.153(11) 0.039(8) 0.003(9) 0.015(8) O28 0.156(9) 0.110(7) 0.140(8) 0.005(7) 0.023(7) 0.001(7) O28' 0.199(10) 0.156(9) 0.176(10) -0.007(8) 0.048(9) -0.015(8) O29 0.107(10) 0.112(10) 0.110(10) -0.007(8) 0.026(8) -0.008(8) O29' 0.16(3) 0.12(2) 0.31(5) 0.03(3) 0.08(3) 0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O5 1.457(4) . ? S1 O7 1.457(4) . ? S1 O6 1.458(3) . ? S1 C4 1.773(4) . ? S2 O10' 1.417(9) . ? S2 O8' 1.418(8) . ? S2 O8 1.435(8) . ? S2 O9' 1.444(11) . ? S2 O9 1.451(10) . ? S2 O10 1.485(8) . ? S2 C11 1.787(5) . ? S3 O13 1.411(18) . ? S3 O11' 1.419(17) . ? S3 O13' 1.423(9) . ? S3 O12' 1.438(9) . ? S3 O11 1.447(9) . ? S3 O12 1.460(10) . ? S3 C18 1.767(5) . ? S4 O16 1.413(9) . ? S4 O14 1.440(7) . ? S4 O14' 1.456(9) . ? S4 O16' 1.458(11) . ? S4 O15' 1.473(9) . ? S4 O15 1.480(10) . ? S4 C25 1.772(5) . ? O1 C7 1.378(5) . ? O1 H1 0.8200 . ? O2 C14 1.365(5) . ? O2 H2 0.8200 . ? O3 C21 1.368(5) . ? O3 H3 0.8200 . ? O4 C28 1.362(5) . ? O4 H4 0.8200 . ? C1 C27 1.516(6) . ? C1 C2 1.520(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.389(6) . ? C2 C7 1.406(6) . ? C3 C4 1.393(6) . ? C3 H3A 0.9300 . ? C4 C5 1.388(6) . ? C5 C6 1.391(6) . ? C5 H5A 0.9300 . ? C6 C7 1.408(6) . ? C6 C8 1.529(6) . ? C8 C9 1.520(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.402(6) . ? C9 C14 1.406(6) . ? C10 C11 1.385(7) . ? C10 H10A 0.9300 . ? C11 C12 1.395(7) . ? C12 C13 1.389(6) . ? C12 H12A 0.9300 . ? C13 C14 1.400(6) . ? C13 C15 1.520(6) . ? C15 C16 1.531(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.395(6) . ? C16 C17 1.398(7) . ? C17 C18 1.392(7) . ? C17 H17A 0.9300 . ? C18 C19 1.400(7) . ? C19 C20 1.388(7) . ? C19 H19A 0.9300 . ? C20 C21 1.410(6) . ? C20 C22 1.530(6) . ? C22 C23 1.517(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.399(6) . ? C23 C28 1.415(6) . ? C24 C25 1.391(7) . ? C24 H24A 0.9300 . ? C25 C26 1.396(7) . ? C26 C27 1.391(6) . ? C26 H26A 0.9300 . ? C27 C28 1.399(6) . ? N2 C44 1.328(10) . ? N2 C43 1.392(8) . ? N2 H2A 0.8600 . ? C38 C39 1.383(10) . ? C38 C43 1.391(8) . ? C38 C46 1.423(10) . ? C39 C40 1.331(12) . ? C39 H39A 0.9300 . ? C40 C41 1.384(13) . ? C40 H40A 0.9300 . ? C41 C42 1.417(12) . ? C41 H41A 0.9300 . ? C42 C43 1.401(9) . ? C42 H42A 0.9300 . ? C44 C45 1.405(12) . ? C44 H44A 0.9300 . ? C45 C46 1.317(12) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? N3 C55 1.315(7) . ? N3 C47 1.381(7) . ? N3 H3B 0.8600 . ? C47 C48 1.406(8) . ? C47 C52 1.407(8) . ? C48 C49 1.337(10) . ? C48 H48A 0.9300 . ? C49 C50 1.400(11) . ? C49 H49A 0.9300 . ? C50 C51 1.372(11) . ? C50 H50A 0.9300 . ? C51 C52 1.418(9) . ? C51 H51A 0.9300 . ? C52 C53 1.411(8) . ? C53 C54 1.358(8) . ? C53 H53A 0.9300 . ? C54 C55 1.367(8) . ? C54 H54A 0.9300 . ? C55 H55A 0.9300 . ? C29 C37 1.390(10) . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C30 H30A 0.9300 . ? C31 C32 1.3900 . ? C31 H31A 0.9300 . ? C32 C33 1.3900 . ? C32 H32A 0.9300 . ? C33 C34 1.3900 . ? C33 H33A 0.9300 . ? C34 N1 1.370(10) . ? N1 C35 1.384(10) . ? N1 H1C 0.8600 . ? C35 C36 1.381(10) . ? C35 H35A 0.9300 . ? C36 C37 1.386(10) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C29' N1' 1.342(8) . ? C29' C30' 1.3900 . ? C29' C34' 1.3900 . ? C30' C31' 1.3900 . ? C30' H30B 0.9300 . ? C31' C32' 1.3900 . ? C31' H31B 0.9300 . ? C32' C33' 1.3900 . ? C32' H32B 0.9300 . ? C33' C34' 1.3900 . ? C33' H33B 0.9300 . ? C34' C35' 1.391(10) . ? C35' C36' 1.389(10) . ? C35' H35B 0.9300 . ? C36' C37' 1.400(10) . ? C36' H36B 0.9300 . ? C37' N1' 1.379(10) . ? C37' H37B 0.9300 . ? N1' H1'A 0.8600 . ? 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 O5 S1 O7 111.7(2) . . ? O5 S1 O6 112.5(2) . . ? O7 S1 O6 112.6(2) . . ? O5 S1 C4 105.0(2) . . ? O7 S1 C4 107.2(2) . . ? O6 S1 C4 107.3(2) . . ? O10' S2 O8' 112.2(11) . . ? O10' S2 O8 144.6(7) . . ? O8' S2 O8 49.4(7) . . ? O10' S2 O9' 110.1(10) . . ? O8' S2 O9' 115.0(9) . . ? O8 S2 O9' 67.5(7) . . ? O10' S2 O9 60.5(9) . . ? O8' S2 O9 147.3(7) . . ? O8 S2 O9 115.9(7) . . ? O9' S2 O9 51.7(6) . . ? O10' S2 O10 47.5(8) . . ? O8' S2 O10 66.5(8) . . ? O8 S2 O10 112.5(6) . . ? O9' S2 O10 143.7(6) . . ? O9 S2 O10 105.8(7) . . ? O10' S2 C11 106.2(6) . . ? O8' S2 C11 105.6(6) . . ? O8 S2 C11 108.1(4) . . ? O9' S2 C11 107.1(5) . . ? O9 S2 C11 107.0(4) . . ? O10 S2 C11 107.1(4) . . ? O13 S3 O11' 142.1(11) . . ? O13 S3 O13' 73.2(11) . . ? O11' S3 O13' 110.9(12) . . ? O13 S3 O12' 27.1(9) . . ? O11' S3 O12' 125.3(11) . . ? O13' S3 O12' 99.6(10) . . ? O13 S3 O11 103.8(9) . . ? O11' S3 O11 80.5(10) . . ? O13' S3 O11 32.3(8) . . ? O12' S3 O11 128.0(7) . . ? O13 S3 O12 120.6(10) . . ? O11' S3 O12 33.7(8) . . ? O13' S3 O12 139.6(9) . . ? O12' S3 O12 96.1(9) . . ? O11 S3 O12 113.0(6) . . ? O13 S3 C18 107.1(9) . . ? O11' S3 C18 107.5(7) . . ? O13' S3 C18 106.3(8) . . ? O12' S3 C18 105.8(5) . . ? O11 S3 C18 106.9(4) . . ? O12 S3 C18 104.7(4) . . ? O16 S4 O14 132.1(8) . . ? O16 S4 O14' 106.0(9) . . ? O14 S4 O14' 32.1(7) . . ? O16 S4 O16' 27.3(7) . . ? O14 S4 O16' 111.5(8) . . ? O14' S4 O16' 81.3(9) . . ? O16 S4 O15' 76.4(8) . . ? O14 S4 O15' 124.3(6) . . ? O14' S4 O15' 147.2(8) . . ? O16' S4 O15' 103.4(7) . . ? O16 S4 O15 110.4(8) . . ? O14 S4 O15 87.0(6) . . ? O14' S4 O15 116.5(8) . . ? O16' S4 O15 133.8(7) . . ? O15' S4 O15 38.9(5) . . ? O16 S4 C25 109.4(7) . . ? O14 S4 C25 106.1(5) . . ? O14' S4 C25 105.8(7) . . ? O16' S4 C25 106.2(5) . . ? O15' S4 C25 103.9(4) . . ? O15 S4 C25 108.4(4) . . ? C7 O1 H1 109.5 . . ? C14 O2 H2 109.5 . . ? C21 O3 H3 109.5 . . ? C28 O4 H4 109.5 . . ? C27 C1 C2 111.6(3) . . ? C27 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? C27 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? C3 C2 C7 117.0(4) . . ? C3 C2 C1 118.2(4) . . ? C7 C2 C1 124.8(4) . . ? C2 C3 C4 121.6(4) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C5 C4 C3 120.2(4) . . ? C5 C4 S1 121.8(3) . . ? C3 C4 S1 117.8(3) . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C7 118.3(4) . . ? C5 C6 C8 119.9(4) . . ? C7 C6 C8 121.8(4) . . ? O1 C7 C2 123.1(4) . . ? O1 C7 C6 114.6(4) . . ? C2 C7 C6 122.2(4) . . ? C9 C8 C6 113.8(4) . . ? C9 C8 H8A 108.8 . . ? C6 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? C6 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C14 117.8(4) . . ? C10 C9 C8 119.8(4) . . ? C14 C9 C8 122.4(4) . . ? C11 C10 C9 120.9(4) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C12 120.3(4) . . ? C10 C11 S2 120.6(4) . . ? C12 C11 S2 119.1(4) . . ? C13 C12 C11 120.6(5) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C12 C13 C14 118.6(4) . . ? C12 C13 C15 121.5(4) . . ? C14 C13 C15 119.8(4) . . ? O2 C14 C13 114.6(4) . . ? O2 C14 C9 123.5(4) . . ? C13 C14 C9 121.9(4) . . ? C13 C15 C16 110.9(3) . . ? C13 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.0 . . ? C21 C16 C17 118.0(4) . . ? C21 C16 C15 124.1(4) . . ? C17 C16 C15 117.9(4) . . ? C18 C17 C16 121.3(4) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C19 119.9(5) . . ? C17 C18 S3 118.7(4) . . ? C19 C18 S3 121.4(4) . . ? C20 C19 C18 120.1(4) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 119.1(4) . . ? C19 C20 C22 120.8(4) . . ? C21 C20 C22 120.1(4) . . ? O3 C21 C16 123.9(4) . . ? O3 C21 C20 114.6(4) . . ? C16 C21 C20 121.5(4) . . ? C23 C22 C20 113.2(4) . . ? C23 C22 H22A 108.9 . . ? C20 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? C20 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C28 117.0(4) . . ? C24 C23 C22 120.5(4) . . ? C28 C23 C22 122.5(4) . . ? C25 C24 C23 122.1(4) . . ? C25 C24 H24A 119.0 . . ? C23 C24 H24A 119.0 . . ? C24 C25 C26 119.5(4) . . ? C24 C25 S4 120.5(4) . . ? C26 C25 S4 119.9(4) . . ? C27 C26 C25 120.4(4) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C26 C27 C28 119.3(4) . . ? C26 C27 C1 120.9(4) . . ? C28 C27 C1 119.8(4) . . ? O4 C28 C27 115.2(4) . . ? O4 C28 C23 123.2(4) . . ? C27 C28 C23 121.6(4) . . ? C44 N2 C43 122.6(7) . . ? C44 N2 H2A 118.7 . . ? C43 N2 H2A 118.7 . . ? C39 C38 C43 118.9(7) . . ? C39 C38 C46 122.3(7) . . ? C43 C38 C46 118.9(7) . . ? C40 C39 C38 119.4(8) . . ? C40 C39 H39A 120.3 . . ? C38 C39 H39A 120.3 . . ? C39 C40 C41 123.9(8) . . ? C39 C40 H40A 118.0 . . ? C41 C40 H40A 118.0 . . ? C40 C41 C42 118.8(8) . . ? C40 C41 H41A 120.6 . . ? C42 C41 H41A 120.6 . . ? C43 C42 C41 116.5(7) . . ? C43 C42 H42A 121.7 . . ? C41 C42 H42A 121.7 . . ? C38 C43 N2 118.4(6) . . ? C38 C43 C42 122.5(6) . . ? N2 C43 C42 119.1(6) . . ? N2 C44 C45 118.2(8) . . ? N2 C44 H44A 120.9 . . ? C45 C44 H44A 120.9 . . ? C46 C45 C44 122.4(8) . . ? C46 C45 H45A 118.8 . . ? C44 C45 H45A 118.8 . . ? C45 C46 C38 119.5(8) . . ? C45 C46 H46A 120.2 . . ? C38 C46 H46A 120.2 . . ? C55 N3 C47 123.4(5) . . ? C55 N3 H3B 118.3 . . ? C47 N3 H3B 118.3 . . ? N3 C47 C48 120.7(5) . . ? N3 C47 C52 117.0(5) . . ? C48 C47 C52 122.3(6) . . ? C49 C48 C47 118.7(7) . . ? C49 C48 H48A 120.7 . . ? C47 C48 H48A 120.7 . . ? C48 C49 C50 121.2(7) . . ? C48 C49 H49A 119.4 . . ? C50 C49 H49A 119.4 . . ? C51 C50 C49 121.0(7) . . ? C51 C50 H50A 119.5 . . ? C49 C50 H50A 119.5 . . ? C50 C51 C52 119.8(7) . . ? C50 C51 H51A 120.1 . . ? C52 C51 H51A 120.1 . . ? C47 C52 C53 118.1(5) . . ? C47 C52 C51 116.9(6) . . ? C53 C52 C51 125.0(6) . . ? C54 C53 C52 121.8(5) . . ? C54 C53 H53A 119.1 . . ? C52 C53 H53A 119.1 . . ? C53 C54 C55 118.2(6) . . ? C53 C54 H54A 120.9 . . ? C55 C54 H54A 120.9 . . ? N3 C55 C54 121.5(5) . . ? N3 C55 H55A 119.2 . . ? C54 C55 H55A 119.2 . . ? C37 C29 C30 123.4(14) . . ? C37 C29 C34 116.6(14) . . ? C30 C29 C34 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31A 120.0 . . ? C30 C31 H31A 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? N1 C34 C33 119.9(15) . . ? N1 C34 C29 120.1(14) . . ? C33 C34 C29 120.0 . . ? C34 N1 C35 124(2) . . ? C34 N1 H1C 118.2 . . ? C35 N1 H1C 118.2 . . ? C36 C35 N1 117(2) . . ? C36 C35 H35A 121.6 . . ? N1 C35 H35A 121.6 . . ? C35 C36 C37 120(2) . . ? C35 C36 H36A 119.9 . . ? C37 C36 H36A 119.9 . . ? C36 C37 C29 122.7(19) . . ? C36 C37 H37A 118.7 . . ? C29 C37 H37A 118.7 . . ? N1' C29' C30' 118.5(10) . . ? N1' C29' C34' 121.5(10) . . ? C30' C29' C34' 120.0 . . ? C31' C30' C29' 120.0 . . ? C31' C30' H30B 120.0 . . ? C29' C30' H30B 120.0 . . ? C30' C31' C32' 120.0 . . ? C30' C31' H31B 120.0 . . ? C32' C31' H31B 120.0 . . ? C31' C32' C33' 120.0 . . ? C31' C32' H32B 120.0 . . ? C33' C32' H32B 120.0 . . ? C34' C33' C32' 120.0 . . ? C34' C33' H33B 120.0 . . ? C32' C33' H33B 120.0 . . ? C33' C34' C29' 120.0 . . ? C33' C34' C35' 125.8(12) . . ? C29' C34' C35' 114.1(12) . . ? C36' C35' C34' 124(2) . . ? C36' C35' H35B 117.8 . . ? C34' C35' H35B 117.8 . . ? C35' C36' C37' 119.4(18) . . ? C35' C36' H36B 120.3 . . ? C37' C36' H36B 120.3 . . ? N1' C37' C36' 115.0(14) . . ? N1' C37' H37B 122.5 . . ? C36' C37' H37B 122.5 . . ? C29' N1' C37' 125.2(13) . . ? C29' N1' H1'A 117.4 . . ? C37' N1' H1'A 117.4 . . ? 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 C27 C1 C2 C3 -75.0(5) . . . . ? C27 C1 C2 C7 104.9(5) . . . . ? C7 C2 C3 C4 -0.8(6) . . . . ? C1 C2 C3 C4 179.1(4) . . . . ? C2 C3 C4 C5 -3.5(7) . . . . ? C2 C3 C4 S1 173.5(3) . . . . ? O5 S1 C4 C5 123.3(4) . . . . ? O7 S1 C4 C5 -117.8(4) . . . . ? O6 S1 C4 C5 3.4(4) . . . . ? O5 S1 C4 C3 -53.6(4) . . . . ? O7 S1 C4 C3 65.4(4) . . . . ? O6 S1 C4 C3 -173.4(4) . . . . ? C3 C4 C5 C6 2.9(7) . . . . ? S1 C4 C5 C6 -173.9(4) . . . . ? C4 C5 C6 C7 1.8(6) . . . . ? C4 C5 C6 C8 179.9(4) . . . . ? C3 C2 C7 O1 -173.5(4) . . . . ? C1 C2 C7 O1 6.6(7) . . . . ? C3 C2 C7 C6 5.7(6) . . . . ? C1 C2 C7 C6 -174.2(4) . . . . ? C5 C6 C7 O1 173.0(4) . . . . ? C8 C6 C7 O1 -5.1(6) . . . . ? C5 C6 C7 C2 -6.2(7) . . . . ? C8 C6 C7 C2 175.7(4) . . . . ? C5 C6 C8 C9 86.9(5) . . . . ? C7 C6 C8 C9 -95.0(5) . . . . ? C6 C8 C9 C10 -107.9(5) . . . . ? C6 C8 C9 C14 72.5(5) . . . . ? C14 C9 C10 C11 -1.0(7) . . . . ? C8 C9 C10 C11 179.3(4) . . . . ? C9 C10 C11 C12 -0.4(7) . . . . ? C9 C10 C11 S2 179.7(3) . . . . ? O10' S2 C11 C10 155.2(10) . . . . ? O8' S2 C11 C10 -85.4(9) . . . . ? O8 S2 C11 C10 -33.7(7) . . . . ? O9' S2 C11 C10 37.6(8) . . . . ? O9 S2 C11 C10 91.8(7) . . . . ? O10 S2 C11 C10 -155.1(6) . . . . ? O10' S2 C11 C12 -24.6(10) . . . . ? O8' S2 C11 C12 94.7(9) . . . . ? O8 S2 C11 C12 146.5(6) . . . . ? O9' S2 C11 C12 -142.3(7) . . . . ? O9 S2 C11 C12 -88.0(7) . . . . ? O10 S2 C11 C12 25.1(7) . . . . ? C10 C11 C12 C13 0.9(7) . . . . ? S2 C11 C12 C13 -179.3(3) . . . . ? C11 C12 C13 C14 0.2(7) . . . . ? C11 C12 C13 C15 -177.8(4) . . . . ? C12 C13 C14 O2 178.7(4) . . . . ? C15 C13 C14 O2 -3.3(6) . . . . ? C12 C13 C14 C9 -1.7(6) . . . . ? C15 C13 C14 C9 176.3(4) . . . . ? C10 C9 C14 O2 -178.3(4) . . . . ? C8 C9 C14 O2 1.3(6) . . . . ? C10 C9 C14 C13 2.1(6) . . . . ? C8 C9 C14 C13 -178.2(4) . . . . ? C12 C13 C15 C16 98.4(5) . . . . ? C14 C13 C15 C16 -79.5(5) . . . . ? C13 C15 C16 C21 108.2(5) . . . . ? C13 C15 C16 C17 -72.4(5) . . . . ? C21 C16 C17 C18 -1.6(7) . . . . ? C15 C16 C17 C18 179.0(4) . . . . ? C16 C17 C18 C19 -1.4(7) . . . . ? C16 C17 C18 S3 178.1(4) . . . . ? O13 S3 C18 C17 176.0(9) . . . . ? O11' S3 C18 C17 -19.9(10) . . . . ? O13' S3 C18 C17 99.0(10) . . . . ? O12' S3 C18 C17 -155.8(8) . . . . ? O11 S3 C18 C17 65.2(6) . . . . ? O12 S3 C18 C17 -54.9(7) . . . . ? O13 S3 C18 C19 -4.5(10) . . . . ? O11' S3 C18 C19 159.7(10) . . . . ? O13' S3 C18 C19 -81.5(10) . . . . ? O12' S3 C18 C19 23.8(9) . . . . ? O11 S3 C18 C19 -115.2(6) . . . . ? O12 S3 C18 C19 124.7(6) . . . . ? C17 C18 C19 C20 0.9(7) . . . . ? S3 C18 C19 C20 -178.7(4) . . . . ? C18 C19 C20 C21 2.6(7) . . . . ? C18 C19 C20 C22 -177.7(4) . . . . ? C17 C16 C21 O3 -175.5(4) . . . . ? C15 C16 C21 O3 3.9(7) . . . . ? C17 C16 C21 C20 5.1(6) . . . . ? C15 C16 C21 C20 -175.5(4) . . . . ? C19 C20 C21 O3 174.8(4) . . . . ? C22 C20 C21 O3 -4.9(6) . . . . ? C19 C20 C21 C16 -5.7(7) . . . . ? C22 C20 C21 C16 174.6(4) . . . . ? C19 C20 C22 C23 83.7(5) . . . . ? C21 C20 C22 C23 -96.6(5) . . . . ? C20 C22 C23 C24 -107.1(5) . . . . ? C20 C22 C23 C28 72.8(6) . . . . ? C28 C23 C24 C25 -0.9(7) . . . . ? C22 C23 C24 C25 179.0(4) . . . . ? C23 C24 C25 C26 -0.1(7) . . . . ? C23 C24 C25 S4 179.7(4) . . . . ? O16 S4 C25 C24 -123.5(8) . . . . ? O14 S4 C25 C24 89.2(7) . . . . ? O14' S4 C25 C24 122.7(8) . . . . ? O16' S4 C25 C24 -151.9(7) . . . . ? O15' S4 C25 C24 -43.2(6) . . . . ? O15 S4 C25 C24 -3.0(8) . . . . ? O16 S4 C25 C26 56.4(8) . . . . ? O14 S4 C25 C26 -90.9(7) . . . . ? O14' S4 C25 C26 -57.4(8) . . . . ? O16' S4 C25 C26 27.9(7) . . . . ? O15' S4 C25 C26 136.6(6) . . . . ? O15 S4 C25 C26 176.9(7) . . . . ? C24 C25 C26 C27 0.3(7) . . . . ? S4 C25 C26 C27 -179.6(3) . . . . ? C25 C26 C27 C28 0.6(6) . . . . ? C25 C26 C27 C1 -179.0(4) . . . . ? C2 C1 C27 C26 99.9(5) . . . . ? C2 C1 C27 C28 -79.7(5) . . . . ? C26 C27 C28 O4 178.2(4) . . . . ? C1 C27 C28 O4 -2.2(6) . . . . ? C26 C27 C28 C23 -1.8(6) . . . . ? C1 C27 C28 C23 177.9(4) . . . . ? C24 C23 C28 O4 -178.0(4) . . . . ? C22 C23 C28 O4 2.0(7) . . . . ? C24 C23 C28 C27 1.9(6) . . . . ? C22 C23 C28 C27 -178.0(4) . . . . ? C43 C38 C39 C40 0.0(10) . . . . ? C46 C38 C39 C40 -179.5(7) . . . . ? C38 C39 C40 C41 0.7(13) . . . . ? C39 C40 C41 C42 -0.9(13) . . . . ? C40 C41 C42 C43 0.3(11) . . . . ? C39 C38 C43 N2 178.2(6) . . . . ? C46 C38 C43 N2 -2.3(8) . . . . ? C39 C38 C43 C42 -0.5(9) . . . . ? C46 C38 C43 C42 179.0(6) . . . . ? C44 N2 C43 C38 1.6(9) . . . . ? C44 N2 C43 C42 -179.7(7) . . . . ? C41 C42 C43 C38 0.4(10) . . . . ? C41 C42 C43 N2 -178.3(6) . . . . ? C43 N2 C44 C45 -0.9(10) . . . . ? N2 C44 C45 C46 1.2(12) . . . . ? C44 C45 C46 C38 -2.0(12) . . . . ? C39 C38 C46 C45 -177.9(7) . . . . ? C43 C38 C46 C45 2.6(10) . . . . ? C55 N3 C47 C48 178.1(5) . . . . ? C55 N3 C47 C52 -2.2(8) . . . . ? N3 C47 C48 C49 179.7(5) . . . . ? C52 C47 C48 C49 -0.1(8) . . . . ? C47 C48 C49 C50 -0.7(9) . . . . ? C48 C49 C50 C51 0.8(11) . . . . ? C49 C50 C51 C52 0.0(10) . . . . ? N3 C47 C52 C53 0.9(7) . . . . ? C48 C47 C52 C53 -179.4(5) . . . . ? N3 C47 C52 C51 -178.9(5) . . . . ? C48 C47 C52 C51 0.8(8) . . . . ? C50 C51 C52 C47 -0.8(9) . . . . ? C50 C51 C52 C53 179.4(6) . . . . ? C47 C52 C53 C54 1.1(8) . . . . ? C51 C52 C53 C54 -179.0(6) . . . . ? C52 C53 C54 C55 -2.0(9) . . . . ? C47 N3 C55 C54 1.3(9) . . . . ? C53 C54 C55 N3 0.8(9) . . . . ? C37 C29 C30 C31 178.1(19) . . . . ? C34 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 N1 177(2) . . . . ? C32 C33 C34 C29 0.0 . . . . ? C37 C29 C34 N1 5(3) . . . . ? C30 C29 C34 N1 -177(2) . . . . ? C37 C29 C34 C33 -178.2(18) . . . . ? C30 C29 C34 C33 0.0 . . . . ? C33 C34 N1 C35 -179(2) . . . . ? C29 C34 N1 C35 -2(4) . . . . ? C34 N1 C35 C36 0(4) . . . . ? N1 C35 C36 C37 -1(3) . . . . ? C35 C36 C37 C29 4(4) . . . . ? C30 C29 C37 C36 176(2) . . . . ? C34 C29 C37 C36 -6(3) . . . . ? N1' C29' C30' C31' -177.3(10) . . . . ? C34' C29' C30' C31' 0.0 . . . . ? C29' C30' C31' C32' 0.0 . . . . ? C30' C31' C32' C33' 0.0 . . . . ? C31' C32' C33' C34' 0.0 . . . . ? C32' C33' C34' C29' 0.0 . . . . ? C32' C33' C34' C35' -175.9(18) . . . . ? N1' C29' C34' C33' 177.2(10) . . . . ? C30' C29' C34' C33' 0.0 . . . . ? N1' C29' C34' C35' -6.4(17) . . . . ? C30' C29' C34' C35' 176.4(16) . . . . ? C33' C34' C35' C36' -176.3(17) . . . . ? C29' C34' C35' C36' 8(3) . . . . ? C34' C35' C36' C37' -4(4) . . . . ? C35' C36' C37' N1' -1(3) . . . . ? C30' C29' N1' C37' 179.3(16) . . . . ? C34' C29' N1' C37' 2(2) . . . . ? C36' C37' N1' C29' 2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.984 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.095