# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email cchen@iccas.ac.cn _publ_contact_author_name 'C.-F. Chen' loop_ _publ_author_name 'Y. Han' 'Y.-K. Gu' 'C.-F. Chen' # Attachment '- complex 1-2.cif' data_a1-2 _database_code_depnum_ccdc_archive 'CCDC 898289' #TrackingRef '- complex 1-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H92 O20, C18 H24 N2 O2, 2(F6 P)' _chemical_formula_sum 'C94 H116 F12 N2 O22 P2' _chemical_formula_weight 1915.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.650(3) _cell_length_b 18.189(4) _cell_length_c 19.264(4) _cell_angle_alpha 82.751(12) _cell_angle_beta 72.674(7) _cell_angle_gamma 80.096(10) _cell_volume 4483.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14523 _cell_measurement_theta_min 1.5788 _cell_measurement_theta_max 27.4777 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7929 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33579 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0810 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15710 _reflns_number_gt 11575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _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. DFIX 1.43 0.01 C26 O3 C26 O3' DFIX 1.43 0.01 O3 C27 O3' C27' DFIX 1.54 0.01 C27 C28 C27' C28 SIMU 0.01 0.02 1.7 O3 C27 SIMU 0.01 0.02 1.7 O3' C27' ISOR 0.01 0.02 O3 C27 ISOR 0.01 0.02 O3' C27' ; _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^)+(0.1044P)^2^+10.7649P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15710 _refine_ls_number_parameters 1212 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.1189 _refine_ls_wR_factor_ref 0.2869 _refine_ls_wR_factor_gt 0.2636 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.28753(14) 0.45591(9) 0.28394(9) 0.0476(4) Uani 1 1 d . . . P2 P 0.67531(19) 0.02719(12) 0.20471(16) 0.0834(8) Uani 1 1 d . . . F1 F 0.3835(4) 0.4289(3) 0.2216(3) 0.1124(19) Uani 1 1 d . . . F2 F 0.3480(5) 0.5126(3) 0.3029(3) 0.108(2) Uani 1 1 d . . . F3 F 0.3235(3) 0.3957(2) 0.3417(2) 0.0650(11) Uani 1 1 d . . . F4 F 0.2217(4) 0.4016(3) 0.2686(3) 0.1088(19) Uani 1 1 d . . . F5 F 0.2517(4) 0.5178(3) 0.2277(3) 0.0987(17) Uani 1 1 d . . . F6 F 0.1891(4) 0.4843(3) 0.3481(3) 0.0966(16) Uani 1 1 d . . . F7 F 0.7973(4) 0.0265(3) 0.1855(4) 0.128(2) Uani 1 1 d . . . F8 F 0.6559(4) 0.1119(3) 0.2194(4) 0.117(2) Uani 1 1 d . . . F9 F 0.6714(6) 0.0029(3) 0.2849(4) 0.129(2) Uani 1 1 d . . . F10 F 0.6948(4) -0.0571(2) 0.1858(3) 0.1035(18) Uani 1 1 d . . . F11 F 0.6826(4) 0.0533(3) 0.1209(3) 0.1140(19) Uani 1 1 d . . . F12 F 0.5540(3) 0.0272(2) 0.2196(3) 0.0859(14) Uani 1 1 d . . . O1 O 0.5599(3) 0.1637(2) -0.0945(2) 0.0360(9) Uani 1 1 d . . . O2 O 0.3910(3) 0.0863(2) -0.0164(2) 0.0476(10) Uani 1 1 d . . . O4 O 0.0764(3) 0.0070(3) 0.2710(2) 0.0574(12) Uani 1 1 d . B . O5 O 0.1650(3) 0.0949(3) 0.3415(2) 0.0575(12) Uani 1 1 d . . . O6 O 0.1585(3) 0.2350(3) 0.2934(2) 0.0545(12) Uani 1 1 d . . . O7 O 0.1816(3) 0.3046(2) 0.1495(2) 0.0448(10) Uani 1 1 d . . . O8 O 0.2215(3) 0.3515(3) -0.0031(2) 0.0510(11) Uani 1 1 d . . . O9 O 0.3488(3) 0.3938(2) -0.1433(2) 0.0436(10) Uani 1 1 d . . . O10 O 0.5442(2) 0.30253(19) -0.14179(19) 0.0323(8) Uani 1 1 d . . . O11 O 0.8569(3) 0.2386(2) 0.22053(19) 0.0387(9) Uani 1 1 d . . . O12 O 0.8069(3) 0.1873(2) 0.3744(2) 0.0474(10) Uani 1 1 d . . . O13 O 0.7841(3) 0.1886(2) 0.5228(2) 0.0461(10) Uani 1 1 d . . . O14 O 0.6611(3) 0.1424(3) 0.6613(2) 0.0611(13) Uani 1 1 d . . . O15 O 0.4629(3) 0.2067(3) 0.6542(2) 0.0560(13) Uani 1 1 d . . . O16 O 0.4430(3) 0.3437(2) 0.6028(2) 0.0401(9) Uani 1 1 d . . . O17 O 0.6087(3) 0.4265(2) 0.5275(2) 0.0373(9) Uani 1 1 d . . . O18 O 0.8086(3) 0.4605(2) 0.4140(2) 0.0374(9) Uani 1 1 d . . . O19 O 0.9249(3) 0.4897(2) 0.23667(19) 0.0379(9) Uani 1 1 d . . . O20 O 0.8457(3) 0.3808(2) 0.18153(19) 0.0355(9) Uani 1 1 d . . . O21 O 0.3868(4) 0.2577(3) 0.2410(3) 0.0701(14) Uani 1 1 d . . . H21 H 0.4427 0.2693 0.2397 0.084 Uiso 1 1 d R . . O22 O 0.5650(5) 0.2857(4) 0.2702(3) 0.0943(18) Uani 1 1 d . . . H22 H 0.6147 0.2524 0.2664 0.113 Uiso 1 1 d R . . N1 N 0.4884(3) 0.2486(3) 0.0808(3) 0.0427(12) Uani 1 1 d . . . N2 N 0.5177(3) 0.2535(3) 0.4325(3) 0.0378(11) Uani 1 1 d . . . C1 C 0.8539(4) 0.3348(3) 0.1270(3) 0.0309(12) Uani 1 1 d . . . C2 C 0.8638(4) 0.2577(3) 0.1480(3) 0.0301(11) Uani 1 1 d . . . C3 C 0.8786(4) 0.2079(3) 0.0962(3) 0.0304(11) Uani 1 1 d . . . H3 H 0.8874 0.1556 0.1093 0.037 Uiso 1 1 calc R . . C4 C 0.8807(4) 0.2341(3) 0.0246(3) 0.0246(10) Uani 1 1 d . . . C5 C 0.8681(3) 0.3102(3) 0.0044(3) 0.0258(11) Uani 1 1 d . . . C6 C 0.8552(4) 0.3612(3) 0.0555(3) 0.0270(11) Uani 1 1 d . . . H6 H 0.8475 0.4135 0.0419 0.032 Uiso 1 1 calc R . . C7 C 0.8928(4) 0.1835(3) -0.0365(3) 0.0272(11) Uani 1 1 d . . . C8 C 0.9081(4) 0.1003(3) -0.0149(3) 0.0330(12) Uani 1 1 d . . . H8A H 0.8475 0.0873 0.0243 0.049 Uiso 1 1 calc R . . H8C H 0.9702 0.0872 0.0021 0.049 Uiso 1 1 calc R . . H8B H 0.9164 0.0725 -0.0572 0.049 Uiso 1 1 calc R . . C9 C 0.9824(4) 0.2105(3) -0.1003(3) 0.0293(11) Uani 1 1 d . . . C10 C 1.0703(4) 0.1651(3) -0.1369(3) 0.0334(12) Uani 1 1 d . . . H10 H 1.0813 0.1132 -0.1223 0.040 Uiso 1 1 calc R . . C11 C 1.1429(4) 0.1970(4) -0.1957(3) 0.0407(14) Uani 1 1 d . . . H11 H 1.2033 0.1666 -0.2216 0.049 Uiso 1 1 calc R . . C12 C 1.1265(4) 0.2724(3) -0.2160(3) 0.0392(14) Uani 1 1 d . . . H12 H 1.1756 0.2933 -0.2564 0.047 Uiso 1 1 calc R . . C13 C 1.0400(4) 0.3184(3) -0.1787(3) 0.0314(12) Uani 1 1 d . . . H13 H 1.0302 0.3706 -0.1925 0.038 Uiso 1 1 calc R . . C14 C 0.9677(4) 0.2868(3) -0.1206(3) 0.0260(11) Uani 1 1 d . . . C15 C 0.8667(4) 0.3299(3) -0.0753(3) 0.0261(11) Uani 1 1 d . . . C16 C 0.8528(4) 0.4130(3) -0.0969(3) 0.0335(12) Uani 1 1 d . . . H16B H 0.8530 0.4213 -0.1482 0.050 Uiso 1 1 calc R . . H16C H 0.9098 0.4350 -0.0903 0.050 Uiso 1 1 calc R . . H16A H 0.7867 0.4366 -0.0663 0.050 Uiso 1 1 calc R . . C17 C 0.7823(3) 0.2877(3) -0.0840(2) 0.0238(10) Uani 1 1 d . . . C18 C 0.6999(4) 0.3203(3) -0.1108(3) 0.0274(11) Uani 1 1 d . . . H18 H 0.6924 0.3723 -0.1257 0.033 Uiso 1 1 calc R . . C19 C 0.6281(3) 0.2767(3) -0.1160(3) 0.0258(11) Uani 1 1 d . . . C20 C 0.6382(4) 0.2008(3) -0.0917(3) 0.0280(11) Uani 1 1 d . . . C21 C 0.7230(4) 0.1672(3) -0.0659(2) 0.0269(11) Uani 1 1 d . . . H21A H 0.7309 0.1153 -0.0508 0.032 Uiso 1 1 calc R . . C22 C 0.7955(4) 0.2117(3) -0.0630(2) 0.0251(11) Uani 1 1 d . . . C23 C 0.5696(4) 0.0841(3) -0.0795(3) 0.0324(12) Uani 1 1 d . . . H23A H 0.5827 0.0696 -0.0314 0.039 Uiso 1 1 calc R . . H23B H 0.6277 0.0593 -0.1173 0.039 Uiso 1 1 calc R . . C24 C 0.4694(4) 0.0619(3) -0.0796(3) 0.0418(14) Uani 1 1 d . . . H24B H 0.4502 0.0849 -0.1240 0.050 Uiso 1 1 calc R . . H24A H 0.4765 0.0068 -0.0797 0.050 Uiso 1 1 calc R . . C25 C 0.2888(5) 0.0958(4) -0.0260(4) 0.0626(19) Uani 1 1 d . B . H25A H 0.2764 0.0488 -0.0407 0.075 Uiso 1 1 calc R . . H25B H 0.2834 0.1357 -0.0653 0.075 Uiso 1 1 calc R . . C26 C 0.2115(5) 0.1157(4) 0.0410(4) 0.074(2) Uani 1 1 d D . . H26A H 0.1465 0.1413 0.0310 0.088 Uiso 1 1 calc R A 1 H26B H 0.2366 0.1494 0.0665 0.088 Uiso 1 1 calc R A 1 O3 O 0.1947(6) 0.0456(4) 0.0849(4) 0.046(2) Uani 0.646(18) 1 d PDU B 1 C27 C 0.1344(10) 0.0645(5) 0.1555(5) 0.052(3) Uani 0.646(18) 1 d PDU B 1 H27A H 0.0770 0.1049 0.1520 0.063 Uiso 0.646(18) 1 calc PR B 1 H27B H 0.1777 0.0824 0.1811 0.063 Uiso 0.646(18) 1 calc PR B 1 O3' O 0.2000(11) 0.0703(10) 0.1081(7) 0.053(5) Uani 0.354(18) 1 d PDU B 2 C27' C 0.0949(11) 0.0567(9) 0.1340(9) 0.046(5) Uani 0.354(18) 1 d PDU B 2 H27C H 0.0732 0.0397 0.0947 0.055 Uiso 0.354(18) 1 calc PR B 2 H27D H 0.0484 0.1027 0.1515 0.055 Uiso 0.354(18) 1 calc PR B 2 C28 C 0.0912(6) -0.0050(3) 0.1971(3) 0.0519(16) Uani 1 1 d D . . H28A H 0.0248 -0.0096 0.1882 0.062 Uiso 1 1 calc R B 1 H28B H 0.1409 -0.0508 0.1830 0.062 Uiso 1 1 calc R B 1 C29 C 0.1674(6) -0.0169(4) 0.2927(5) 0.079(3) Uani 1 1 d . . . H29A H 0.2280 -0.0015 0.2540 0.095 Uiso 1 1 calc R B . H29B H 0.1781 -0.0722 0.3009 0.095 Uiso 1 1 calc R . . C30 C 0.1569(6) 0.0180(4) 0.3628(5) 0.069(2) Uani 1 1 d . B . H30A H 0.0891 0.0121 0.3986 0.083 Uiso 1 1 calc R . . H30B H 0.2128 -0.0056 0.3847 0.083 Uiso 1 1 calc R . . C31 C 0.1545(4) 0.1435(3) 0.3934(3) 0.0399(14) Uani 1 1 d . . . C32 C 0.1521(4) 0.1240(3) 0.4658(3) 0.0351(12) Uani 1 1 d . . . H32 H 0.1585 0.0728 0.4836 0.042 Uiso 1 1 calc R . . C33 C 0.1403(4) 0.1797(3) 0.5121(3) 0.0312(12) Uani 1 1 d . . . C34 C 0.1295(4) 0.2547(3) 0.4864(3) 0.0267(11) Uani 1 1 d . . . C35 C 0.1338(4) 0.2744(3) 0.4132(3) 0.0321(12) Uani 1 1 d . . . H35 H 0.1279 0.3256 0.3952 0.039 Uiso 1 1 calc R . . C36 C 0.1468(4) 0.2188(4) 0.3673(3) 0.0397(14) Uani 1 1 d . . . C37 C 0.0746(4) 0.2770(4) 0.2721(3) 0.0473(15) Uani 1 1 d . . . H37B H 0.0679 0.3300 0.2821 0.057 Uiso 1 1 calc R . . H37A H 0.0095 0.2574 0.2998 0.057 Uiso 1 1 calc R . . C38 C 0.0939(5) 0.2713(4) 0.1929(3) 0.0585(19) Uani 1 1 d . . . H38A H 0.1046 0.2178 0.1835 0.070 Uiso 1 1 calc R . . H38B H 0.0318 0.2961 0.1782 0.070 Uiso 1 1 calc R . . C39 C 0.1541(5) 0.3782(3) 0.1203(3) 0.0507(16) Uani 1 1 d . . . H39B H 0.2123 0.4071 0.1120 0.061 Uiso 1 1 calc R . . H39A H 0.0932 0.4034 0.1559 0.061 Uiso 1 1 calc R . . C40 C 0.1291(5) 0.3775(4) 0.0501(4) 0.0599(19) Uani 1 1 d . . . H40A H 0.0765 0.3440 0.0565 0.072 Uiso 1 1 calc R . . H40B H 0.1007 0.4285 0.0344 0.072 Uiso 1 1 calc R . . C41 C 0.2058(4) 0.3365(4) -0.0693(3) 0.0508(16) Uani 1 1 d . . . H41B H 0.1610 0.3793 -0.0864 0.061 Uiso 1 1 calc R . . H41A H 0.1710 0.2914 -0.0613 0.061 Uiso 1 1 calc R . . C42 C 0.3093(4) 0.3241(4) -0.1257(3) 0.0454(15) Uani 1 1 d . . . H42B H 0.3576 0.2860 -0.1062 0.055 Uiso 1 1 calc R . . H42A H 0.3013 0.3061 -0.1698 0.055 Uiso 1 1 calc R . . C43 C 0.4430(4) 0.3921(4) -0.2021(3) 0.0439(15) Uani 1 1 d . . . H43B H 0.4430 0.4408 -0.2316 0.053 Uiso 1 1 calc R . . H43A H 0.4462 0.3527 -0.2340 0.053 Uiso 1 1 calc R . . C44 C 0.5370(4) 0.3770(3) -0.1741(3) 0.0345(12) Uani 1 1 d . . . H44B H 0.6001 0.3834 -0.2148 0.041 Uiso 1 1 calc R . . H44A H 0.5307 0.4125 -0.1376 0.041 Uiso 1 1 calc R . . C45 C 0.1422(4) 0.1675(3) 0.5922(3) 0.0295(11) Uani 1 1 d . . . C46 C 0.1560(4) 0.0861(3) 0.6200(3) 0.0387(13) Uani 1 1 d . . . H46A H 0.0960 0.0634 0.6199 0.058 Uiso 1 1 calc R . . H46C H 0.1621 0.0823 0.6697 0.058 Uiso 1 1 calc R . . H46B H 0.2190 0.0599 0.5882 0.058 Uiso 1 1 calc R . . C47 C 0.0417(4) 0.2142(3) 0.6349(3) 0.0277(11) Uani 1 1 d . . . C48 C -0.0301(4) 0.1877(3) 0.6963(3) 0.0326(12) Uani 1 1 d . . . H48 H -0.0206 0.1366 0.7141 0.039 Uiso 1 1 calc R . . C49 C -0.1157(4) 0.2358(3) 0.7317(3) 0.0340(13) Uani 1 1 d . . . H49 H -0.1646 0.2178 0.7741 0.041 Uiso 1 1 calc R . . C50 C -0.1299(4) 0.3101(3) 0.7052(3) 0.0371(13) Uani 1 1 d . . . H50 H -0.1891 0.3428 0.7292 0.045 Uiso 1 1 calc R . . C51 C -0.0575(4) 0.3372(3) 0.6432(3) 0.0329(12) Uani 1 1 d . . . H51 H -0.0670 0.3882 0.6251 0.040 Uiso 1 1 calc R . . C52 C 0.0285(3) 0.2886(3) 0.6085(2) 0.0256(11) Uani 1 1 d . . . C53 C 0.1170(4) 0.3108(3) 0.5431(3) 0.0258(11) Uani 1 1 d . . . C54 C 0.1042(4) 0.3921(3) 0.5135(3) 0.0321(12) Uani 1 1 d . . . H54B H 0.1634 0.4006 0.4711 0.048 Uiso 1 1 calc R . . H54C H 0.1010 0.4244 0.5514 0.048 Uiso 1 1 calc R . . H54A H 0.0401 0.4038 0.4988 0.048 Uiso 1 1 calc R . . C55 C 0.2143(4) 0.2861(3) 0.5706(3) 0.0280(11) Uani 1 1 d . . . C56 C 0.2271(4) 0.2115(3) 0.5957(3) 0.0264(11) Uani 1 1 d . . . C57 C 0.3100(4) 0.1823(3) 0.6239(3) 0.0315(12) Uani 1 1 d . . . H57 H 0.3188 0.1310 0.6413 0.038 Uiso 1 1 calc R . . C58 C 0.3794(4) 0.2283(3) 0.6265(3) 0.0352(13) Uani 1 1 d . . . C59 C 0.3670(4) 0.3040(3) 0.6000(3) 0.0319(12) Uani 1 1 d . . . C60 C 0.2833(4) 0.3335(3) 0.5726(3) 0.0269(11) Uani 1 1 d . . . H60 H 0.2736 0.3848 0.5556 0.032 Uiso 1 1 calc R . . C61 C 0.4766(5) 0.1379(4) 0.6885(4) 0.066(2) Uani 1 1 d . . . H61A H 0.4912 0.0989 0.6539 0.079 Uiso 1 1 calc R . . H61B H 0.4137 0.1292 0.7286 0.079 Uiso 1 1 calc R . . C62 C 0.5688(4) 0.1356(5) 0.7188(4) 0.068(2) Uani 1 1 d . . . H62B H 0.5550 0.1770 0.7507 0.082 Uiso 1 1 calc R . . H62A H 0.5777 0.0878 0.7486 0.082 Uiso 1 1 calc R . . C63 C 0.6844(5) 0.2166(4) 0.6423(3) 0.0555(18) Uani 1 1 d . . . H63B H 0.6845 0.2395 0.6862 0.067 Uiso 1 1 calc R . . H63A H 0.6315 0.2473 0.6211 0.067 Uiso 1 1 calc R . . C64 C 0.7896(4) 0.2137(4) 0.5875(3) 0.0493(16) Uani 1 1 d . . . H64A H 0.8113 0.2640 0.5776 0.059 Uiso 1 1 calc R . . H64B H 0.8413 0.1791 0.6070 0.059 Uiso 1 1 calc R . . C65 C 0.8822(4) 0.1775(4) 0.4716(3) 0.0546(18) Uani 1 1 d . . . H65B H 0.9327 0.1463 0.4947 0.065 Uiso 1 1 calc R . . H65A H 0.9071 0.2263 0.4532 0.065 Uiso 1 1 calc R . . C66 C 0.8733(5) 0.1394(4) 0.4099(3) 0.0528(16) Uani 1 1 d . . . H66B H 0.9426 0.1276 0.3750 0.063 Uiso 1 1 calc R . . H66A H 0.8449 0.0919 0.4287 0.063 Uiso 1 1 calc R . . C67 C 0.7841(6) 0.1537(4) 0.3197(3) 0.063(2) Uani 1 1 d . . . H67A H 0.7145 0.1766 0.3161 0.076 Uiso 1 1 calc R . . H67B H 0.7815 0.0998 0.3350 0.076 Uiso 1 1 calc R . . C68 C 0.8577(7) 0.1607(4) 0.2483(3) 0.065(2) Uani 1 1 d . . . H68A H 0.8398 0.1323 0.2143 0.079 Uiso 1 1 calc R . . H68B H 0.9281 0.1392 0.2514 0.079 Uiso 1 1 calc R . . C69 C 0.8257(4) 0.4591(3) 0.1655(3) 0.0347(12) Uani 1 1 d . . . H69A H 0.7586 0.4727 0.1538 0.042 Uiso 1 1 calc R . . H69B H 0.8811 0.4758 0.1231 0.042 Uiso 1 1 calc R . . C70 C 0.8225(4) 0.4956(3) 0.2325(3) 0.0368(13) Uani 1 1 d . . . H70B H 0.7919 0.5489 0.2291 0.044 Uiso 1 1 calc R . . H70A H 0.7795 0.4702 0.2768 0.044 Uiso 1 1 calc R . . C71 C 0.9318(5) 0.5057(3) 0.3051(3) 0.0416(14) Uani 1 1 d . . . H71A H 0.8837 0.5519 0.3204 0.050 Uiso 1 1 calc R . . H71B H 1.0030 0.5156 0.2993 0.050 Uiso 1 1 calc R . . C72 C 0.9067(5) 0.4440(4) 0.3640(3) 0.0534(17) Uani 1 1 d . . . H72A H 0.9088 0.3976 0.3413 0.064 Uiso 1 1 calc R . . H72B H 0.9602 0.4347 0.3904 0.064 Uiso 1 1 calc R . . C73 C 0.7925(4) 0.4043(3) 0.4740(3) 0.0423(14) Uani 1 1 d . . . H73B H 0.8569 0.3900 0.4891 0.051 Uiso 1 1 calc R . . H73A H 0.7763 0.3592 0.4583 0.051 Uiso 1 1 calc R . . C74 C 0.7057(4) 0.4321(4) 0.5374(3) 0.0427(14) Uani 1 1 d . . . H74A H 0.7129 0.4023 0.5827 0.051 Uiso 1 1 calc R . . H74B H 0.7093 0.4850 0.5425 0.051 Uiso 1 1 calc R . . C75 C 0.5259(4) 0.4496(3) 0.5889(3) 0.0403(14) Uani 1 1 d . . . H75A H 0.5148 0.5049 0.5885 0.048 Uiso 1 1 calc R . . H75B H 0.5434 0.4286 0.6344 0.048 Uiso 1 1 calc R . . C76 C 0.4281(4) 0.4227(3) 0.5864(3) 0.0386(13) Uani 1 1 d . . . H76B H 0.3669 0.4465 0.6229 0.046 Uiso 1 1 calc R . . H76A H 0.4174 0.4349 0.5374 0.046 Uiso 1 1 calc R . . C77 C 0.5646(4) 0.2775(4) 0.0955(3) 0.0497(16) Uani 1 1 d . . . H77 H 0.6099 0.2462 0.1194 0.060 Uiso 1 1 calc R . . C78 C 0.5769(4) 0.3505(4) 0.0764(3) 0.0451(15) Uani 1 1 d . . . H78 H 0.6306 0.3700 0.0871 0.054 Uiso 1 1 calc R . . C79 C 0.5114(4) 0.3967(3) 0.0412(3) 0.0399(14) Uani 1 1 d . . . C80 C 0.5264(4) 0.4752(4) 0.0189(3) 0.0452(15) Uani 1 1 d . . . H80 H 0.5791 0.4925 0.0329 0.054 Uiso 1 1 calc R . . C81 C 0.4331(4) 0.3653(4) 0.0265(3) 0.0432(14) Uani 1 1 d . . . H81 H 0.3873 0.3951 0.0019 0.052 Uiso 1 1 calc R . . C82 C 0.4234(4) 0.2920(3) 0.0477(3) 0.0421(14) Uani 1 1 d . . . H82 H 0.3694 0.2713 0.0387 0.050 Uiso 1 1 calc R . . C83 C 0.4744(5) 0.1685(3) 0.1024(4) 0.0512(16) Uani 1 1 d . . . H83B H 0.5390 0.1404 0.1111 0.061 Uiso 1 1 calc R . . H83A H 0.4620 0.1469 0.0616 0.061 Uiso 1 1 calc R . . C84 C 0.3855(5) 0.1584(4) 0.1699(4) 0.0492(16) Uani 1 1 d . . . H84A H 0.3219 0.1882 0.1611 0.059 Uiso 1 1 calc R . . H84B H 0.3753 0.1051 0.1770 0.059 Uiso 1 1 calc R . . C85 C 0.3967(5) 0.1799(4) 0.2385(4) 0.0543(17) Uani 1 1 d . . . H85A H 0.3434 0.1597 0.2802 0.065 Uiso 1 1 calc R . . H85B H 0.4656 0.1568 0.2438 0.065 Uiso 1 1 calc R . . C86 C 0.4416(4) 0.2277(3) 0.4152(3) 0.0442(14) Uani 1 1 d . . . H86 H 0.3970 0.2611 0.3921 0.053 Uiso 1 1 calc R . . C87 C 0.4281(5) 0.1538(3) 0.4308(3) 0.0472(15) Uani 1 1 d . . . H87 H 0.3742 0.1363 0.4184 0.057 Uiso 1 1 calc R . . C88 C 0.4931(5) 0.1043(3) 0.4646(3) 0.0488(16) Uani 1 1 d . . . C89 C 0.4763(5) 0.0248(3) 0.4811(4) 0.0573(18) Uani 1 1 d . . . H89 H 0.4270 0.0090 0.4624 0.069 Uiso 1 1 calc R . . C90 C 0.5702(4) 0.1342(4) 0.4824(4) 0.0497(16) Uani 1 1 d . . . H90 H 0.6157 0.1024 0.5058 0.060 Uiso 1 1 calc R . . C91 C 0.5803(4) 0.2074(3) 0.4665(3) 0.0420(14) Uani 1 1 d . . . H91 H 0.6323 0.2266 0.4795 0.050 Uiso 1 1 calc R . . C92 C 0.5317(5) 0.3337(3) 0.4161(3) 0.0443(14) Uani 1 1 d . . . H92B H 0.5445 0.3519 0.4585 0.053 Uiso 1 1 calc R . . H92A H 0.4669 0.3631 0.4087 0.053 Uiso 1 1 calc R . . C93 C 0.6212(4) 0.3471(4) 0.3485(4) 0.0502(16) Uani 1 1 d . . . H93B H 0.6460 0.3942 0.3521 0.060 Uiso 1 1 calc R . . H93A H 0.6790 0.3058 0.3480 0.060 Uiso 1 1 calc R . . C94 C 0.5952(6) 0.3522(5) 0.2790(4) 0.072(2) Uani 1 1 d . . . H94A H 0.5382 0.3939 0.2783 0.086 Uiso 1 1 calc R . . H94B H 0.6563 0.3629 0.2381 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0619(11) 0.0450(10) 0.0448(10) 0.0095(7) -0.0258(8) -0.0225(8) P2 0.0846(16) 0.0541(13) 0.135(2) -0.0042(13) -0.0741(16) 0.0029(10) F1 0.112(4) 0.151(5) 0.053(3) -0.009(3) 0.003(3) -0.006(4) F2 0.183(6) 0.106(4) 0.070(3) 0.020(3) -0.055(3) -0.098(4) F3 0.064(2) 0.070(3) 0.056(2) 0.019(2) -0.021(2) -0.0030(19) F4 0.147(5) 0.103(4) 0.121(4) 0.027(3) -0.085(4) -0.079(4) F5 0.145(5) 0.073(3) 0.095(4) 0.038(3) -0.071(3) -0.030(3) F6 0.085(3) 0.090(3) 0.087(4) 0.011(3) -0.012(3) 0.024(3) F7 0.088(4) 0.085(4) 0.239(8) -0.026(4) -0.093(5) 0.002(3) F8 0.090(4) 0.069(3) 0.225(7) -0.029(4) -0.096(4) 0.001(3) F9 0.195(7) 0.098(4) 0.139(5) 0.008(4) -0.122(5) -0.016(4) F10 0.117(4) 0.060(3) 0.159(5) -0.012(3) -0.083(4) -0.002(3) F11 0.088(4) 0.118(4) 0.138(5) 0.025(4) -0.050(4) -0.016(3) F12 0.081(3) 0.066(3) 0.119(4) 0.006(3) -0.045(3) -0.013(2) O1 0.035(2) 0.038(2) 0.041(2) 0.0079(17) -0.0160(17) -0.0168(16) O2 0.033(2) 0.064(3) 0.046(3) 0.002(2) -0.0064(19) -0.0233(19) O4 0.053(3) 0.074(3) 0.055(3) -0.030(2) -0.027(2) 0.003(2) O5 0.060(3) 0.074(3) 0.046(3) -0.030(2) -0.012(2) -0.019(2) O6 0.044(2) 0.086(3) 0.028(2) -0.013(2) -0.0102(18) 0.012(2) O7 0.034(2) 0.058(3) 0.039(2) 0.0105(19) -0.0083(18) -0.0107(18) O8 0.028(2) 0.088(3) 0.034(2) 0.013(2) -0.0092(17) -0.011(2) O9 0.029(2) 0.052(3) 0.045(2) 0.0141(19) -0.0099(18) -0.0075(17) O10 0.0224(18) 0.038(2) 0.038(2) 0.0091(16) -0.0132(16) -0.0094(15) O11 0.060(3) 0.038(2) 0.0219(19) -0.0002(16) -0.0142(17) -0.0116(18) O12 0.064(3) 0.055(3) 0.029(2) -0.0031(19) -0.017(2) -0.017(2) O13 0.033(2) 0.079(3) 0.029(2) -0.002(2) -0.0089(17) -0.0148(19) O14 0.028(2) 0.096(4) 0.053(3) 0.026(3) -0.011(2) -0.013(2) O15 0.027(2) 0.068(3) 0.068(3) 0.037(2) -0.020(2) -0.0134(19) O16 0.030(2) 0.048(2) 0.047(2) 0.0132(19) -0.0172(18) -0.0193(17) O17 0.031(2) 0.049(2) 0.036(2) -0.0046(18) -0.0076(16) -0.0184(17) O18 0.027(2) 0.043(2) 0.039(2) -0.0011(17) -0.0061(17) -0.0054(16) O19 0.035(2) 0.051(2) 0.029(2) -0.0098(17) -0.0043(16) -0.0145(17) O20 0.039(2) 0.039(2) 0.032(2) -0.0077(17) -0.0132(17) -0.0062(16) O21 0.060(3) 0.077(4) 0.074(3) -0.027(3) -0.006(3) -0.022(3) O22 0.086(4) 0.115(5) 0.084(4) -0.015(4) -0.024(3) -0.018(4) N1 0.032(3) 0.060(3) 0.037(3) -0.017(2) -0.010(2) 0.002(2) N2 0.030(3) 0.042(3) 0.039(3) -0.006(2) -0.004(2) -0.007(2) C1 0.031(3) 0.040(3) 0.028(3) -0.011(2) -0.014(2) -0.006(2) C2 0.028(3) 0.039(3) 0.024(3) 0.000(2) -0.008(2) -0.010(2) C3 0.031(3) 0.031(3) 0.029(3) -0.002(2) -0.007(2) -0.004(2) C4 0.023(2) 0.030(3) 0.020(2) -0.003(2) -0.005(2) -0.0042(19) C5 0.017(2) 0.036(3) 0.024(3) 0.000(2) -0.0041(19) -0.0064(19) C6 0.024(3) 0.032(3) 0.027(3) -0.002(2) -0.009(2) -0.009(2) C7 0.031(3) 0.032(3) 0.021(2) -0.004(2) -0.009(2) -0.005(2) C8 0.036(3) 0.036(3) 0.028(3) -0.007(2) -0.010(2) -0.003(2) C9 0.027(3) 0.044(3) 0.020(3) -0.006(2) -0.010(2) -0.006(2) C10 0.028(3) 0.043(3) 0.028(3) -0.007(2) -0.008(2) 0.002(2) C11 0.025(3) 0.065(4) 0.030(3) -0.012(3) -0.003(2) 0.000(3) C12 0.032(3) 0.062(4) 0.025(3) -0.002(3) -0.004(2) -0.017(3) C13 0.024(3) 0.046(3) 0.026(3) 0.002(2) -0.008(2) -0.011(2) C14 0.023(3) 0.038(3) 0.020(2) -0.005(2) -0.009(2) -0.005(2) C15 0.027(3) 0.032(3) 0.021(3) 0.003(2) -0.009(2) -0.006(2) C16 0.039(3) 0.036(3) 0.031(3) 0.002(2) -0.014(2) -0.016(2) C17 0.020(2) 0.035(3) 0.016(2) -0.003(2) -0.0018(19) -0.0060(19) C18 0.023(3) 0.033(3) 0.024(3) 0.002(2) -0.004(2) -0.007(2) C19 0.019(2) 0.035(3) 0.021(2) 0.004(2) -0.0023(19) -0.007(2) C20 0.022(3) 0.040(3) 0.023(3) 0.003(2) -0.003(2) -0.016(2) C21 0.030(3) 0.030(3) 0.018(2) 0.003(2) -0.002(2) -0.007(2) C22 0.022(2) 0.035(3) 0.017(2) 0.001(2) -0.0026(19) -0.011(2) C23 0.034(3) 0.036(3) 0.028(3) 0.000(2) -0.006(2) -0.014(2) C24 0.047(3) 0.041(3) 0.043(3) 0.001(3) -0.012(3) -0.023(3) C25 0.045(4) 0.076(5) 0.065(5) 0.016(4) -0.015(3) -0.020(3) C26 0.041(4) 0.089(6) 0.070(5) 0.026(4) -0.002(4) -0.001(4) O3 0.043(4) 0.048(4) 0.044(4) -0.001(3) -0.004(3) -0.017(3) C27 0.048(6) 0.052(5) 0.053(5) -0.001(4) -0.003(4) -0.018(4) O3' 0.042(6) 0.066(7) 0.044(7) 0.007(6) -0.010(5) -0.001(5) C27' 0.045(7) 0.048(7) 0.050(8) -0.004(6) -0.019(6) -0.012(6) C28 0.076(5) 0.042(4) 0.043(4) -0.003(3) -0.022(3) -0.013(3) C29 0.071(5) 0.077(5) 0.110(7) -0.051(5) -0.055(5) 0.021(4) C30 0.086(5) 0.050(4) 0.092(6) -0.029(4) -0.055(5) 0.006(4) C31 0.030(3) 0.051(4) 0.039(3) -0.020(3) -0.004(2) -0.005(2) C32 0.031(3) 0.038(3) 0.037(3) -0.007(2) -0.006(2) -0.010(2) C33 0.019(3) 0.046(3) 0.028(3) -0.004(2) -0.003(2) -0.008(2) C34 0.024(3) 0.034(3) 0.024(3) -0.004(2) -0.008(2) -0.008(2) C35 0.027(3) 0.039(3) 0.027(3) 0.002(2) -0.005(2) -0.002(2) C36 0.022(3) 0.075(4) 0.021(3) -0.014(3) -0.004(2) 0.001(3) C37 0.037(3) 0.061(4) 0.043(4) 0.007(3) -0.012(3) -0.013(3) C38 0.054(4) 0.092(5) 0.043(4) 0.014(4) -0.027(3) -0.035(4) C39 0.043(4) 0.049(4) 0.046(4) 0.006(3) 0.000(3) 0.003(3) C40 0.037(4) 0.079(5) 0.049(4) 0.017(4) -0.003(3) -0.001(3) C41 0.032(3) 0.080(5) 0.043(4) 0.016(3) -0.016(3) -0.017(3) C42 0.034(3) 0.066(4) 0.037(3) 0.003(3) -0.012(3) -0.016(3) C43 0.029(3) 0.056(4) 0.036(3) 0.018(3) -0.004(2) -0.005(3) C44 0.026(3) 0.040(3) 0.035(3) 0.014(2) -0.009(2) -0.012(2) C45 0.025(3) 0.036(3) 0.028(3) 0.001(2) -0.007(2) -0.008(2) C46 0.032(3) 0.037(3) 0.047(4) 0.005(3) -0.011(3) -0.011(2) C47 0.021(2) 0.042(3) 0.024(3) -0.004(2) -0.007(2) -0.011(2) C48 0.031(3) 0.045(3) 0.027(3) 0.001(2) -0.010(2) -0.019(2) C49 0.028(3) 0.059(4) 0.018(3) -0.004(2) -0.001(2) -0.021(2) C50 0.020(3) 0.062(4) 0.029(3) -0.016(3) -0.003(2) -0.003(2) C51 0.028(3) 0.048(3) 0.028(3) -0.009(2) -0.012(2) -0.008(2) C52 0.021(2) 0.043(3) 0.015(2) -0.003(2) -0.0056(19) -0.007(2) C53 0.023(3) 0.033(3) 0.023(3) -0.002(2) -0.011(2) -0.002(2) C54 0.032(3) 0.038(3) 0.026(3) 0.001(2) -0.009(2) -0.005(2) C55 0.022(3) 0.039(3) 0.023(3) -0.005(2) -0.005(2) -0.007(2) C56 0.021(2) 0.038(3) 0.019(2) 0.002(2) -0.0033(19) -0.006(2) C57 0.022(3) 0.040(3) 0.027(3) 0.007(2) -0.003(2) -0.005(2) C58 0.023(3) 0.053(4) 0.031(3) 0.008(3) -0.013(2) -0.007(2) C59 0.027(3) 0.043(3) 0.026(3) 0.003(2) -0.003(2) -0.016(2) C60 0.028(3) 0.031(3) 0.020(2) 0.004(2) -0.004(2) -0.008(2) C61 0.043(4) 0.084(5) 0.063(5) 0.013(4) -0.012(3) -0.009(3) C62 0.026(3) 0.127(7) 0.043(4) 0.040(4) -0.012(3) -0.018(4) C63 0.036(3) 0.093(5) 0.041(4) -0.008(4) -0.009(3) -0.019(3) C64 0.030(3) 0.089(5) 0.033(3) 0.000(3) -0.011(3) -0.017(3) C65 0.033(3) 0.104(6) 0.027(3) 0.001(3) -0.008(3) -0.016(3) C66 0.047(4) 0.060(4) 0.046(4) -0.009(3) -0.008(3) 0.001(3) C67 0.100(6) 0.062(5) 0.036(4) 0.005(3) -0.020(4) -0.035(4) C68 0.108(6) 0.050(4) 0.032(4) -0.003(3) -0.008(4) -0.017(4) C69 0.041(3) 0.031(3) 0.036(3) -0.004(2) -0.019(3) -0.002(2) C70 0.041(3) 0.036(3) 0.037(3) -0.008(2) -0.015(3) -0.006(2) C71 0.047(3) 0.054(4) 0.029(3) -0.006(3) -0.011(3) -0.017(3) C72 0.057(4) 0.059(4) 0.035(3) -0.002(3) -0.011(3) 0.012(3) C73 0.031(3) 0.054(4) 0.044(3) 0.009(3) -0.019(3) -0.007(3) C74 0.038(3) 0.059(4) 0.038(3) 0.000(3) -0.014(3) -0.023(3) C75 0.037(3) 0.047(3) 0.037(3) -0.010(3) -0.002(3) -0.017(3) C76 0.026(3) 0.048(4) 0.043(3) -0.003(3) -0.007(2) -0.013(2) C77 0.028(3) 0.081(5) 0.039(3) -0.014(3) -0.009(3) 0.000(3) C78 0.028(3) 0.070(5) 0.041(3) -0.009(3) -0.010(3) -0.013(3) C79 0.024(3) 0.063(4) 0.032(3) -0.011(3) 0.000(2) -0.012(3) C80 0.030(3) 0.072(5) 0.038(3) -0.013(3) -0.006(2) -0.020(3) C81 0.030(3) 0.059(4) 0.043(3) -0.006(3) -0.011(3) -0.008(3) C82 0.027(3) 0.053(4) 0.049(4) -0.003(3) -0.016(3) -0.005(2) C83 0.051(4) 0.050(4) 0.055(4) -0.018(3) -0.022(3) 0.007(3) C84 0.041(4) 0.047(4) 0.062(4) -0.007(3) -0.016(3) -0.009(3) C85 0.039(4) 0.059(4) 0.061(4) -0.011(3) -0.007(3) -0.003(3) C86 0.038(3) 0.046(4) 0.045(4) -0.006(3) -0.006(3) -0.007(3) C87 0.038(3) 0.047(4) 0.057(4) -0.001(3) -0.011(3) -0.014(3) C88 0.047(4) 0.043(4) 0.049(4) -0.004(3) 0.004(3) -0.017(3) C89 0.047(4) 0.046(4) 0.067(5) 0.006(3) 0.001(3) -0.014(3) C90 0.033(3) 0.050(4) 0.057(4) 0.010(3) -0.003(3) -0.008(3) C91 0.034(3) 0.047(4) 0.044(3) 0.004(3) -0.010(3) -0.008(3) C92 0.044(3) 0.035(3) 0.054(4) -0.009(3) -0.010(3) -0.010(3) C93 0.034(3) 0.045(4) 0.071(5) -0.004(3) -0.013(3) -0.010(3) C94 0.052(4) 0.091(6) 0.071(5) -0.013(4) 0.000(4) -0.035(4) _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 P1 F1 1.546(5) . ? P1 F4 1.551(4) . ? P1 F2 1.564(4) . ? P1 F5 1.580(4) . ? P1 F3 1.585(4) . ? P1 F6 1.591(5) . ? P2 F9 1.540(6) . ? P2 F8 1.565(5) . ? P2 F10 1.580(5) . ? P2 F7 1.593(6) . ? P2 F12 1.594(5) . ? P2 F11 1.603(6) . ? O1 C20 1.375(6) . ? O1 C23 1.431(6) . ? O2 C24 1.421(7) . ? O2 C25 1.439(7) . ? O4 C29 1.409(8) . ? O4 C28 1.415(7) . ? O5 C31 1.377(6) . ? O5 C30 1.421(8) . ? O6 C36 1.384(6) . ? O6 C37 1.401(7) . ? O7 C39 1.418(7) . ? O7 C38 1.423(7) . ? O8 C41 1.419(7) . ? O8 C40 1.420(7) . ? O9 C42 1.426(7) . ? O9 C43 1.436(6) . ? O10 C19 1.369(6) . ? O10 C44 1.417(6) . ? O11 C2 1.375(6) . ? O11 C68 1.449(7) . ? O12 C66 1.412(7) . ? O12 C67 1.416(7) . ? O13 C64 1.405(7) . ? O13 C65 1.407(7) . ? O14 C63 1.417(8) . ? O14 C62 1.421(7) . ? O15 C61 1.351(8) . ? O15 C58 1.375(6) . ? O16 C59 1.379(6) . ? O16 C76 1.423(7) . ? O17 C74 1.414(6) . ? O17 C75 1.421(6) . ? O18 C72 1.406(7) . ? O18 C73 1.433(6) . ? O19 C70 1.408(6) . ? O19 C71 1.418(6) . ? O20 C1 1.392(6) . ? O20 C69 1.416(6) . ? O21 C85 1.403(8) . ? O21 H21 0.8199 . ? O22 C94 1.389(9) . ? O22 H22 0.8201 . ? N1 C82 1.337(7) . ? N1 C77 1.355(7) . ? N1 C83 1.492(8) . ? N2 C91 1.346(7) . ? N2 C86 1.350(7) . ? N2 C92 1.486(7) . ? C1 C6 1.396(7) . ? C1 C2 1.404(7) . ? C2 C3 1.379(7) . ? C3 C4 1.394(7) . ? C3 H3 0.9500 . ? C4 C5 1.385(7) . ? C4 C7 1.538(6) . ? C5 C6 1.389(7) . ? C5 C15 1.537(6) . ? C6 H6 0.9500 . ? C7 C8 1.514(7) . ? C7 C22 1.547(6) . ? C7 C9 1.551(7) . ? C8 H8A 0.9800 . ? C8 H8C 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.385(7) . ? C9 C14 1.390(7) . ? C10 C11 1.402(8) . ? C10 H10 0.9500 . ? C11 C12 1.376(8) . ? C11 H11 0.9500 . ? C12 C13 1.385(7) . ? C12 H12 0.9500 . ? C13 C14 1.390(7) . ? C13 H13 0.9500 . ? C14 C15 1.537(7) . ? C15 C16 1.512(7) . ? C15 C17 1.548(6) . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 H16A 0.9800 . ? C17 C22 1.387(7) . ? C17 C18 1.387(7) . ? C18 C19 1.395(7) . ? C18 H18 0.9500 . ? C19 C20 1.398(7) . ? C20 C21 1.409(7) . ? C21 C22 1.398(7) . ? C21 H21A 0.9500 . ? C23 C24 1.492(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24B 0.9900 . ? C24 H24A 0.9900 . ? C25 C26 1.444(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O3' 1.424(9) . ? C26 O3 1.452(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O3 C27 1.413(8) . ? C27 C28 1.519(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? O3' C27' 1.426(10) . ? C27' C28 1.542(9) . ? C27' H27C 0.9900 . ? C27' H27D 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.521(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.387(8) . ? C31 C36 1.396(8) . ? C32 C33 1.392(7) . ? C32 H32 0.9500 . ? C33 C34 1.390(7) . ? C33 C45 1.539(7) . ? C34 C35 1.396(7) . ? C34 C53 1.541(7) . ? C35 C36 1.381(8) . ? C35 H35 0.9500 . ? C37 C38 1.483(8) . ? C37 H37B 0.9900 . ? C37 H37A 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.491(9) . ? C39 H39B 0.9900 . ? C39 H39A 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.506(8) . ? C41 H41B 0.9900 . ? C41 H41A 0.9900 . ? C42 H42B 0.9900 . ? C42 H42A 0.9900 . ? C43 C44 1.505(7) . ? C43 H43B 0.9900 . ? C43 H43A 0.9900 . ? C44 H44B 0.9900 . ? C44 H44A 0.9900 . ? C45 C46 1.508(7) . ? C45 C56 1.539(7) . ? C45 C47 1.544(7) . ? C46 H46A 0.9800 . ? C46 H46C 0.9800 . ? C46 H46B 0.9800 . ? C47 C48 1.385(7) . ? C47 C52 1.385(7) . ? C48 C49 1.385(7) . ? C48 H48 0.9500 . ? C49 C50 1.386(8) . ? C49 H49 0.9500 . ? C50 C51 1.401(7) . ? C50 H50 0.9500 . ? C51 C52 1.390(7) . ? C51 H51 0.9500 . ? C52 C53 1.531(6) . ? C53 C54 1.516(7) . ? C53 C55 1.549(6) . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C54 H54A 0.9800 . ? C55 C56 1.382(7) . ? C55 C60 1.394(7) . ? C56 C57 1.395(7) . ? C57 C58 1.383(7) . ? C57 H57 0.9500 . ? C58 C59 1.407(8) . ? C59 C60 1.396(7) . ? C60 H60 0.9500 . ? C61 C62 1.528(9) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62B 0.9900 . ? C62 H62A 0.9900 . ? C63 C64 1.504(8) . ? C63 H63B 0.9900 . ? C63 H63A 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.494(9) . ? C65 H65B 0.9900 . ? C65 H65A 0.9900 . ? C66 H66B 0.9900 . ? C66 H66A 0.9900 . ? C67 C68 1.447(9) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.511(7) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70B 0.9900 . ? C70 H70A 0.9900 . ? C71 C72 1.498(8) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.497(8) . ? C73 H73B 0.9900 . ? C73 H73A 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.515(7) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76B 0.9900 . ? C76 H76A 0.9900 . ? C77 C78 1.359(9) . ? C77 H77 0.9500 . ? C78 C79 1.386(8) . ? C78 H78 0.9500 . ? C79 C81 1.408(7) . ? C79 C80 1.469(8) . ? C80 C80 1.338(12) 2_665 ? C80 H80 0.9500 . ? C81 C82 1.361(8) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.507(9) . ? C83 H83B 0.9900 . ? C83 H83A 0.9900 . ? C84 C85 1.482(9) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C87 1.372(8) . ? C86 H86 0.9500 . ? C87 C88 1.395(9) . ? C87 H87 0.9500 . ? C88 C90 1.406(9) . ? C88 C89 1.484(8) . ? C89 C89 1.295(13) 2_656 ? C89 H89 0.9500 . ? C90 C91 1.349(8) . ? C90 H90 0.9500 . ? C91 H91 0.9500 . ? C92 C93 1.524(8) . ? C92 H92B 0.9900 . ? C92 H92A 0.9900 . ? C93 C94 1.473(10) . ? C93 H93B 0.9900 . ? C93 H93A 0.9900 . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? 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 F1 P1 F4 92.6(3) . . ? F1 P1 F2 90.8(3) . . ? F4 P1 F2 176.6(4) . . ? F1 P1 F5 88.8(3) . . ? F4 P1 F5 90.4(3) . . ? F2 P1 F5 89.4(3) . . ? F1 P1 F3 92.0(3) . . ? F4 P1 F3 90.9(3) . . ? F2 P1 F3 89.2(3) . . ? F5 P1 F3 178.4(3) . . ? F1 P1 F6 179.6(3) . . ? F4 P1 F6 87.8(3) . . ? F2 P1 F6 88.8(3) . . ? F5 P1 F6 91.0(3) . . ? F3 P1 F6 88.1(2) . . ? F9 P2 F8 91.5(4) . . ? F9 P2 F10 91.3(3) . . ? F8 P2 F10 177.2(4) . . ? F9 P2 F7 89.8(4) . . ? F8 P2 F7 90.6(3) . . ? F10 P2 F7 89.5(3) . . ? F9 P2 F12 92.9(4) . . ? F8 P2 F12 90.6(3) . . ? F10 P2 F12 89.1(3) . . ? F7 P2 F12 177.0(4) . . ? F9 P2 F11 178.3(4) . . ? F8 P2 F11 87.9(4) . . ? F10 P2 F11 89.3(3) . . ? F7 P2 F11 88.6(4) . . ? F12 P2 F11 88.7(3) . . ? C20 O1 C23 119.2(4) . . ? C24 O2 C25 112.3(5) . . ? C29 O4 C28 112.0(5) . . ? C31 O5 C30 119.9(5) . . ? C36 O6 C37 117.8(4) . . ? C39 O7 C38 112.6(5) . . ? C41 O8 C40 114.1(5) . . ? C42 O9 C43 113.7(4) . . ? C19 O10 C44 117.3(4) . . ? C2 O11 C68 119.4(4) . . ? C66 O12 C67 113.7(5) . . ? C64 O13 C65 111.8(4) . . ? C63 O14 C62 114.5(6) . . ? C61 O15 C58 120.3(5) . . ? C59 O16 C76 118.0(4) . . ? C74 O17 C75 111.2(4) . . ? C72 O18 C73 111.0(4) . . ? C70 O19 C71 113.9(4) . . ? C1 O20 C69 117.6(4) . . ? C85 O21 H21 109.5 . . ? C94 O22 H22 108.7 . . ? C82 N1 C77 120.2(6) . . ? C82 N1 C83 118.9(5) . . ? C77 N1 C83 120.9(5) . . ? C91 N2 C86 120.5(5) . . ? C91 N2 C92 119.1(5) . . ? C86 N2 C92 120.4(5) . . ? O20 C1 C6 123.9(5) . . ? O20 C1 C2 115.2(4) . . ? C6 C1 C2 120.9(5) . . ? O11 C2 C3 125.4(5) . . ? O11 C2 C1 115.6(4) . . ? C3 C2 C1 118.9(5) . . ? C2 C3 C4 120.2(5) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.8(4) . . ? C5 C4 C7 114.9(4) . . ? C3 C4 C7 124.3(4) . . ? C4 C5 C6 119.8(5) . . ? C4 C5 C15 114.3(4) . . ? C6 C5 C15 125.9(5) . . ? C5 C6 C1 119.3(5) . . ? C5 C6 H6 120.4 . . ? C1 C6 H6 120.4 . . ? C8 C7 C4 115.0(4) . . ? C8 C7 C22 114.5(4) . . ? C4 C7 C22 103.6(4) . . ? C8 C7 C9 114.2(4) . . ? C4 C7 C9 104.6(4) . . ? C22 C7 C9 103.5(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? C10 C9 C14 120.4(5) . . ? C10 C9 C7 125.4(5) . . ? C14 C9 C7 114.1(4) . . ? C9 C10 C11 119.0(5) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 119.9(5) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.4(5) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C14 118.7(5) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C13 C14 C9 120.5(5) . . ? C13 C14 C15 124.8(5) . . ? C9 C14 C15 114.6(4) . . ? C16 C15 C14 114.0(4) . . ? C16 C15 C5 114.0(4) . . ? C14 C15 C5 104.9(4) . . ? C16 C15 C17 114.9(4) . . ? C14 C15 C17 103.1(4) . . ? C5 C15 C17 104.7(4) . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? C22 C17 C18 120.9(4) . . ? C22 C17 C15 114.2(4) . . ? C18 C17 C15 124.9(4) . . ? C17 C18 C19 119.9(5) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? O10 C19 C18 125.1(4) . . ? O10 C19 C20 115.4(4) . . ? C18 C19 C20 119.5(4) . . ? O1 C20 C19 115.1(4) . . ? O1 C20 C21 124.2(5) . . ? C19 C20 C21 120.6(4) . . ? C22 C21 C20 118.8(5) . . ? C22 C21 H21A 120.6 . . ? C20 C21 H21A 120.6 . . ? C17 C22 C21 120.2(4) . . ? C17 C22 C7 114.6(4) . . ? C21 C22 C7 125.2(4) . . ? O1 C23 C24 106.4(4) . . ? O1 C23 H23A 110.5 . . ? C24 C23 H23A 110.5 . . ? O1 C23 H23B 110.5 . . ? C24 C23 H23B 110.5 . . ? H23A C23 H23B 108.6 . . ? O2 C24 C23 109.2(4) . . ? O2 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? O2 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? H24B C24 H24A 108.3 . . ? O2 C25 C26 110.2(6) . . ? O2 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? O2 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? O3' C26 C25 123.4(9) . . ? O3' C26 O3 28.1(7) . . ? C25 C26 O3 105.7(6) . . ? O3' C26 H26A 115.9 . . ? C25 C26 H26A 110.6 . . ? O3 C26 H26A 110.6 . . ? O3' C26 H26B 83.3 . . ? C25 C26 H26B 110.6 . . ? O3 C26 H26B 110.6 . . ? H26A C26 H26B 108.7 . . ? C27 O3 C26 106.5(6) . . ? O3 C27 C28 108.1(7) . . ? O3 C27 H27A 110.1 . . ? C28 C27 H27A 110.1 . . ? O3 C27 H27B 110.1 . . ? C28 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? C26 O3' C27' 107.8(9) . . ? O3' C27' C28 105.9(9) . . ? O3' C27' H27C 110.6 . . ? C28 C27' H27C 110.6 . . ? O3' C27' H27D 110.6 . . ? C28 C27' H27D 110.6 . . ? H27C C27' H27D 108.7 . . ? O4 C28 C27 103.6(6) . . ? O4 C28 C27' 125.6(9) . . ? C27 C28 C27' 30.7(6) . . ? O4 C28 H28A 111.0 . . ? C27 C28 H28A 111.0 . . ? C27' C28 H28A 82.2 . . ? O4 C28 H28B 111.0 . . ? C27 C28 H28B 111.0 . . ? C27' C28 H28B 113.4 . . ? H28A C28 H28B 109.0 . . ? O4 C29 C30 109.0(6) . . ? O4 C29 H29A 109.9 . . ? C30 C29 H29A 109.9 . . ? O4 C29 H29B 109.9 . . ? C30 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? O5 C30 C29 105.1(7) . . ? O5 C30 H30A 110.7 . . ? C29 C30 H30A 110.7 . . ? O5 C30 H30B 110.7 . . ? C29 C30 H30B 110.7 . . ? H30A C30 H30B 108.8 . . ? O5 C31 C32 126.3(6) . . ? O5 C31 C36 114.0(5) . . ? C32 C31 C36 119.8(5) . . ? C31 C32 C33 119.7(5) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C34 C33 C32 120.3(5) . . ? C34 C33 C45 113.5(4) . . ? C32 C33 C45 126.2(5) . . ? C33 C34 C35 120.1(5) . . ? C33 C34 C53 115.2(4) . . ? C35 C34 C53 124.7(5) . . ? C36 C35 C34 119.3(5) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 O6 121.6(6) . . ? C35 C36 C31 120.8(5) . . ? O6 C36 C31 117.4(5) . . ? O6 C37 C38 108.2(5) . . ? O6 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? O6 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? H37B C37 H37A 108.4 . . ? O7 C38 C37 112.8(5) . . ? O7 C38 H38A 109.0 . . ? C37 C38 H38A 109.0 . . ? O7 C38 H38B 109.0 . . ? C37 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? O7 C39 C40 111.5(6) . . ? O7 C39 H39B 109.3 . . ? C40 C39 H39B 109.3 . . ? O7 C39 H39A 109.3 . . ? C40 C39 H39A 109.3 . . ? H39B C39 H39A 108.0 . . ? O8 C40 C39 108.3(5) . . ? O8 C40 H40A 110.0 . . ? C39 C40 H40A 110.0 . . ? O8 C40 H40B 110.0 . . ? C39 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? O8 C41 C42 108.9(4) . . ? O8 C41 H41B 109.9 . . ? C42 C41 H41B 109.9 . . ? O8 C41 H41A 109.9 . . ? C42 C41 H41A 109.9 . . ? H41B C41 H41A 108.3 . . ? O9 C42 C41 107.6(5) . . ? O9 C42 H42B 110.2 . . ? C41 C42 H42B 110.2 . . ? O9 C42 H42A 110.2 . . ? C41 C42 H42A 110.2 . . ? H42B C42 H42A 108.5 . . ? O9 C43 C44 111.5(5) . . ? O9 C43 H43B 109.3 . . ? C44 C43 H43B 109.3 . . ? O9 C43 H43A 109.3 . . ? C44 C43 H43A 109.3 . . ? H43B C43 H43A 108.0 . . ? O10 C44 C43 108.4(4) . . ? O10 C44 H44B 110.0 . . ? C43 C44 H44B 110.0 . . ? O10 C44 H44A 110.0 . . ? C43 C44 H44A 110.0 . . ? H44B C44 H44A 108.4 . . ? C46 C45 C33 113.7(4) . . ? C46 C45 C56 114.6(4) . . ? C33 C45 C56 104.8(4) . . ? C46 C45 C47 114.6(4) . . ? C33 C45 C47 105.1(4) . . ? C56 C45 C47 102.8(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? H46C C46 H46B 109.5 . . ? C48 C47 C52 120.4(5) . . ? C48 C47 C45 125.2(5) . . ? C52 C47 C45 114.4(4) . . ? C47 C48 C49 120.0(5) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C48 C49 C50 119.9(5) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C49 C50 C51 120.4(5) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C52 C51 C50 119.2(5) . . ? C52 C51 H51 120.4 . . ? C50 C51 H51 120.4 . . ? C47 C52 C51 120.1(5) . . ? C47 C52 C53 114.6(4) . . ? C51 C52 C53 125.2(5) . . ? C54 C53 C52 115.4(4) . . ? C54 C53 C34 113.8(4) . . ? C52 C53 C34 105.2(4) . . ? C54 C53 C55 114.4(4) . . ? C52 C53 C55 103.2(4) . . ? C34 C53 C55 103.3(4) . . ? C53 C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C54 H54A 109.5 . . ? H54B C54 H54A 109.5 . . ? H54C C54 H54A 109.5 . . ? C56 C55 C60 121.2(5) . . ? C56 C55 C53 114.2(4) . . ? C60 C55 C53 124.6(5) . . ? C55 C56 C57 120.1(5) . . ? C55 C56 C45 114.7(4) . . ? C57 C56 C45 125.1(5) . . ? C58 C57 C56 119.7(5) . . ? C58 C57 H57 120.2 . . ? C56 C57 H57 120.2 . . ? O15 C58 C57 125.3(5) . . ? O15 C58 C59 114.7(5) . . ? C57 C58 C59 120.0(5) . . ? O16 C59 C60 124.8(5) . . ? O16 C59 C58 114.9(4) . . ? C60 C59 C58 120.3(5) . . ? C55 C60 C59 118.6(5) . . ? C55 C60 H60 120.7 . . ? C59 C60 H60 120.7 . . ? O15 C61 C62 106.5(6) . . ? O15 C61 H61A 110.4 . . ? C62 C61 H61A 110.4 . . ? O15 C61 H61B 110.4 . . ? C62 C61 H61B 110.4 . . ? H61A C61 H61B 108.6 . . ? O14 C62 C61 110.8(5) . . ? O14 C62 H62B 109.5 . . ? C61 C62 H62B 109.5 . . ? O14 C62 H62A 109.5 . . ? C61 C62 H62A 109.5 . . ? H62B C62 H62A 108.1 . . ? O14 C63 C64 108.3(6) . . ? O14 C63 H63B 110.0 . . ? C64 C63 H63B 110.0 . . ? O14 C63 H63A 110.0 . . ? C64 C63 H63A 110.0 . . ? H63B C63 H63A 108.4 . . ? O13 C64 C63 108.8(5) . . ? O13 C64 H64A 109.9 . . ? C63 C64 H64A 109.9 . . ? O13 C64 H64B 109.9 . . ? C63 C64 H64B 109.9 . . ? H64A C64 H64B 108.3 . . ? O13 C65 C66 108.7(5) . . ? O13 C65 H65B 110.0 . . ? C66 C65 H65B 110.0 . . ? O13 C65 H65A 110.0 . . ? C66 C65 H65A 110.0 . . ? H65B C65 H65A 108.3 . . ? O12 C66 C65 108.9(5) . . ? O12 C66 H66B 109.9 . . ? C65 C66 H66B 109.9 . . ? O12 C66 H66A 109.9 . . ? C65 C66 H66A 109.9 . . ? H66B C66 H66A 108.3 . . ? O12 C67 C68 114.5(6) . . ? O12 C67 H67A 108.6 . . ? C68 C67 H67A 108.6 . . ? O12 C67 H67B 108.6 . . ? C68 C67 H67B 108.6 . . ? H67A C67 H67B 107.6 . . ? C67 C68 O11 110.7(6) . . ? C67 C68 H68A 109.5 . . ? O11 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? O11 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? O20 C69 C70 106.9(4) . . ? O20 C69 H69A 110.3 . . ? C70 C69 H69A 110.3 . . ? O20 C69 H69B 110.3 . . ? C70 C69 H69B 110.3 . . ? H69A C69 H69B 108.6 . . ? O19 C70 C69 108.0(4) . . ? O19 C70 H70B 110.1 . . ? C69 C70 H70B 110.1 . . ? O19 C70 H70A 110.1 . . ? C69 C70 H70A 110.1 . . ? H70B C70 H70A 108.4 . . ? O19 C71 C72 113.6(5) . . ? O19 C71 H71A 108.8 . . ? C72 C71 H71A 108.8 . . ? O19 C71 H71B 108.8 . . ? C72 C71 H71B 108.8 . . ? H71A C71 H71B 107.7 . . ? O18 C72 C71 112.7(5) . . ? O18 C72 H72A 109.0 . . ? C71 C72 H72A 109.0 . . ? O18 C72 H72B 109.0 . . ? C71 C72 H72B 109.0 . . ? H72A C72 H72B 107.8 . . ? O18 C73 C74 111.1(5) . . ? O18 C73 H73B 109.4 . . ? C74 C73 H73B 109.4 . . ? O18 C73 H73A 109.4 . . ? C74 C73 H73A 109.4 . . ? H73B C73 H73A 108.0 . . ? O17 C74 C73 110.8(4) . . ? O17 C74 H74A 109.5 . . ? C73 C74 H74A 109.5 . . ? O17 C74 H74B 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 108.1 . . ? O17 C75 C76 109.4(4) . . ? O17 C75 H75A 109.8 . . ? C76 C75 H75A 109.8 . . ? O17 C75 H75B 109.8 . . ? C76 C75 H75B 109.8 . . ? H75A C75 H75B 108.2 . . ? O16 C76 C75 105.9(4) . . ? O16 C76 H76B 110.5 . . ? C75 C76 H76B 110.5 . . ? O16 C76 H76A 110.5 . . ? C75 C76 H76A 110.5 . . ? H76B C76 H76A 108.7 . . ? N1 C77 C78 120.9(6) . . ? N1 C77 H77 119.5 . . ? C78 C77 H77 119.5 . . ? C77 C78 C79 120.1(5) . . ? C77 C78 H78 119.9 . . ? C79 C78 H78 119.9 . . ? C78 C79 C81 117.9(6) . . ? C78 C79 C80 120.1(5) . . ? C81 C79 C80 122.0(5) . . ? C80 C80 C79 126.8(7) 2_665 . ? C80 C80 H80 116.6 2_665 . ? C79 C80 H80 116.6 . . ? C82 C81 C79 119.5(6) . . ? C82 C81 H81 120.2 . . ? C79 C81 H81 120.2 . . ? N1 C82 C81 121.3(5) . . ? N1 C82 H82 119.3 . . ? C81 C82 H82 119.3 . . ? N1 C83 C84 112.9(5) . . ? N1 C83 H83B 109.0 . . ? C84 C83 H83B 109.0 . . ? N1 C83 H83A 109.0 . . ? C84 C83 H83A 109.0 . . ? H83B C83 H83A 107.8 . . ? C85 C84 C83 116.3(5) . . ? C85 C84 H84A 108.2 . . ? C83 C84 H84A 108.2 . . ? C85 C84 H84B 108.2 . . ? C83 C84 H84B 108.2 . . ? H84A C84 H84B 107.4 . . ? O21 C85 C84 112.9(6) . . ? O21 C85 H85A 109.0 . . ? C84 C85 H85A 109.0 . . ? O21 C85 H85B 109.0 . . ? C84 C85 H85B 109.0 . . ? H85A C85 H85B 107.8 . . ? N2 C86 C87 120.6(6) . . ? N2 C86 H86 119.7 . . ? C87 C86 H86 119.7 . . ? C86 C87 C88 120.2(6) . . ? C86 C87 H87 119.9 . . ? C88 C87 H87 119.9 . . ? C87 C88 C90 116.9(6) . . ? C87 C88 C89 119.0(6) . . ? C90 C88 C89 124.0(6) . . ? C89 C89 C88 125.1(9) 2_656 . ? C89 C89 H89 117.5 2_656 . ? C88 C89 H89 117.5 . . ? C91 C90 C88 120.9(6) . . ? C91 C90 H90 119.6 . . ? C88 C90 H90 119.6 . . ? N2 C91 C90 120.9(6) . . ? N2 C91 H91 119.6 . . ? C90 C91 H91 119.6 . . ? N2 C92 C93 112.8(5) . . ? N2 C92 H92B 109.0 . . ? C93 C92 H92B 109.0 . . ? N2 C92 H92A 109.0 . . ? C93 C92 H92A 109.0 . . ? H92B C92 H92A 107.8 . . ? C94 C93 C92 114.5(5) . . ? C94 C93 H93B 108.6 . . ? C92 C93 H93B 108.6 . . ? C94 C93 H93A 108.6 . . ? C92 C93 H93A 108.6 . . ? H93B C93 H93A 107.6 . . ? O22 C94 C93 110.4(7) . . ? O22 C94 H94A 109.6 . . ? C93 C94 H94A 109.6 . . ? O22 C94 H94B 109.6 . . ? C93 C94 H94B 109.6 . . ? H94A C94 H94B 108.1 . . ? 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 C69 O20 C1 C6 7.4(7) . . . . ? C69 O20 C1 C2 -174.2(4) . . . . ? C68 O11 C2 C3 -4.5(8) . . . . ? C68 O11 C2 C1 175.0(5) . . . . ? O20 C1 C2 O11 4.3(6) . . . . ? C6 C1 C2 O11 -177.3(4) . . . . ? O20 C1 C2 C3 -176.2(4) . . . . ? C6 C1 C2 C3 2.3(7) . . . . ? O11 C2 C3 C4 177.7(5) . . . . ? C1 C2 C3 C4 -1.8(7) . . . . ? C2 C3 C4 C5 0.1(7) . . . . ? C2 C3 C4 C7 -177.8(5) . . . . ? C3 C4 C5 C6 1.3(7) . . . . ? C7 C4 C5 C6 179.3(4) . . . . ? C3 C4 C5 C15 -177.0(4) . . . . ? C7 C4 C5 C15 1.0(6) . . . . ? C4 C5 C6 C1 -0.8(7) . . . . ? C15 C5 C6 C1 177.2(4) . . . . ? O20 C1 C6 C5 177.4(4) . . . . ? C2 C1 C6 C5 -1.0(7) . . . . ? C5 C4 C7 C8 179.2(4) . . . . ? C3 C4 C7 C8 -2.9(7) . . . . ? C5 C4 C7 C22 -55.1(5) . . . . ? C3 C4 C7 C22 122.9(5) . . . . ? C5 C4 C7 C9 53.1(5) . . . . ? C3 C4 C7 C9 -129.0(5) . . . . ? C8 C7 C9 C10 0.4(7) . . . . ? C4 C7 C9 C10 127.0(5) . . . . ? C22 C7 C9 C10 -124.8(5) . . . . ? C8 C7 C9 C14 179.4(4) . . . . ? C4 C7 C9 C14 -54.0(5) . . . . ? C22 C7 C9 C14 54.2(5) . . . . ? C14 C9 C10 C11 -1.6(7) . . . . ? C7 C9 C10 C11 177.3(5) . . . . ? C9 C10 C11 C12 0.5(8) . . . . ? C10 C11 C12 C13 1.0(8) . . . . ? C11 C12 C13 C14 -1.4(8) . . . . ? C12 C13 C14 C9 0.2(7) . . . . ? C12 C13 C14 C15 -178.2(4) . . . . ? C10 C9 C14 C13 1.3(7) . . . . ? C7 C9 C14 C13 -177.8(4) . . . . ? C10 C9 C14 C15 179.9(4) . . . . ? C7 C9 C14 C15 0.9(6) . . . . ? C13 C14 C15 C16 -2.6(7) . . . . ? C9 C14 C15 C16 178.8(4) . . . . ? C13 C14 C15 C5 -128.0(5) . . . . ? C9 C14 C15 C5 53.4(5) . . . . ? C13 C14 C15 C17 122.6(5) . . . . ? C9 C14 C15 C17 -55.9(5) . . . . ? C4 C5 C15 C16 179.9(4) . . . . ? C6 C5 C15 C16 1.8(7) . . . . ? C4 C5 C15 C14 -54.6(5) . . . . ? C6 C5 C15 C14 127.2(5) . . . . ? C4 C5 C15 C17 53.5(5) . . . . ? C6 C5 C15 C17 -124.6(5) . . . . ? C16 C15 C17 C22 -179.3(4) . . . . ? C14 C15 C17 C22 56.1(5) . . . . ? C5 C15 C17 C22 -53.4(5) . . . . ? C16 C15 C17 C18 1.5(7) . . . . ? C14 C15 C17 C18 -123.2(5) . . . . ? C5 C15 C17 C18 127.3(5) . . . . ? C22 C17 C18 C19 1.0(7) . . . . ? C15 C17 C18 C19 -179.8(4) . . . . ? C44 O10 C19 C18 8.3(7) . . . . ? C44 O10 C19 C20 -173.4(4) . . . . ? C17 C18 C19 O10 -179.7(4) . . . . ? C17 C18 C19 C20 2.0(7) . . . . ? C23 O1 C20 C19 172.3(4) . . . . ? C23 O1 C20 C21 -8.5(7) . . . . ? O10 C19 C20 O1 -2.6(6) . . . . ? C18 C19 C20 O1 175.8(4) . . . . ? O10 C19 C20 C21 178.2(4) . . . . ? C18 C19 C20 C21 -3.4(7) . . . . ? O1 C20 C21 C22 -177.4(4) . . . . ? C19 C20 C21 C22 1.8(7) . . . . ? C18 C17 C22 C21 -2.7(7) . . . . ? C15 C17 C22 C21 178.0(4) . . . . ? C18 C17 C22 C7 178.2(4) . . . . ? C15 C17 C22 C7 -1.0(6) . . . . ? C20 C21 C22 C17 1.3(7) . . . . ? C20 C21 C22 C7 -179.8(4) . . . . ? C8 C7 C22 C17 -179.0(4) . . . . ? C4 C7 C22 C17 54.9(5) . . . . ? C9 C7 C22 C17 -54.0(5) . . . . ? C8 C7 C22 C21 2.0(7) . . . . ? C4 C7 C22 C21 -124.1(5) . . . . ? C9 C7 C22 C21 126.9(5) . . . . ? C20 O1 C23 C24 174.6(4) . . . . ? C25 O2 C24 C23 155.8(5) . . . . ? O1 C23 C24 O2 -71.2(5) . . . . ? C24 O2 C25 C26 176.2(5) . . . . ? O2 C25 C26 O3' -58.5(12) . . . . ? O2 C25 C26 O3 -82.6(8) . . . . ? O3' C26 O3 C27 35.8(13) . . . . ? C25 C26 O3 C27 169.4(9) . . . . ? C26 O3 C27 C28 165.3(7) . . . . ? C25 C26 O3' C27' -125.5(16) . . . . ? O3 C26 O3' C27' -68.8(17) . . . . ? C26 O3' C27' C28 168.7(11) . . . . ? C29 O4 C28 C27 -85.6(8) . . . . ? C29 O4 C28 C27' -109.3(9) . . . . ? O3 C27 C28 O4 153.5(9) . . . . ? O3 C27 C28 C27' -66.4(15) . . . . ? O3' C27' C28 O4 86.8(18) . . . . ? O3' C27' C28 C27 36.7(11) . . . . ? C28 O4 C29 C30 163.0(6) . . . . ? C31 O5 C30 C29 177.5(5) . . . . ? O4 C29 C30 O5 -72.0(8) . . . . ? C30 O5 C31 C32 10.6(8) . . . . ? C30 O5 C31 C36 -169.9(5) . . . . ? O5 C31 C32 C33 -179.5(5) . . . . ? C36 C31 C32 C33 1.1(8) . . . . ? C31 C32 C33 C34 0.9(7) . . . . ? C31 C32 C33 C45 -176.3(5) . . . . ? C32 C33 C34 C35 -2.0(7) . . . . ? C45 C33 C34 C35 175.5(4) . . . . ? C32 C33 C34 C53 -180.0(4) . . . . ? C45 C33 C34 C53 -2.4(6) . . . . ? C33 C34 C35 C36 1.3(7) . . . . ? C53 C34 C35 C36 179.0(5) . . . . ? C34 C35 C36 O6 -175.7(4) . . . . ? C34 C35 C36 C31 0.7(8) . . . . ? C37 O6 C36 C35 -65.0(7) . . . . ? C37 O6 C36 C31 118.6(6) . . . . ? O5 C31 C36 C35 178.6(5) . . . . ? C32 C31 C36 C35 -1.9(8) . . . . ? O5 C31 C36 O6 -4.9(7) . . . . ? C32 C31 C36 O6 174.6(5) . . . . ? C36 O6 C37 C38 -166.1(5) . . . . ? C39 O7 C38 C37 -98.0(6) . . . . ? O6 C37 C38 O7 -64.9(7) . . . . ? C38 O7 C39 C40 -86.1(6) . . . . ? C41 O8 C40 C39 170.3(5) . . . . ? O7 C39 C40 O8 -67.6(7) . . . . ? C40 O8 C41 C42 169.1(5) . . . . ? C43 O9 C42 C41 -174.1(4) . . . . ? O8 C41 C42 O9 -68.3(6) . . . . ? C42 O9 C43 C44 -94.8(6) . . . . ? C19 O10 C44 C43 177.0(4) . . . . ? O9 C43 C44 O10 67.9(6) . . . . ? C34 C33 C45 C46 -178.8(4) . . . . ? C32 C33 C45 C46 -1.4(7) . . . . ? C34 C33 C45 C56 -52.9(5) . . . . ? C32 C33 C45 C56 124.4(5) . . . . ? C34 C33 C45 C47 55.1(5) . . . . ? C32 C33 C45 C47 -127.6(5) . . . . ? C46 C45 C47 C48 3.2(7) . . . . ? C33 C45 C47 C48 128.8(5) . . . . ? C56 C45 C47 C48 -121.8(5) . . . . ? C46 C45 C47 C52 -179.0(4) . . . . ? C33 C45 C47 C52 -53.5(5) . . . . ? C56 C45 C47 C52 55.9(5) . . . . ? C52 C47 C48 C49 -0.1(7) . . . . ? C45 C47 C48 C49 177.6(4) . . . . ? C47 C48 C49 C50 0.7(7) . . . . ? C48 C49 C50 C51 -0.8(7) . . . . ? C49 C50 C51 C52 0.3(7) . . . . ? C48 C47 C52 C51 -0.5(7) . . . . ? C45 C47 C52 C51 -178.3(4) . . . . ? C48 C47 C52 C53 176.6(4) . . . . ? C45 C47 C52 C53 -1.2(6) . . . . ? C50 C51 C52 C47 0.3(7) . . . . ? C50 C51 C52 C53 -176.4(4) . . . . ? C47 C52 C53 C54 -179.8(4) . . . . ? C51 C52 C53 C54 -2.9(7) . . . . ? C47 C52 C53 C34 53.8(5) . . . . ? C51 C52 C53 C34 -129.3(5) . . . . ? C47 C52 C53 C55 -54.2(5) . . . . ? C51 C52 C53 C55 122.7(5) . . . . ? C33 C34 C53 C54 -179.3(4) . . . . ? C35 C34 C53 C54 2.9(7) . . . . ? C33 C34 C53 C52 -52.0(5) . . . . ? C35 C34 C53 C52 130.2(5) . . . . ? C33 C34 C53 C55 56.0(5) . . . . ? C35 C34 C53 C55 -121.8(5) . . . . ? C54 C53 C55 C56 -178.4(4) . . . . ? C52 C53 C55 C56 55.4(5) . . . . ? C34 C53 C55 C56 -54.1(5) . . . . ? C54 C53 C55 C60 3.3(7) . . . . ? C52 C53 C55 C60 -123.0(5) . . . . ? C34 C53 C55 C60 127.6(5) . . . . ? C60 C55 C56 C57 0.2(7) . . . . ? C53 C55 C56 C57 -178.3(4) . . . . ? C60 C55 C56 C45 178.0(4) . . . . ? C53 C55 C56 C45 -0.5(6) . . . . ? C46 C45 C56 C55 -179.8(4) . . . . ? C33 C45 C56 C55 54.9(5) . . . . ? C47 C45 C56 C55 -54.7(5) . . . . ? C46 C45 C56 C57 -2.1(7) . . . . ? C33 C45 C56 C57 -127.4(5) . . . . ? C47 C45 C56 C57 122.9(5) . . . . ? C55 C56 C57 C58 -0.1(7) . . . . ? C45 C56 C57 C58 -177.6(5) . . . . ? C61 O15 C58 C57 -6.9(9) . . . . ? C61 O15 C58 C59 172.7(6) . . . . ? C56 C57 C58 O15 178.7(5) . . . . ? C56 C57 C58 C59 -0.8(8) . . . . ? C76 O16 C59 C60 9.4(7) . . . . ? C76 O16 C59 C58 -171.5(5) . . . . ? O15 C58 C59 O16 2.8(7) . . . . ? C57 C58 C59 O16 -177.6(5) . . . . ? O15 C58 C59 C60 -178.0(5) . . . . ? C57 C58 C59 C60 1.6(8) . . . . ? C56 C55 C60 C59 0.6(7) . . . . ? C53 C55 C60 C59 178.9(4) . . . . ? O16 C59 C60 C55 177.6(5) . . . . ? C58 C59 C60 C55 -1.4(7) . . . . ? C58 O15 C61 C62 -174.3(5) . . . . ? C63 O14 C62 C61 93.8(7) . . . . ? O15 C61 C62 O14 -64.5(8) . . . . ? C62 O14 C63 C64 173.3(5) . . . . ? C65 O13 C64 C63 -174.2(6) . . . . ? O14 C63 C64 O13 66.1(7) . . . . ? C64 O13 C65 C66 170.8(5) . . . . ? C67 O12 C66 C65 -173.7(5) . . . . ? O13 C65 C66 O12 63.8(7) . . . . ? C66 O12 C67 C68 -87.9(7) . . . . ? O12 C67 C68 O11 -63.9(9) . . . . ? C2 O11 C68 C67 -139.8(6) . . . . ? C1 O20 C69 C70 -178.9(4) . . . . ? C71 O19 C70 C69 -166.2(4) . . . . ? O20 C69 C70 O19 73.8(5) . . . . ? C70 O19 C71 C72 75.7(6) . . . . ? C73 O18 C72 C71 -173.2(5) . . . . ? O19 C71 C72 O18 -105.4(6) . . . . ? C72 O18 C73 C74 162.5(5) . . . . ? C75 O17 C74 C73 177.4(5) . . . . ? O18 C73 C74 O17 80.9(6) . . . . ? C74 O17 C75 C76 -164.0(5) . . . . ? C59 O16 C76 C75 -176.3(4) . . . . ? O17 C75 C76 O16 71.5(6) . . . . ? C82 N1 C77 C78 -0.5(8) . . . . ? C83 N1 C77 C78 -179.5(5) . . . . ? N1 C77 C78 C79 -0.1(9) . . . . ? C77 C78 C79 C81 0.0(8) . . . . ? C77 C78 C79 C80 -178.5(5) . . . . ? C78 C79 C80 C80 175.8(7) . . . 2_665 ? C81 C79 C80 C80 -2.6(11) . . . 2_665 ? C78 C79 C81 C82 0.8(8) . . . . ? C80 C79 C81 C82 179.3(5) . . . . ? C77 N1 C82 C81 1.4(9) . . . . ? C83 N1 C82 C81 -179.6(5) . . . . ? C79 C81 C82 N1 -1.5(9) . . . . ? C82 N1 C83 C84 -76.7(7) . . . . ? C77 N1 C83 C84 102.3(6) . . . . ? N1 C83 C84 C85 -65.3(7) . . . . ? C83 C84 C85 O21 72.4(7) . . . . ? C91 N2 C86 C87 -1.3(8) . . . . ? C92 N2 C86 C87 -179.6(5) . . . . ? N2 C86 C87 C88 -0.1(9) . . . . ? C86 C87 C88 C90 0.9(9) . . . . ? C86 C87 C88 C89 179.7(6) . . . . ? C87 C88 C89 C89 -172.3(8) . . . 2_656 ? C90 C88 C89 C89 6.4(13) . . . 2_656 ? C87 C88 C90 C91 -0.5(9) . . . . ? C89 C88 C90 C91 -179.2(6) . . . . ? C86 N2 C91 C90 1.8(8) . . . . ? C92 N2 C91 C90 -180.0(5) . . . . ? C88 C90 C91 N2 -0.8(9) . . . . ? C91 N2 C92 C93 79.7(7) . . . . ? C86 N2 C92 C93 -102.1(6) . . . . ? N2 C92 C93 C94 82.5(7) . . . . ? C92 C93 C94 O22 -61.4(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O21 H21 O22 0.82 2.00 2.794(8) 161.5 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.000 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.084 # Attachment '- complex 1-3.cif' data_a1-3 _database_code_depnum_ccdc_archive 'CCDC 898290' #TrackingRef '- complex 1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H118 F12 N2 O22 P2' _chemical_formula_weight 1965.88 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.768(3) _cell_length_b 13.623(3) _cell_length_c 14.010(3) _cell_angle_alpha 72.17(3) _cell_angle_beta 88.99(3) _cell_angle_gamma 83.52(3) _cell_volume 2304.6(8) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7583 _cell_measurement_theta_min 1.5272 _cell_measurement_theta_max 27.4750 _exptl_crystal_description bolck _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1034 _exptl_absorpt_coefficient_mu 0.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6796 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007HF + CCD (Saturn724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17391 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0581 _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 -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8092 _reflns_number_gt 6798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _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. DFIX 1.43 0.01 O9 C5 O9 C5' DFIX 1.54 0.01 C5 C4 C5' C4' DFIX 1.43 0.01 C4 O10 C4' O10 DFIX 1.54 0.01 C48 C49 C48 C49' DFIX 1.43 0.01 C49 O11 C49' O11' SIMU 0.01 0.02 1.7 C4 C5 SIMU 0.01 0.02 1.7 C4' C5' SIMU 0.01 0.02 1.7 P1 F1 F2 F3 F4 F5 F6 SIMU 0.01 0.02 1.7 P1' F1' F2' F3' F4' F5' F6' SIMU 0.01 0.02 1.7 C49 O11 SIMU 0.01 0.02 1.7 C49' O11' ISOR 0.01 0.02 C4 C5 ISOR 0.01 0.02 C4' C5' ISOR 0.01 0.02 P1' F1' F2' F3' F4' F5' F6' ISOR 0.01 0.02 P1 F1 F2 F3 F4 F5 F6 ISOR 0.01 0.02 C49 O11 ISOR 0.01 0.02 C49' O11' ISOR 0.005 0.01 C36 O5 C37 C38 ; _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^)+(0.0859P)^2^+4.0834P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8092 _refine_ls_number_parameters 719 _refine_ls_number_restraints 262 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_gt 0.0969 _refine_ls_wR_factor_ref 0.2375 _refine_ls_wR_factor_gt 0.2248 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 0.002 _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 P1 P 0.8057(5) 0.3156(6) 0.2574(4) 0.0652(14) Uani 0.511(8) 1 d PU A 1 F1 F 0.8395(12) 0.3569(13) 0.1426(12) 0.113(5) Uani 0.511(8) 1 d PU A 1 F2 F 0.6875(7) 0.3197(9) 0.2194(8) 0.100(3) Uani 0.511(8) 1 d PU A 1 F3 F 0.7816(6) 0.4338(8) 0.2557(7) 0.075(2) Uani 0.511(8) 1 d PU A 1 F4 F 0.9215(7) 0.3154(8) 0.2919(11) 0.102(3) Uani 0.511(8) 1 d PU A 1 F5 F 0.8299(8) 0.1957(7) 0.2586(8) 0.090(3) Uani 0.511(8) 1 d PU A 1 F6 F 0.7720(7) 0.2783(7) 0.3689(6) 0.089(3) Uani 0.511(8) 1 d PU A 1 P1' P 0.8240(4) 0.2731(5) 0.2475(4) 0.0509(12) Uani 0.489(8) 1 d PU A 2 F1' F 0.7886(10) 0.3492(11) 0.1429(10) 0.086(4) Uani 0.489(8) 1 d PU A 2 F2' F 0.7093(7) 0.2439(11) 0.2724(9) 0.110(4) Uani 0.489(8) 1 d PU A 2 F3' F 0.7982(7) 0.3666(10) 0.2984(9) 0.091(3) Uani 0.489(8) 1 d PU A 2 F4' F 0.9398(6) 0.3042(7) 0.2322(8) 0.072(3) Uani 0.489(8) 1 d PU A 2 F5' F 0.8527(8) 0.1822(7) 0.2034(8) 0.093(3) Uani 0.489(8) 1 d PU A 2 F6' F 0.8605(7) 0.1984(7) 0.3549(6) 0.095(3) Uani 0.489(8) 1 d PU A 2 O1 O 0.2256(3) 0.1698(3) -0.0709(2) 0.0453(8) Uani 1 1 d . B . O2 O 0.2726(3) 0.0776(2) -0.2263(2) 0.0501(8) Uani 1 1 d . . . O3 O 0.4437(2) 0.4590(2) 0.3606(2) 0.0389(7) Uani 1 1 d . B . O4 O 0.5258(3) 0.6539(2) 0.2800(3) 0.0499(9) Uani 1 1 d . . . O6 O 0.2605(2) 0.4483(2) 0.4371(2) 0.0392(7) Uani 1 1 d . . . O7 O 0.1017(3) 0.6196(2) 0.4324(2) 0.0475(8) Uani 1 1 d . . . O8 O -0.0552(3) 0.8149(2) 0.3600(3) 0.0526(9) Uani 1 1 d . . . O9 O 0.0467(2) 0.1600(3) 0.0215(2) 0.0480(8) Uani 1 1 d D . . O10 O -0.1674(3) 0.1657(3) -0.0485(3) 0.0654(11) Uani 1 1 d D . . N1 N 0.1166(3) 0.5205(3) 0.2037(3) 0.0458(10) Uani 1 1 d . . . C1 C 0.2153(4) 0.0697(4) -0.3095(4) 0.0476(12) Uani 1 1 d . . . H1A H 0.2354 0.0000 -0.3168 0.057 Uiso 1 1 calc R . . H1B H 0.2369 0.1214 -0.3710 0.057 Uiso 1 1 calc R . . C2 C 0.2875(4) 0.1802(4) -0.2324(3) 0.0477(12) Uani 1 1 d . . . H2A H 0.2216 0.2268 -0.2557 0.057 Uiso 1 1 calc R . . H2B H 0.3438 0.2047 -0.2804 0.057 Uiso 1 1 calc R . . C3 C 0.3183(4) 0.1800(4) -0.1285(3) 0.0484(12) Uani 1 1 d . . . H3A H 0.3728 0.1214 -0.0982 0.058 Uiso 1 1 calc R . . H3B H 0.3469 0.2456 -0.1318 0.058 Uiso 1 1 calc R . . C4 C -0.0813(7) 0.0903(8) -0.0450(9) 0.071(3) Uani 0.524(8) 1 d PDU B 1 H4B H -0.0430 0.1113 -0.1088 0.085 Uiso 0.524(8) 1 calc PR B 1 H4A H -0.1085 0.0236 -0.0396 0.085 Uiso 0.524(8) 1 calc PR B 1 C5 C -0.0043(8) 0.0735(7) 0.0411(8) 0.062(3) Uani 0.524(8) 1 d PDU B 1 H5B H -0.0407 0.0619 0.1035 0.074 Uiso 0.524(8) 1 d PR B 1 H5A H 0.0458 0.0141 0.0456 0.074 Uiso 0.524(8) 1 d PR B 1 C4' C -0.1461(7) 0.1633(9) 0.0513(6) 0.051(3) Uani 0.476(8) 1 d PDU . 2 H4'A H -0.1329 0.0932 0.0947 0.061 Uiso 0.476(8) 1 d PR B 2 H4'B H -0.2032 0.1993 0.0772 0.061 Uiso 0.476(8) 1 d PR B 2 C5' C -0.0482(6) 0.2179(7) 0.0393(8) 0.050(3) Uani 0.476(8) 1 d PDU B 2 H5'A H -0.0603 0.2829 -0.0173 0.059 Uiso 0.476(8) 1 calc PR B 2 H5'B H -0.0377 0.2373 0.1007 0.059 Uiso 0.476(8) 1 calc PR B 2 C6 C 0.1364(3) 0.1517(3) 0.0784(3) 0.0342(9) Uani 1 1 d . B . C7 C 0.2311(3) 0.1596(3) 0.0298(3) 0.0343(9) Uani 1 1 d . . . C8 C 0.3234(3) 0.1573(3) 0.0830(3) 0.0318(9) Uani 1 1 d . B . H8 H 0.3887 0.1646 0.0493 0.038 Uiso 1 1 calc R . . C9 C 0.3193(3) 0.1443(3) 0.1853(3) 0.0267(8) Uani 1 1 d . . . C10 C 0.2235(3) 0.1336(3) 0.2343(3) 0.0251(8) Uani 1 1 d . B . C11 C 0.1318(3) 0.1373(3) 0.1814(3) 0.0294(8) Uani 1 1 d . . . H11 H 0.0664 0.1301 0.2148 0.035 Uiso 1 1 calc R B . C12 C 0.4130(3) 0.1419(3) 0.2537(3) 0.0274(8) Uani 1 1 d . B . C13 C 0.5169(3) 0.1547(3) 0.2002(3) 0.0357(9) Uani 1 1 d . . . H13A H 0.5350 0.0971 0.1727 0.054 Uiso 1 1 calc R B . H13C H 0.5722 0.1550 0.2476 0.054 Uiso 1 1 calc R . . H13B H 0.5106 0.2204 0.1455 0.054 Uiso 1 1 calc R . . C14 C 0.4126(3) 0.0403(3) 0.3405(3) 0.0268(8) Uani 1 1 d . . . C15 C 0.4980(3) -0.0338(3) 0.3739(3) 0.0338(9) Uani 1 1 d . B . H15 H 0.5636 -0.0255 0.3410 0.041 Uiso 1 1 calc R . . C16 C 0.4878(4) -0.1205(3) 0.4558(3) 0.0400(11) Uani 1 1 d . . . H16 H 0.5467 -0.1710 0.4792 0.048 Uiso 1 1 calc R B . C17 C 0.3934(4) -0.1335(3) 0.5027(3) 0.0412(11) Uani 1 1 d . B . H17 H 0.3870 -0.1939 0.5577 0.049 Uiso 1 1 calc R . . C18 C 0.3059(3) -0.0588(3) 0.4708(3) 0.0335(9) Uani 1 1 d . . . H18 H 0.2406 -0.0678 0.5042 0.040 Uiso 1 1 calc R B . C19 C 0.3162(3) 0.0284(3) 0.3899(3) 0.0273(8) Uani 1 1 d . B . C20 C 0.2304(3) 0.1203(3) 0.3478(3) 0.0255(8) Uani 1 1 d . . . C21 C 0.1259(3) 0.1080(3) 0.4001(3) 0.0334(9) Uani 1 1 d . B . H21B H 0.0759 0.1693 0.3692 0.050 Uiso 1 1 calc R . . H21C H 0.1359 0.1007 0.4712 0.050 Uiso 1 1 calc R . . H21A H 0.0983 0.0460 0.3936 0.050 Uiso 1 1 calc R . . C22 C 0.2819(3) 0.2155(3) 0.3519(3) 0.0248(8) Uani 1 1 d . B . C23 C 0.2400(3) 0.2876(3) 0.3990(3) 0.0263(8) Uani 1 1 d . . . H23 H 0.1741 0.2804 0.4315 0.032 Uiso 1 1 calc R B . C24 C 0.2951(3) 0.3692(3) 0.3978(3) 0.0283(8) Uani 1 1 d . B . C25 C 0.3941(3) 0.3776(3) 0.3532(3) 0.0290(8) Uani 1 1 d . . . C26 C 0.4348(3) 0.3075(3) 0.3047(3) 0.0271(8) Uani 1 1 d . B . H26 H 0.5009 0.3146 0.2727 0.033 Uiso 1 1 calc R . . C27 C 0.3778(3) 0.2267(3) 0.3032(3) 0.0244(8) Uani 1 1 d . . . C28 C 0.1674(3) 0.4401(3) 0.4939(3) 0.0370(10) Uani 1 1 d . . . H28B H 0.1780 0.3810 0.5564 0.044 Uiso 1 1 calc R . . H28A H 0.1083 0.4293 0.4548 0.044 Uiso 1 1 calc R . . C29 C 0.1446(4) 0.5407(4) 0.5178(4) 0.0459(11) Uani 1 1 d . . . H29A H 0.0941 0.5323 0.5734 0.055 Uiso 1 1 calc R . . H29B H 0.2105 0.5603 0.5395 0.055 Uiso 1 1 calc R . . C30 C 0.1046(5) 0.7201(4) 0.4454(5) 0.0653(16) Uani 1 1 d . . . H30A H 0.1786 0.7310 0.4547 0.078 Uiso 1 1 calc R . . H30B H 0.0656 0.7230 0.5064 0.078 Uiso 1 1 calc R . . C31 C 0.0564(4) 0.8045(4) 0.3563(5) 0.0642(16) Uani 1 1 d . . . H31B H 0.0820 0.8710 0.3544 0.077 Uiso 1 1 calc R . . H31A H 0.0789 0.7886 0.2942 0.077 Uiso 1 1 calc R . . C32 C -0.0977(4) 0.9141(5) 0.3023(5) 0.0669(16) Uani 1 1 d . . . H32A H -0.0787 0.9245 0.2313 0.080 Uiso 1 1 calc R . . H32B H -0.0663 0.9665 0.3250 0.080 Uiso 1 1 calc R . . C33 C 0.5497(3) 0.4654(3) 0.3286(4) 0.0399(10) Uani 1 1 d . . . H33A H 0.5545 0.4690 0.2571 0.048 Uiso 1 1 calc R B . H33B H 0.5957 0.4035 0.3686 0.048 Uiso 1 1 calc R . . C34 C 0.5834(3) 0.5621(3) 0.3437(4) 0.0445(11) Uani 1 1 d . B . H34A H 0.5727 0.5597 0.4145 0.053 Uiso 1 1 calc R . . H34B H 0.6595 0.5643 0.3298 0.053 Uiso 1 1 calc R . . C35 C 0.4369(4) 0.6918(4) 0.3269(5) 0.0633(16) Uani 1 1 d . . . H35B H 0.4580 0.6945 0.3937 0.076 Uiso 1 1 calc R . . H35A H 0.3815 0.6445 0.3363 0.076 Uiso 1 1 calc R . . C36 C 0.3952(5) 0.7974(4) 0.2629(5) 0.0748(17) Uani 1 1 d U . . H36A H 0.3413 0.8289 0.2996 0.090 Uiso 1 1 calc R . . H36B H 0.4530 0.8422 0.2457 0.090 Uiso 1 1 calc R . . O5 O 0.3500(3) 0.7897(3) 0.1741(3) 0.0753(12) Uani 1 1 d U . . C37 C 0.3155(6) 0.8887(6) 0.1075(7) 0.102(2) Uani 1 1 d U . . H37B H 0.3762 0.9291 0.0861 0.122 Uiso 1 1 calc R . . H37A H 0.2647 0.9271 0.1412 0.122 Uiso 1 1 calc R . . C38 C 0.2646(7) 0.8746(7) 0.0198(6) 0.107(3) Uani 1 1 d U . . H38B H 0.2523 0.9419 -0.0338 0.128 Uiso 1 1 calc R . . H38A H 0.3111 0.8261 -0.0067 0.128 Uiso 1 1 calc R . . C39 C 0.4234(5) 0.4417(4) -0.0116(4) 0.0562(14) Uani 1 1 d . . . H39 H 0.3709 0.4007 -0.0200 0.067 Uiso 1 1 calc R . . C40 C 0.4031(4) 0.5044(3) 0.0516(3) 0.0447(11) Uani 1 1 d . . . C41 C 0.4847(5) 0.5621(4) 0.0608(4) 0.0557(13) Uani 1 1 d . . . H41 H 0.4752 0.6052 0.1029 0.067 Uiso 1 1 calc R . . C42 C 0.1445(4) 0.4391(4) 0.1674(3) 0.0464(12) Uani 1 1 d . . . H42 H 0.0987 0.3868 0.1759 0.056 Uiso 1 1 calc R . . C43 C 0.2349(4) 0.4323(3) 0.1203(3) 0.0437(11) Uani 1 1 d . . . H43 H 0.2526 0.3746 0.0963 0.052 Uiso 1 1 calc R . . C44 C 0.3053(4) 0.5076(3) 0.1049(3) 0.0445(11) Uani 1 1 d . . . C45 C 0.2750(4) 0.5877(4) 0.1461(4) 0.0541(13) Uani 1 1 d . . . H45 H 0.3200 0.6401 0.1405 0.065 Uiso 1 1 calc R . . C46 C 0.1827(4) 0.5913(4) 0.1937(4) 0.0532(13) Uani 1 1 d . . . H46 H 0.1643 0.6466 0.2210 0.064 Uiso 1 1 calc R . . C47 C 0.0155(4) 0.5311(4) 0.2516(4) 0.0565(13) Uani 1 1 d . C . H47B H 0.0270 0.5490 0.3137 0.068 Uiso 1 1 calc R . . H47A H -0.0134 0.4634 0.2711 0.068 Uiso 1 1 calc R . . C48 C -0.0654(5) 0.6132(4) 0.1853(4) 0.0637(15) Uani 1 1 d D . . H48A H -0.0426 0.6826 0.1756 0.076 Uiso 0.524(8) 1 calc PR B 1 H48B H -0.1339 0.6108 0.2197 0.076 Uiso 0.524(8) 1 calc PR B 1 H48C H -0.0293 0.6704 0.1474 0.076 Uiso 0.476(8) 1 d PR . . H48D H -0.1144 0.6384 0.2275 0.076 Uiso 0.476(8) 1 d PR . . C49 C -0.0804(10) 0.5981(9) 0.0821(7) 0.058(3) Uani 0.567(17) 1 d PDU C 1 H49A H -0.0976 0.5265 0.0931 0.070 Uiso 0.567(17) 1 calc PR C 1 H49B H -0.1422 0.6458 0.0482 0.070 Uiso 0.567(17) 1 calc PR C 1 O11 O 0.0078(8) 0.6149(8) 0.0143(6) 0.074(4) Uani 0.567(17) 1 d PDU C 1 H11A H 0.0195 0.5650 -0.0091 0.089 Uiso 0.567(17) 1 calc PR C 1 C49' C -0.1273(10) 0.5779(11) 0.1121(10) 0.058(4) Uani 0.433(17) 1 d PDU C 2 H49C H -0.1582 0.5131 0.1467 0.070 Uiso 0.433(17) 1 calc PR C 2 H49D H -0.1843 0.6321 0.0778 0.070 Uiso 0.433(17) 1 calc PR C 2 O11' O -0.0485(9) 0.5611(10) 0.0428(8) 0.061(4) Uani 0.433(17) 1 d PDU C 2 H11B H -0.0519 0.5029 0.0347 0.073 Uiso 0.433(17) 1 calc PR 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 P1 0.057(2) 0.079(3) 0.076(3) -0.042(3) 0.0195(18) -0.032(2) F1 0.153(11) 0.084(6) 0.103(8) -0.025(6) 0.047(8) -0.028(8) F2 0.081(5) 0.109(7) 0.121(7) -0.041(6) -0.028(5) -0.036(5) F3 0.057(4) 0.080(5) 0.103(6) -0.045(5) 0.021(4) -0.019(4) F4 0.057(5) 0.089(6) 0.164(9) -0.043(6) 0.003(6) -0.011(4) F5 0.131(7) 0.052(5) 0.099(7) -0.032(5) 0.038(5) -0.039(4) F6 0.099(6) 0.096(6) 0.083(5) -0.035(4) 0.021(4) -0.039(5) P1' 0.0391(19) 0.064(3) 0.058(2) -0.027(2) 0.0058(14) -0.016(2) F1' 0.110(8) 0.070(6) 0.075(6) -0.020(5) -0.042(7) 0.011(6) F2' 0.054(5) 0.139(8) 0.138(8) -0.034(7) 0.009(5) -0.038(5) F3' 0.086(6) 0.097(8) 0.114(8) -0.072(7) -0.010(5) 0.001(6) F4' 0.040(4) 0.059(4) 0.113(7) -0.017(5) 0.019(4) -0.017(3) F5' 0.114(7) 0.080(6) 0.101(7) -0.052(5) 0.016(5) -0.008(5) F6' 0.086(6) 0.103(6) 0.087(6) -0.008(5) -0.007(4) -0.034(5) O1 0.0521(19) 0.056(2) 0.0315(15) -0.0188(15) -0.0066(14) -0.0026(15) O2 0.073(2) 0.0401(18) 0.0411(17) -0.0175(15) -0.0134(16) -0.0034(16) O3 0.0312(15) 0.0259(15) 0.065(2) -0.0207(14) -0.0036(14) -0.0068(12) O4 0.0484(19) 0.0252(16) 0.074(2) -0.0105(16) -0.0213(17) -0.0031(14) O6 0.0371(16) 0.0335(16) 0.0567(19) -0.0282(15) 0.0025(14) -0.0038(12) O7 0.0531(19) 0.0333(17) 0.060(2) -0.0252(16) -0.0152(16) 0.0107(14) O8 0.0431(18) 0.0371(18) 0.076(2) -0.0163(17) -0.0104(17) -0.0011(14) O9 0.0418(18) 0.056(2) 0.0483(18) -0.0192(16) -0.0226(15) -0.0002(15) O10 0.056(2) 0.068(2) 0.075(3) -0.031(2) -0.0301(19) 0.0166(19) N1 0.064(3) 0.034(2) 0.038(2) -0.0079(17) -0.0121(19) -0.0067(18) C1 0.048(3) 0.056(3) 0.045(3) -0.024(2) -0.008(2) -0.007(2) C2 0.068(3) 0.046(3) 0.035(2) -0.020(2) 0.005(2) -0.014(2) C3 0.057(3) 0.053(3) 0.042(3) -0.022(2) -0.001(2) -0.016(2) C4 0.066(5) 0.059(5) 0.095(6) -0.037(5) -0.035(5) 0.002(4) C5 0.050(5) 0.051(5) 0.084(6) -0.019(4) -0.025(4) -0.008(4) C4' 0.039(5) 0.060(5) 0.058(5) -0.024(4) -0.006(4) -0.003(4) C5' 0.039(5) 0.055(5) 0.060(5) -0.025(4) -0.016(4) -0.002(4) C6 0.034(2) 0.031(2) 0.039(2) -0.0130(18) -0.0128(18) -0.0016(17) C7 0.044(2) 0.030(2) 0.030(2) -0.0119(18) -0.0078(18) 0.0029(18) C8 0.034(2) 0.028(2) 0.033(2) -0.0101(17) -0.0019(17) 0.0027(16) C9 0.030(2) 0.0177(17) 0.033(2) -0.0097(16) -0.0069(16) 0.0010(15) C10 0.030(2) 0.0180(17) 0.0292(19) -0.0106(15) -0.0057(15) -0.0012(14) C11 0.029(2) 0.0245(19) 0.037(2) -0.0123(17) -0.0074(17) -0.0030(15) C12 0.0246(19) 0.0220(18) 0.038(2) -0.0132(17) -0.0043(16) 0.0008(15) C13 0.030(2) 0.034(2) 0.046(2) -0.017(2) 0.0013(18) -0.0024(17) C14 0.031(2) 0.0199(18) 0.033(2) -0.0134(16) -0.0081(16) 0.0012(15) C15 0.033(2) 0.030(2) 0.042(2) -0.0174(19) -0.0138(18) 0.0017(17) C16 0.046(3) 0.027(2) 0.047(3) -0.014(2) -0.022(2) 0.0069(18) C17 0.059(3) 0.024(2) 0.038(2) -0.0047(18) -0.019(2) -0.0039(19) C18 0.039(2) 0.028(2) 0.034(2) -0.0095(18) -0.0050(18) -0.0065(17) C19 0.032(2) 0.0225(19) 0.0301(19) -0.0108(16) -0.0095(16) -0.0033(15) C20 0.0257(19) 0.0230(19) 0.0290(19) -0.0091(16) -0.0046(15) -0.0034(15) C21 0.030(2) 0.035(2) 0.039(2) -0.0149(19) 0.0002(17) -0.0113(17) C22 0.0252(19) 0.0219(18) 0.0255(18) -0.0052(15) -0.0056(15) -0.0004(15) C23 0.0228(18) 0.0268(19) 0.0287(19) -0.0083(16) -0.0012(15) -0.0008(15) C24 0.0274(19) 0.0232(19) 0.035(2) -0.0107(17) -0.0061(16) 0.0023(15) C25 0.032(2) 0.0203(18) 0.036(2) -0.0090(16) -0.0097(17) -0.0039(15) C26 0.0200(18) 0.029(2) 0.032(2) -0.0082(17) -0.0041(15) -0.0017(15) C27 0.0251(18) 0.0198(18) 0.0293(19) -0.0101(15) -0.0067(15) 0.0016(14) C28 0.034(2) 0.038(2) 0.040(2) -0.017(2) -0.0001(18) 0.0048(18) C29 0.049(3) 0.046(3) 0.046(3) -0.024(2) -0.005(2) 0.012(2) C30 0.061(3) 0.046(3) 0.099(4) -0.040(3) -0.028(3) 0.008(2) C31 0.056(3) 0.034(3) 0.103(5) -0.023(3) -0.006(3) -0.002(2) C32 0.047(3) 0.062(4) 0.074(4) 0.004(3) 0.001(3) -0.002(3) C33 0.029(2) 0.025(2) 0.061(3) -0.006(2) -0.009(2) -0.0037(16) C34 0.030(2) 0.032(2) 0.069(3) -0.010(2) -0.020(2) -0.0062(18) C35 0.062(3) 0.044(3) 0.093(4) -0.038(3) -0.033(3) 0.008(2) C36 0.072(3) 0.051(3) 0.112(4) -0.038(3) -0.039(3) -0.005(2) O5 0.073(2) 0.0325(17) 0.113(3) -0.0089(19) -0.058(2) -0.0048(16) C37 0.080(4) 0.069(4) 0.138(5) 0.002(3) -0.040(3) -0.024(3) C38 0.090(4) 0.105(4) 0.096(4) 0.005(3) 0.002(4) 0.004(4) C39 0.071(4) 0.047(3) 0.063(3) -0.030(3) -0.007(3) -0.022(3) C40 0.063(3) 0.031(2) 0.042(2) -0.012(2) -0.017(2) -0.009(2) C41 0.071(4) 0.047(3) 0.055(3) -0.021(3) -0.005(3) -0.016(3) C42 0.061(3) 0.035(2) 0.044(3) -0.010(2) -0.014(2) -0.010(2) C43 0.055(3) 0.031(2) 0.046(3) -0.012(2) -0.014(2) -0.003(2) C44 0.061(3) 0.033(2) 0.039(2) -0.009(2) -0.019(2) -0.007(2) C45 0.067(3) 0.036(3) 0.064(3) -0.019(2) -0.011(3) -0.016(2) C46 0.072(4) 0.041(3) 0.050(3) -0.016(2) -0.009(3) -0.013(2) C47 0.074(4) 0.049(3) 0.048(3) -0.014(2) 0.002(3) -0.013(3) C48 0.075(4) 0.050(3) 0.063(3) -0.014(3) -0.010(3) 0.001(3) C49 0.068(7) 0.052(6) 0.059(6) -0.026(5) -0.005(5) 0.002(5) O11 0.091(7) 0.068(6) 0.066(5) -0.033(4) -0.006(4) 0.016(5) C49' 0.054(7) 0.049(7) 0.067(7) -0.011(6) 0.000(6) -0.003(5) O11' 0.062(7) 0.057(6) 0.070(6) -0.028(5) -0.005(5) -0.009(5) _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 P1 F6 1.556(9) . ? P1 F4 1.563(11) . ? P1 F3 1.597(10) . ? P1 F2 1.599(10) . ? P1 F1 1.602(16) . ? P1 F5 1.623(10) . ? P1' F5' 1.551(10) . ? P1' F1' 1.554(13) . ? P1' F2' 1.566(9) . ? P1' F4' 1.577(9) . ? P1' F6' 1.580(10) . ? P1' F3' 1.642(10) . ? O1 C7 1.377(5) . ? O1 C3 1.417(6) . ? O2 C2 1.407(5) . ? O2 C1 1.425(5) . ? O3 C25 1.369(4) . ? O3 C33 1.422(5) . ? O4 C34 1.426(5) . ? O4 C35 1.427(7) . ? O6 C24 1.381(5) . ? O6 C28 1.415(5) . ? O7 C29 1.410(6) . ? O7 C30 1.439(6) . ? O8 C32 1.397(6) . ? O8 C31 1.417(6) . ? O9 C5 1.363(7) . ? O9 C6 1.380(5) . ? O9 C5' 1.431(7) . ? O10 C4 1.407(8) . ? O10 C38 1.416(9) 2_565 ? O10 C4' 1.419(8) . ? N1 C46 1.326(6) . ? N1 C42 1.366(6) . ? N1 C47 1.458(7) . ? C1 C32 1.499(7) 2_565 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.513(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.515(9) . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C5 H5B 0.9599 . ? C5 H5A 0.9602 . ? C4' C5' 1.506(9) . ? C4' C38 2.022(12) 2_565 ? C4' H4'A 0.9599 . ? C4' H4'B 0.9599 . ? C5' H5'A 0.9900 . ? C5' H5'B 0.9900 . ? C6 C7 1.376(6) . ? C6 C11 1.397(6) . ? C7 C8 1.397(6) . ? C8 C9 1.390(5) . ? C8 H8 0.9500 . ? C9 C10 1.392(5) . ? C9 C12 1.537(5) . ? C10 C11 1.385(5) . ? C10 C20 1.547(5) . ? C11 H11 0.9500 . ? C12 C13 1.513(5) . ? C12 C14 1.538(5) . ? C12 C27 1.542(5) . ? C13 H13A 0.9800 . ? C13 H13C 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.381(5) . ? C14 C19 1.403(5) . ? C15 C16 1.388(6) . ? C15 H15 0.9500 . ? C16 C17 1.366(7) . ? C16 H16 0.9500 . ? C17 C18 1.402(6) . ? C17 H17 0.9500 . ? C18 C19 1.385(6) . ? C18 H18 0.9500 . ? C19 C20 1.542(5) . ? C20 C21 1.511(5) . ? C20 C22 1.535(5) . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 H21A 0.9800 . ? C22 C27 1.392(5) . ? C22 C23 1.397(5) . ? C23 C24 1.376(5) . ? C23 H23 0.9500 . ? C24 C25 1.401(6) . ? C25 C26 1.384(5) . ? C26 C27 1.391(5) . ? C26 H26 0.9500 . ? C28 C29 1.505(6) . ? C28 H28B 0.9900 . ? C28 H28A 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.499(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31B 0.9900 . ? C31 H31A 0.9900 . ? C32 C1 1.499(7) 2_565 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.505(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.487(8) . ? C35 H35B 0.9900 . ? C35 H35A 0.9900 . ? C36 O5 1.418(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O5 C37 1.413(7) . ? C37 C38 1.474(11) . ? C37 H37B 0.9900 . ? C37 H37A 0.9900 . ? C38 O10 1.416(9) 2_565 ? C38 C4' 2.022(12) 2_565 ? C38 H38B 0.9900 . ? C38 H38A 0.9900 . ? C39 C41 1.353(8) 2_665 ? C39 C40 1.409(7) . ? C39 H39 0.9500 . ? C40 C41 1.404(7) . ? C40 C44 1.447(7) . ? C41 C39 1.353(8) 2_665 ? C41 H41 0.9500 . ? C42 C43 1.328(7) . ? C42 H42 0.9500 . ? C43 C44 1.404(6) . ? C43 H43 0.9500 . ? C44 C45 1.399(7) . ? C45 C46 1.347(7) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.523(7) . ? C47 H47B 0.9900 . ? C47 H47A 0.9900 . ? C48 C49' 1.524(9) . ? C48 C49 1.540(8) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C48 H48C 0.9600 . ? C48 H48D 0.9600 . ? C49 O11 1.452(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? O11 H11A 0.8400 . ? C49' O11' 1.434(9) . ? C49' H49C 0.9900 . ? C49' H49D 0.9900 . ? O11' H11B 0.8400 . ? 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 F6 P1 F4 90.1(7) . . ? F6 P1 F3 90.5(6) . . ? F4 P1 F3 89.2(6) . . ? F6 P1 F2 91.3(6) . . ? F4 P1 F2 178.0(8) . . ? F3 P1 F2 89.3(6) . . ? F6 P1 F1 178.6(10) . . ? F4 P1 F1 90.0(7) . . ? F3 P1 F1 88.1(8) . . ? F2 P1 F1 88.6(7) . . ? F6 P1 F5 89.8(6) . . ? F4 P1 F5 90.9(6) . . ? F3 P1 F5 179.7(7) . . ? F2 P1 F5 90.5(6) . . ? F1 P1 F5 91.6(8) . . ? F5' P1' F1' 92.0(8) . . ? F5' P1' F2' 92.6(6) . . ? F1' P1' F2' 92.1(7) . . ? F5' P1' F4' 91.3(6) . . ? F1' P1' F4' 91.4(6) . . ? F2' P1' F4' 174.7(7) . . ? F5' P1' F6' 89.5(6) . . ? F1' P1' F6' 178.4(8) . . ? F2' P1' F6' 88.4(6) . . ? F4' P1' F6' 88.0(5) . . ? F5' P1' F3' 177.2(6) . . ? F1' P1' F3' 90.5(8) . . ? F2' P1' F3' 88.7(6) . . ? F4' P1' F3' 87.2(6) . . ? F6' P1' F3' 88.0(7) . . ? C7 O1 C3 119.8(3) . . ? C2 O2 C1 113.7(4) . . ? C25 O3 C33 118.5(3) . . ? C34 O4 C35 113.5(4) . . ? C24 O6 C28 118.4(3) . . ? C29 O7 C30 110.4(4) . . ? C32 O8 C31 110.8(4) . . ? C5 O9 C6 116.4(5) . . ? C5 O9 C5' 90.0(6) . . ? C6 O9 C5' 120.1(5) . . ? C4 O10 C38 114.7(7) . 2_565 ? C4 O10 C4' 91.4(6) . . ? C38 O10 C4' 91.0(6) 2_565 . ? C46 N1 C42 119.0(5) . . ? C46 N1 C47 119.9(4) . . ? C42 N1 C47 121.1(4) . . ? O2 C1 C32 115.1(4) . 2_565 ? O2 C1 H1A 108.5 . . ? C32 C1 H1A 108.5 2_565 . ? O2 C1 H1B 108.5 . . ? C32 C1 H1B 108.5 2_565 . ? H1A C1 H1B 107.5 . . ? O2 C2 C3 107.4(4) . . ? O2 C2 H2A 110.2 . . ? C3 C2 H2A 110.2 . . ? O2 C2 H2B 110.2 . . ? C3 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O1 C3 C2 106.7(4) . . ? O1 C3 H3A 110.4 . . ? C2 C3 H3A 110.4 . . ? O1 C3 H3B 110.4 . . ? C2 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? O10 C4 C5 114.2(8) . . ? O10 C4 H4B 108.7 . . ? C5 C4 H4B 108.7 . . ? O10 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? H4B C4 H4A 107.6 . . ? O9 C5 C4 107.4(7) . . ? O9 C5 H5B 110.6 . . ? C4 C5 H5B 110.7 . . ? O9 C5 H5A 109.7 . . ? C4 C5 H5A 109.9 . . ? H5B C5 H5A 108.5 . . ? O10 C4' C5' 102.1(7) . . ? O10 C4' C38 44.4(4) . 2_565 ? C5' C4' C38 145.9(7) . 2_565 ? O10 C4' H4'A 111.0 . . ? C5' C4' H4'A 111.2 . . ? C38 C4' H4'A 91.1 2_565 . ? O10 C4' H4'B 111.6 . . ? C5' C4' H4'B 111.6 . . ? C38 C4' H4'B 82.8 2_565 . ? H4'A C4' H4'B 109.3 . . ? O9 C5' C4' 115.8(7) . . ? O9 C5' H5'A 108.3 . . ? C4' C5' H5'A 108.3 . . ? O9 C5' H5'B 108.3 . . ? C4' C5' H5'B 108.3 . . ? H5'A C5' H5'B 107.4 . . ? C7 C6 O9 117.7(4) . . ? C7 C6 C11 120.7(4) . . ? O9 C6 C11 121.6(4) . . ? C6 C7 O1 115.1(4) . . ? C6 C7 C8 119.9(4) . . ? O1 C7 C8 125.0(4) . . ? C9 C8 C7 119.7(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.9(3) . . ? C8 C9 C12 126.0(4) . . ? C10 C9 C12 114.0(3) . . ? C11 C10 C9 120.3(3) . . ? C11 C10 C20 125.2(3) . . ? C9 C10 C20 114.5(3) . . ? C10 C11 C6 119.4(4) . . ? C10 C11 H11 120.3 . . ? C6 C11 H11 120.3 . . ? C13 C12 C9 114.0(3) . . ? C13 C12 C14 114.3(3) . . ? C9 C12 C14 105.3(3) . . ? C13 C12 C27 114.2(3) . . ? C9 C12 C27 104.3(3) . . ? C14 C12 C27 103.6(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? C15 C14 C19 120.0(4) . . ? C15 C14 C12 125.8(4) . . ? C19 C14 C12 114.2(3) . . ? C14 C15 C16 119.8(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.4(4) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.9(4) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 118.9(4) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C14 120.0(3) . . ? C18 C19 C20 126.0(4) . . ? C14 C19 C20 114.0(3) . . ? C21 C20 C22 114.6(3) . . ? C21 C20 C19 114.4(3) . . ? C22 C20 C19 104.2(3) . . ? C21 C20 C10 113.8(3) . . ? C22 C20 C10 103.7(3) . . ? C19 C20 C10 104.9(3) . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C21 H21A 109.5 . . ? H21B C21 H21A 109.5 . . ? H21C C21 H21A 109.5 . . ? C27 C22 C23 120.3(3) . . ? C27 C22 C20 114.3(3) . . ? C23 C22 C20 125.3(3) . . ? C24 C23 C22 119.3(3) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 O6 125.2(3) . . ? C23 C24 C25 120.3(3) . . ? O6 C24 C25 114.4(3) . . ? O3 C25 C26 124.5(4) . . ? O3 C25 C24 115.2(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C27 119.4(3) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C22 120.1(3) . . ? C26 C27 C12 125.6(3) . . ? C22 C27 C12 114.3(3) . . ? O6 C28 C29 106.1(4) . . ? O6 C28 H28B 110.5 . . ? C29 C28 H28B 110.5 . . ? O6 C28 H28A 110.5 . . ? C29 C28 H28A 110.5 . . ? H28B C28 H28A 108.7 . . ? O7 C29 C28 110.0(4) . . ? O7 C29 H29A 109.7 . . ? C28 C29 H29A 109.7 . . ? O7 C29 H29B 109.7 . . ? C28 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? O7 C30 C31 111.0(4) . . ? O7 C30 H30A 109.4 . . ? C31 C30 H30A 109.4 . . ? O7 C30 H30B 109.4 . . ? C31 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? O8 C31 C30 111.4(5) . . ? O8 C31 H31B 109.3 . . ? C30 C31 H31B 109.3 . . ? O8 C31 H31A 109.3 . . ? C30 C31 H31A 109.3 . . ? H31B C31 H31A 108.0 . . ? O8 C32 C1 112.4(4) . 2_565 ? O8 C32 H32A 109.1 . . ? C1 C32 H32A 109.1 2_565 . ? O8 C32 H32B 109.1 . . ? C1 C32 H32B 109.1 2_565 . ? H32A C32 H32B 107.9 . . ? O3 C33 C34 107.2(4) . . ? O3 C33 H33A 110.3 . . ? C34 C33 H33A 110.3 . . ? O3 C33 H33B 110.3 . . ? C34 C33 H33B 110.3 . . ? H33A C33 H33B 108.5 . . ? O4 C34 C33 112.1(3) . . ? O4 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? O4 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? O4 C35 C36 109.3(5) . . ? O4 C35 H35B 109.8 . . ? C36 C35 H35B 109.8 . . ? O4 C35 H35A 109.8 . . ? C36 C35 H35A 109.8 . . ? H35B C35 H35A 108.3 . . ? O5 C36 C35 109.0(4) . . ? O5 C36 H36A 109.9 . . ? C35 C36 H36A 109.9 . . ? O5 C36 H36B 109.9 . . ? C35 C36 H36B 109.9 . . ? H36A C36 H36B 108.3 . . ? C37 O5 C36 111.2(5) . . ? O5 C37 C38 108.2(6) . . ? O5 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? O5 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? H37B C37 H37A 108.4 . . ? O10 C38 C37 109.3(6) 2_565 . ? O10 C38 C4' 44.6(4) 2_565 2_565 ? C37 C38 C4' 153.8(7) . 2_565 ? O10 C38 H38B 109.8 2_565 . ? C37 C38 H38B 109.8 . . ? C4' C38 H38B 83.5 2_565 . ? O10 C38 H38A 109.8 2_565 . ? C37 C38 H38A 109.8 . . ? C4' C38 H38A 85.7 2_565 . ? H38B C38 H38A 108.3 . . ? C41 C39 C40 122.2(5) 2_665 . ? C41 C39 H39 118.9 2_665 . ? C40 C39 H39 118.9 . . ? C41 C40 C39 115.6(5) . . ? C41 C40 C44 122.3(4) . . ? C39 C40 C44 122.1(4) . . ? C39 C41 C40 122.2(5) 2_665 . ? C39 C41 H41 118.9 2_665 . ? C40 C41 H41 118.9 . . ? C43 C42 N1 120.6(4) . . ? C43 C42 H42 119.7 . . ? N1 C42 H42 119.7 . . ? C42 C43 C44 122.3(4) . . ? C42 C43 H43 118.9 . . ? C44 C43 H43 118.9 . . ? C45 C44 C43 115.0(5) . . ? C45 C44 C40 121.1(4) . . ? C43 C44 C40 123.9(4) . . ? C46 C45 C44 120.8(5) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? N1 C46 C45 122.3(5) . . ? N1 C46 H46 118.8 . . ? C45 C46 H46 118.8 . . ? N1 C47 C48 113.6(4) . . ? N1 C47 H47B 108.8 . . ? C48 C47 H47B 108.8 . . ? N1 C47 H47A 108.8 . . ? C48 C47 H47A 108.8 . . ? H47B C47 H47A 107.7 . . ? C47 C48 C49' 115.6(7) . . ? C47 C48 C49 112.7(6) . . ? C49' C48 C49 28.5(5) . . ? C47 C48 H48A 109.1 . . ? C49' C48 H48A 127.9 . . ? C49 C48 H48A 109.1 . . ? C47 C48 H48B 109.1 . . ? C49' C48 H48B 82.0 . . ? C49 C48 H48B 109.1 . . ? H48A C48 H48B 107.8 . . ? C47 C48 H48C 108.1 . . ? C49' C48 H48C 108.1 . . ? C49 C48 H48C 83.3 . . ? H48A C48 H48C 29.4 . . ? H48B C48 H48C 131.7 . . ? C47 C48 H48D 108.6 . . ? C49' C48 H48D 108.6 . . ? C49 C48 H48D 131.3 . . ? H48A C48 H48D 79.8 . . ? H48B C48 H48D 30.5 . . ? H48C C48 H48D 107.5 . . ? O11 C49 C48 117.0(8) . . ? O11 C49 H49A 108.1 . . ? C48 C49 H49A 108.1 . . ? O11 C49 H49B 108.1 . . ? C48 C49 H49B 108.1 . . ? H49A C49 H49B 107.3 . . ? O11' C49' C48 102.9(8) . . ? O11' C49' H49C 111.2 . . ? C48 C49' H49C 111.2 . . ? O11' C49' H49D 111.2 . . ? C48 C49' H49D 111.2 . . ? H49C C49' H49D 109.1 . . ? C49' O11' H11B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 O2 C1 C32 -84.0(5) . . . 2_565 ? C1 O2 C2 C3 163.1(4) . . . . ? C7 O1 C3 C2 175.1(4) . . . . ? O2 C2 C3 O1 -74.2(5) . . . . ? C38 O10 C4 C5 -107.0(9) 2_565 . . . ? C4' O10 C4 C5 -15.3(10) . . . . ? C6 O9 C5 C4 -165.8(6) . . . . ? C5' O9 C5 C4 70.2(9) . . . . ? O10 C4 C5 O9 -69.9(12) . . . . ? C4 O10 C4' C5' 72.6(8) . . . . ? C38 O10 C4' C5' -172.7(7) 2_565 . . . ? C4 O10 C4' C38 -114.8(7) . . . 2_565 ? C5 O9 C5' C4' -9.0(9) . . . . ? C6 O9 C5' C4' -129.9(7) . . . . ? O10 C4' C5' O9 -73.3(10) . . . . ? C38 C4' C5' O9 -82.5(16) 2_565 . . . ? C5 O9 C6 C7 114.4(7) . . . . ? C5' O9 C6 C7 -138.9(6) . . . . ? C5 O9 C6 C11 -66.6(7) . . . . ? C5' O9 C6 C11 40.1(7) . . . . ? O9 C6 C7 O1 -3.2(5) . . . . ? C11 C6 C7 O1 177.8(4) . . . . ? O9 C6 C7 C8 176.5(4) . . . . ? C11 C6 C7 C8 -2.5(6) . . . . ? C3 O1 C7 C6 179.1(4) . . . . ? C3 O1 C7 C8 -0.6(6) . . . . ? C6 C7 C8 C9 1.7(6) . . . . ? O1 C7 C8 C9 -178.6(4) . . . . ? C7 C8 C9 C10 0.0(6) . . . . ? C7 C8 C9 C12 -178.9(4) . . . . ? C8 C9 C10 C11 -0.9(5) . . . . ? C12 C9 C10 C11 178.1(3) . . . . ? C8 C9 C10 C20 -179.7(3) . . . . ? C12 C9 C10 C20 -0.6(4) . . . . ? C9 C10 C11 C6 0.1(5) . . . . ? C20 C10 C11 C6 178.7(3) . . . . ? C7 C6 C11 C10 1.6(6) . . . . ? O9 C6 C11 C10 -177.4(4) . . . . ? C8 C9 C12 C13 -0.4(5) . . . . ? C10 C9 C12 C13 -179.4(3) . . . . ? C8 C9 C12 C14 -126.4(4) . . . . ? C10 C9 C12 C14 54.7(4) . . . . ? C8 C9 C12 C27 124.8(4) . . . . ? C10 C9 C12 C27 -54.1(4) . . . . ? C13 C12 C14 C15 3.2(5) . . . . ? C9 C12 C14 C15 128.9(4) . . . . ? C27 C12 C14 C15 -121.8(4) . . . . ? C13 C12 C14 C19 -179.8(3) . . . . ? C9 C12 C14 C19 -54.0(4) . . . . ? C27 C12 C14 C19 55.3(4) . . . . ? C19 C14 C15 C16 0.7(6) . . . . ? C12 C14 C15 C16 177.5(3) . . . . ? C14 C15 C16 C17 0.7(6) . . . . ? C15 C16 C17 C18 -1.4(6) . . . . ? C16 C17 C18 C19 0.6(6) . . . . ? C17 C18 C19 C14 0.8(6) . . . . ? C17 C18 C19 C20 -177.0(4) . . . . ? C15 C14 C19 C18 -1.4(5) . . . . ? C12 C14 C19 C18 -178.7(3) . . . . ? C15 C14 C19 C20 176.6(3) . . . . ? C12 C14 C19 C20 -0.6(4) . . . . ? C18 C19 C20 C21 -2.5(5) . . . . ? C14 C19 C20 C21 179.6(3) . . . . ? C18 C19 C20 C22 123.5(4) . . . . ? C14 C19 C20 C22 -54.5(4) . . . . ? C18 C19 C20 C10 -127.9(4) . . . . ? C14 C19 C20 C10 54.2(4) . . . . ? C11 C10 C20 C21 1.7(5) . . . . ? C9 C10 C20 C21 -179.5(3) . . . . ? C11 C10 C20 C22 -123.4(4) . . . . ? C9 C10 C20 C22 55.3(4) . . . . ? C11 C10 C20 C19 127.6(4) . . . . ? C9 C10 C20 C19 -53.7(4) . . . . ? C21 C20 C22 C27 -179.7(3) . . . . ? C19 C20 C22 C27 54.5(4) . . . . ? C10 C20 C22 C27 -55.0(4) . . . . ? C21 C20 C22 C23 0.1(5) . . . . ? C19 C20 C22 C23 -125.7(4) . . . . ? C10 C20 C22 C23 124.8(4) . . . . ? C27 C22 C23 C24 -0.8(5) . . . . ? C20 C22 C23 C24 179.4(3) . . . . ? C22 C23 C24 O6 176.8(3) . . . . ? C22 C23 C24 C25 -2.5(5) . . . . ? C28 O6 C24 C23 8.1(6) . . . . ? C28 O6 C24 C25 -172.6(3) . . . . ? C33 O3 C25 C26 -8.9(6) . . . . ? C33 O3 C25 C24 172.2(3) . . . . ? C23 C24 C25 O3 -177.1(3) . . . . ? O6 C24 C25 O3 3.6(5) . . . . ? C23 C24 C25 C26 3.9(6) . . . . ? O6 C24 C25 C26 -175.4(3) . . . . ? O3 C25 C26 C27 179.1(3) . . . . ? C24 C25 C26 C27 -2.0(5) . . . . ? C25 C26 C27 C22 -1.3(5) . . . . ? C25 C26 C27 C12 -179.1(3) . . . . ? C23 C22 C27 C26 2.7(5) . . . . ? C20 C22 C27 C26 -177.5(3) . . . . ? C23 C22 C27 C12 -179.2(3) . . . . ? C20 C22 C27 C12 0.6(4) . . . . ? C13 C12 C27 C26 -2.5(5) . . . . ? C9 C12 C27 C26 -127.6(4) . . . . ? C14 C12 C27 C26 122.4(4) . . . . ? C13 C12 C27 C22 179.6(3) . . . . ? C9 C12 C27 C22 54.5(4) . . . . ? C14 C12 C27 C22 -55.5(4) . . . . ? C24 O6 C28 C29 -174.8(3) . . . . ? C30 O7 C29 C28 -165.3(4) . . . . ? O6 C28 C29 O7 76.2(4) . . . . ? C29 O7 C30 C31 -178.3(4) . . . . ? C32 O8 C31 C30 157.2(5) . . . . ? O7 C30 C31 O8 80.0(6) . . . . ? C31 O8 C32 C1 -176.4(5) . . . 2_565 ? C25 O3 C33 C34 179.2(3) . . . . ? C35 O4 C34 C33 95.1(5) . . . . ? O3 C33 C34 O4 -65.6(5) . . . . ? C34 O4 C35 C36 168.9(4) . . . . ? O4 C35 C36 O5 68.8(6) . . . . ? C35 C36 O5 C37 -176.1(6) . . . . ? C36 O5 C37 C38 -177.1(6) . . . . ? O5 C37 C38 O10 70.6(8) . . . 2_565 ? O5 C37 C38 C4' 73.7(18) . . . 2_565 ? C41 C39 C40 C41 -0.5(8) 2_665 . . . ? C41 C39 C40 C44 -179.3(5) 2_665 . . . ? C39 C40 C41 C39 0.5(8) . . . 2_665 ? C44 C40 C41 C39 179.3(5) . . . 2_665 ? C46 N1 C42 C43 -1.9(6) . . . . ? C47 N1 C42 C43 177.3(4) . . . . ? N1 C42 C43 C44 -0.5(7) . . . . ? C42 C43 C44 C45 2.4(6) . . . . ? C42 C43 C44 C40 -178.2(4) . . . . ? C41 C40 C44 C45 17.6(7) . . . . ? C39 C40 C44 C45 -163.6(5) . . . . ? C41 C40 C44 C43 -161.8(5) . . . . ? C39 C40 C44 C43 17.0(7) . . . . ? C43 C44 C45 C46 -2.1(7) . . . . ? C40 C44 C45 C46 178.5(4) . . . . ? C42 N1 C46 C45 2.2(7) . . . . ? C47 N1 C46 C45 -177.0(5) . . . . ? C44 C45 C46 N1 -0.1(8) . . . . ? C46 N1 C47 C48 75.5(6) . . . . ? C42 N1 C47 C48 -103.7(5) . . . . ? N1 C47 C48 C49' 83.8(8) . . . . ? N1 C47 C48 C49 52.7(8) . . . . ? C47 C48 C49 O11 -67.8(10) . . . . ? C49' C48 C49 O11 -170(2) . . . . ? C47 C48 C49' O11' -68.1(10) . . . . ? C49 C48 C49' O11' 22.6(12) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.659 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.065