# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Pradyut Ghosh' _publ_contact_author_email ICPG@IACS.RES.IN _publ_section_title ; F2(H2O)62- Cluster Selective Dimeric Capsule Formation of Arene Capped Tripodal Amide Receptor ; loop_ _publ_author_name 'Pradyut Ghosh' 'M Arunachalam' # Attachment 'complex-1.cif' data_tonaf2_0m _database_code_depnum_ccdc_archive 'CCDC 733118' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H160 F2 N14 O28' _chemical_formula_weight 2116.48 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' _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 12.9823(7) _cell_length_b 20.3519(12) _cell_length_c 23.1725(13) _cell_angle_alpha 105.659(2) _cell_angle_beta 92.575(2) _cell_angle_gamma 105.648(2) _cell_volume 5630.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4538 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 21.20 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9745 _exptl_absorpt_correction_T_max 0.9853 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'BRUKER CCD AREA DETECTOR' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54203 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 22.67 _reflns_number_total 14944 _reflns_number_gt 9162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'MERCURY 2.2' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1384P)^2^+7.5152P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14944 _refine_ls_number_parameters 1388 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2570 _refine_ls_wR_factor_gt 0.2118 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.005 _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 F1 F 0.87669(19) 0.46000(13) 0.03922(11) 0.0228(6) Uani 1 1 d . . . F2 F 0.61812(19) 0.04068(13) 0.45772(11) 0.0231(6) Uani 1 1 d . . . O3 O 0.9939(3) 0.5851(2) 0.11307(17) 0.0312(9) Uani 1 1 d D . . H3A H 0.970(4) 0.621(2) 0.112(3) 0.06(2) Uiso 1 1 d D . . H3B H 0.949(5) 0.545(3) 0.088(3) 0.11(3) Uiso 1 1 d D . . O4 O 0.0755(3) 0.44601(18) 0.03733(16) 0.0284(8) Uani 1 1 d D . . H4A H 0.010(2) 0.451(3) 0.038(3) 0.06(2) Uiso 1 1 d D . . H4B H 0.109(4) 0.475(3) 0.018(2) 0.06(2) Uiso 1 1 d D . . O5 O 0.6973(3) 0.1264(2) 0.56943(19) 0.0263(9) Uani 1 1 d . . . H5A H 0.637(5) 0.112(3) 0.583(3) 0.06(2) Uiso 1 1 d . . . H5B H 0.682(4) 0.100(3) 0.536(3) 0.026(17) Uiso 1 1 d . . . O6 O 0.4156(3) 0.05065(18) 0.46162(16) 0.0277(8) Uani 1 1 d D . . H6A H 0.387(4) 0.024(3) 0.485(2) 0.056(19) Uiso 1 1 d D . . H6B H 0.484(2) 0.052(4) 0.462(3) 0.08(2) Uiso 1 1 d D . . O7 O 0.8012(3) 0.3790(2) 0.9249(2) 0.0257(9) Uani 1 1 d . . . H7A H 0.859(5) 0.391(3) 0.914(3) 0.05(2) Uiso 1 1 d . . . H7B H 0.812(4) 0.399(3) 0.957(3) 0.04(2) Uiso 1 1 d . . . O8 O 0.4951(3) 0.0899(2) 0.61024(17) 0.0292(9) Uani 1 1 d . . . H8A H 0.457(4) 0.053(3) 0.587(2) 0.026(16) Uiso 1 1 d . . . H8B H 0.457(4) 0.118(3) 0.605(2) 0.036(16) Uiso 1 1 d . . . O9 O 0.6831(3) 0.2948(2) 1.21599(19) 0.0408(10) Uani 1 1 d . . . N10 N 0.7605(4) 0.3345(2) 1.2520(2) 0.0327(11) Uani 1 1 d . . . O11 O 0.7633(3) 0.3501(2) 1.30716(18) 0.0462(11) Uani 1 1 d . . . C12 C 0.8605(4) 0.3628(3) 1.2279(2) 0.0264(12) Uani 1 1 d . . . C13 C 0.9496(4) 0.3434(3) 1.2430(2) 0.0325(13) Uani 1 1 d . . . H13 H 0.9476 0.3165 1.2698 0.039 Uiso 1 1 calc R . . C14 C 1.0413(4) 0.3646(3) 1.2173(2) 0.0346(13) Uani 1 1 d . . . H14 H 1.1020 0.3516 1.2267 0.042 Uiso 1 1 calc R . . C15 C 1.0449(4) 0.4049(3) 1.1777(2) 0.0280(12) Uani 1 1 d . . . H15 H 1.1070 0.4181 1.1599 0.034 Uiso 1 1 calc R . . C16 C 0.9558(4) 0.4256(2) 1.1646(2) 0.0218(11) Uani 1 1 d . . . H16 H 0.9595 0.4538 1.1387 0.026 Uiso 1 1 calc R . . C17 C 0.8611(4) 0.4051(2) 1.1891(2) 0.0201(11) Uani 1 1 d . . . C18 C 0.7647(4) 0.4296(2) 1.1795(2) 0.0195(11) Uani 1 1 d . . . O19 O 0.7068(3) 0.43830(18) 1.22019(14) 0.0293(8) Uani 1 1 d . . . N20 N 0.7442(3) 0.44166(19) 1.12718(16) 0.0185(9) Uani 1 1 d . . . H20 H 0.7862 0.4361 1.0998 0.022 Uiso 1 1 calc R . . C21 C 0.6491(3) 0.4645(2) 1.1168(2) 0.0205(11) Uani 1 1 d . . . H21B H 0.6444 0.5011 1.1526 0.025 Uiso 1 1 calc R . . H21A H 0.5848 0.4243 1.1099 0.025 Uiso 1 1 calc R . . C22 C 0.6536(3) 0.4934(2) 1.0633(2) 0.0160(10) Uani 1 1 d . . . C23 C 0.7045(3) 0.5664(2) 1.0726(2) 0.0160(10) Uani 1 1 d . . . C24 C 0.7540(4) 0.6133(2) 1.1359(2) 0.0209(11) Uani 1 1 d . . . H24B H 0.8050 0.6563 1.1337 0.031 Uiso 1 1 calc R . . H24C H 0.7901 0.5881 1.1554 0.031 Uiso 1 1 calc R . . H24A H 0.6982 0.6251 1.1587 0.031 Uiso 1 1 calc R . . C25 C 0.7088(3) 0.5944(2) 1.0234(2) 0.0186(11) Uani 1 1 d . . . C26 C 0.7646(4) 0.6721(2) 1.0312(2) 0.0210(11) Uani 1 1 d . . . H26A H 0.7202 0.6911 1.0092 0.025 Uiso 1 1 calc R . . H26B H 0.7744 0.6988 1.0736 0.025 Uiso 1 1 calc R . . N27 N 0.8692(3) 0.68059(19) 1.00895(16) 0.0190(9) Uani 1 1 d . . . H27 H 0.8940 0.6445 0.9984 0.023 Uiso 1 1 calc R . . C28 C 0.9267(4) 0.7438(3) 1.0049(2) 0.0196(11) Uani 1 1 d . . . O29 O 0.8997(3) 0.79885(16) 1.02191(14) 0.0261(8) Uani 1 1 d . . . C30 C 1.0296(4) 0.7447(2) 0.9773(2) 0.0228(11) Uani 1 1 d . . . C31 C 1.1066(4) 0.7180(3) 0.9988(2) 0.0289(12) Uani 1 1 d . . . H31 H 1.0938 0.6969 1.0298 0.035 Uiso 1 1 calc R . . C32 C 1.2027(4) 0.7229(3) 0.9740(3) 0.0411(15) Uani 1 1 d . . . H32 H 1.2538 0.7052 0.9889 0.049 Uiso 1 1 calc R . . C33 C 1.2240(5) 0.7528(3) 0.9285(3) 0.0464(16) Uani 1 1 d . . . H33 H 1.2884 0.7547 0.9121 0.056 Uiso 1 1 calc R . . C34 C 1.1495(5) 0.7807(3) 0.9064(3) 0.0477(17) Uani 1 1 d . . . H34 H 1.1629 0.8016 0.8754 0.057 Uiso 1 1 calc R . . C35 C 1.0553(4) 0.7764(3) 0.9320(2) 0.0325(13) Uani 1 1 d . . . N36 N 0.9728(5) 0.8014(3) 0.9057(2) 0.0584(15) Uani 1 1 d . . . O37 O 0.8821(4) 0.7602(3) 0.88958(18) 0.0595(12) Uani 1 1 d . . . O38 O 0.9996(5) 0.8605(4) 0.9001(4) 0.140(3) Uani 1 1 d . . . C39 C 0.6616(3) 0.5496(2) 0.9654(2) 0.0170(10) Uani 1 1 d . . . C40 C 0.6676(4) 0.5792(3) 0.9119(2) 0.0243(11) Uani 1 1 d . . . H40A H 0.6687 0.5424 0.8760 0.036 Uiso 1 1 calc R . . H40C H 0.7320 0.6183 0.9186 0.036 Uiso 1 1 calc R . . H40B H 0.6058 0.5954 0.9070 0.036 Uiso 1 1 calc R . . C41 C 0.6109(3) 0.4773(2) 0.9572(2) 0.0190(11) Uani 1 1 d . . . C42 C 0.5544(3) 0.4298(3) 0.8955(2) 0.0228(11) Uani 1 1 d . . . H42A H 0.4973 0.3903 0.9003 0.027 Uiso 1 1 calc R . . H42B H 0.5215 0.4569 0.8757 0.027 Uiso 1 1 calc R . . N43 N 0.6286(3) 0.40137(19) 0.85705(16) 0.0196(9) Uani 1 1 d . . . H43 H 0.6827 0.3930 0.8733 0.024 Uiso 1 1 calc R . . C44 C 0.6134(4) 0.3885(2) 0.7979(2) 0.0208(11) Uani 1 1 d . . . O45 O 0.5377(3) 0.39905(18) 0.77112(14) 0.0287(8) Uani 1 1 d . . . C46 C 0.6956(4) 0.3616(2) 0.7627(2) 0.0201(11) Uani 1 1 d . . . C47 C 0.8056(4) 0.3948(2) 0.7806(2) 0.0241(11) Uani 1 1 d . . . H47 H 0.8286 0.4312 0.8168 0.029 Uiso 1 1 calc R . . C48 C 0.8808(4) 0.3741(3) 0.7452(2) 0.0312(13) Uani 1 1 d . . . H48 H 0.9540 0.3966 0.7578 0.037 Uiso 1 1 calc R . . C49 C 0.8480(4) 0.3205(3) 0.6913(2) 0.0305(13) Uani 1 1 d . . . H49 H 0.8992 0.3071 0.6677 0.037 Uiso 1 1 calc R . . C50 C 0.7391(4) 0.2862(3) 0.6722(2) 0.0255(12) Uani 1 1 d . . . H50 H 0.7162 0.2498 0.6359 0.031 Uiso 1 1 calc R . . C51 C 0.6660(4) 0.3076(2) 0.7082(2) 0.0208(11) Uani 1 1 d . . . N52 N 0.5515(3) 0.2670(2) 0.6890(2) 0.0249(10) Uani 1 1 d . . . O53 O 0.5174(3) 0.25263(19) 0.63520(16) 0.0385(9) Uani 1 1 d . . . O54 O 0.4968(3) 0.24786(18) 0.72594(16) 0.0320(9) Uani 1 1 d . . . C55 C 0.6095(3) 0.4485(2) 1.0056(2) 0.0172(11) Uani 1 1 d . . . C56 C 0.5631(4) 0.3684(2) 0.9950(2) 0.0258(12) Uani 1 1 d . . . H56C H 0.5943 0.3549 1.0266 0.039 Uiso 1 1 calc R . . H56A H 0.5795 0.3433 0.9567 0.039 Uiso 1 1 calc R . . H56B H 0.4863 0.3566 0.9948 0.039 Uiso 1 1 calc R . . N57 N 0.9378(3) 0.96619(19) 0.15601(17) 0.0240(9) Uiso 1 1 d D . . C58 C 0.8586(6) 0.9287(4) 0.1928(4) 0.0276(19) Uiso 0.62 1 d PD . . C58B C 0.8786(9) 0.8915(6) 0.1576(5) 0.020(3) Uiso 0.38 1 d PD . . C59 C 0.7934(7) 0.8525(5) 0.1573(4) 0.041(2) Uiso 0.62 1 d PD . . C59B C 0.8001(9) 0.8896(6) 0.2058(6) 0.027(3) Uiso 0.38 1 d PD . . C60 C 0.6905(10) 0.8311(6) 0.1884(5) 0.030(3) Uiso 0.42 1 d PD . . C60B C 0.7282(8) 0.8129(5) 0.1956(4) 0.031(2) Uiso 0.58 1 d PD . . C61 C 0.6144(8) 0.7611(6) 0.1484(4) 0.047(3) Uiso 0.64 1 d PD . . C61B C 0.6392(14) 0.7908(11) 0.1442(7) 0.048(5) Uiso 0.36 1 d PD . . C62 C 0.8833(7) 0.9664(5) 0.0987(4) 0.039(2) Uiso 0.63 1 d PD . . C62B C 0.8559(11) 1.0017(7) 0.1363(6) 0.038(4) Uiso 0.37 1 d PD . . C63 C 0.7807(8) 0.9898(6) 0.1069(5) 0.063(3) Uiso 0.65 1 d PD . . C63B C 0.7888(13) 0.9628(10) 0.0753(8) 0.055(5) Uiso 0.35 1 d PD . . C64 C 0.7474(11) 1.0044(7) 0.0469(6) 0.067(4) Uiso 0.55 1 d PD . . C64B C 0.7012(11) 0.9950(7) 0.0671(7) 0.049(4) Uiso 0.45 1 d PD . . C65 C 0.6354(12) 1.0161(9) 0.0494(8) 0.089(5) Uiso 0.50 1 d PD . . C65B C 0.6077(14) 0.9756(11) 0.1025(9) 0.109(6) Uiso 0.50 1 d PD . . C66 C 1.0231(6) 0.9265(4) 0.1449(4) 0.0255(19) Uiso 0.60 1 d PD . . C66B C 1.0105(10) 0.9569(8) 0.1050(6) 0.041(4) Uiso 0.40 1 d PD . . C67 C 1.1111(8) 0.9610(6) 0.1118(5) 0.061(3) Uiso 0.64 1 d PD . . C67B C 1.1071(12) 0.9343(11) 0.1218(8) 0.048(5) Uiso 0.36 1 d PD . . C68 C 1.1983(10) 0.9197(6) 0.1089(6) 0.051(3) Uiso 0.51 1 d PD . . C68B C 1.1866(12) 0.9394(9) 0.0757(7) 0.081(5) Uiso 0.49 1 d PD . . C69 C 1.289(2) 0.9639(16) 0.1532(13) 0.166(12) Uiso 0.42 1 d PD . . C69B C 1.2930(11) 0.9285(8) 0.0835(7) 0.083(4) Uiso 0.58 1 d PD . . C70 C 0.9879(6) 1.0444(4) 0.1958(3) 0.035(2) Uiso 0.67 1 d PD . . C70B C 0.9944(10) 1.0139(7) 0.2143(5) 0.017(3) Uiso 0.33 1 d PD . . C71 C 1.0581(6) 1.0561(4) 0.2531(4) 0.042(2) Uiso 0.70 1 d PD . . C71B C 1.0816(14) 1.0804(8) 0.2127(7) 0.044(5) Uiso 0.30 1 d PD . . C72 C 1.097(2) 1.1333(10) 0.2929(14) 0.031(10) Uiso 0.18 1 d PD . . C72B C 1.1174(6) 1.1361(4) 0.2759(4) 0.041(3) Uiso 0.82 1 d PD . . C73 C 1.0397(8) 1.1825(5) 0.2832(4) 0.057(3) Uiso 0.69 1 d PD . . C73B C 1.165(2) 1.2000(11) 0.2602(11) 0.079(7) Uiso 0.31 1 d PD . . O74 O 0.0651(3) 0.3489(2) 0.37659(19) 0.0560(12) Uani 1 1 d . . . C75 C 0.1632(5) 0.3536(3) 0.4100(3) 0.0497(16) Uani 1 1 d . . . H75B H 0.1942 0.4020 0.4363 0.060 Uiso 1 1 calc R . . H75A H 0.2143 0.3429 0.3823 0.060 Uiso 1 1 calc R . . C76 C 0.1443(5) 0.3026(3) 0.4475(3) 0.0476(16) Uani 1 1 d . . . H76A H 0.1184 0.2539 0.4211 0.057 Uiso 1 1 calc R . . H76B H 0.2118 0.3079 0.4706 0.057 Uiso 1 1 calc R . . O77 O 0.0670(3) 0.3160(2) 0.48770(19) 0.0549(11) Uani 1 1 d . . . C78 C -0.0308(5) 0.3107(4) 0.4535(3) 0.0578(19) Uani 1 1 d . . . H78B H -0.0830 0.3204 0.4808 0.069 Uiso 1 1 calc R . . H78A H -0.0604 0.2625 0.4268 0.069 Uiso 1 1 calc R . . C79 C -0.0120(5) 0.3620(4) 0.4172(3) 0.0579(18) Uani 1 1 d . . . H79A H -0.0795 0.3572 0.3943 0.069 Uiso 1 1 calc R . . H79B H 0.0142 0.4104 0.4439 0.069 Uiso 1 1 calc R . . O80 O 0.3896(4) 0.1875(3) 0.0187(2) 0.0883(17) Uani 1 1 d . . . C81 C 0.4893(6) 0.1946(5) 0.0490(4) 0.089(3) Uani 1 1 d . . . H81B H 0.5213 0.2440 0.0727 0.106 Uiso 1 1 calc R . . H81A H 0.5370 0.1823 0.0196 0.106 Uiso 1 1 calc R . . C82 C 0.4798(6) 0.1483(4) 0.0894(4) 0.071(2) Uani 1 1 d . . . H82A H 0.4560 0.0986 0.0653 0.085 Uiso 1 1 calc R . . H82B H 0.5498 0.1574 0.1115 0.085 Uiso 1 1 calc R . . O83 O 0.4044(4) 0.1617(3) 0.1313(2) 0.0782(15) Uani 1 1 d . . . C84 C 0.3039(5) 0.1534(4) 0.0997(3) 0.0630(19) Uani 1 1 d . . . H84B H 0.2541 0.1639 0.1284 0.076 Uiso 1 1 calc R . . H84A H 0.2740 0.1043 0.0748 0.076 Uiso 1 1 calc R . . C85 C 0.3163(6) 0.2016(4) 0.0611(3) 0.065(2) Uani 1 1 d . . . H85A H 0.2467 0.1950 0.0396 0.078 Uiso 1 1 calc R . . H85B H 0.3428 0.2508 0.0862 0.078 Uiso 1 1 calc R . . O9' O 1.0061(3) 1.25890(19) 0.76754(15) 0.0333(9) Uani 1 1 d . . . N10' N 0.9507(3) 1.2399(2) 0.80453(19) 0.0253(10) Uani 1 1 d . . . O11' O 0.9836(3) 1.25373(18) 0.85834(16) 0.0330(9) Uani 1 1 d . . . C12' C 0.8363(4) 1.1992(2) 0.7843(2) 0.0203(11) Uani 1 1 d . . . C13' C 0.7621(4) 1.2208(3) 0.8207(2) 0.0254(12) Uani 1 1 d . . . H13' H 0.7846 1.2572 0.8570 0.030 Uiso 1 1 calc R . . C14' C 0.6533(4) 1.1862(3) 0.8010(2) 0.0288(12) Uani 1 1 d . . . H14' H 0.6017 1.1996 0.8243 0.035 Uiso 1 1 calc R . . C15' C 0.6213(4) 1.1321(3) 0.7472(2) 0.0294(12) Uani 1 1 d . . . H15' H 0.5484 1.1092 0.7342 0.035 Uiso 1 1 calc R . . C16' C 0.6979(4) 1.1117(2) 0.7124(2) 0.0225(11) Uani 1 1 d . . . H16' H 0.6755 1.0747 0.6766 0.027 Uiso 1 1 calc R . . C17' C 0.8076(4) 1.1453(2) 0.7300(2) 0.0199(11) Uani 1 1 d . . . C18' C 0.8909(4) 1.1188(2) 0.6954(2) 0.0196(11) Uani 1 1 d . . . O19' O 0.9658(3) 1.10806(18) 0.72206(14) 0.0286(8) Uani 1 1 d . . . N20' N 0.8761(3) 1.10679(19) 0.63603(17) 0.0205(9) Uani 1 1 d . . . H20' H 0.8223 1.1157 0.6201 0.025 Uiso 1 1 calc R . . C21' C 0.9497(3) 1.0786(2) 0.5970(2) 0.0221(11) Uani 1 1 d . . . H21C H 0.9840 1.0522 0.6169 0.027 Uiso 1 1 calc R . . H21D H 1.0057 1.1181 0.5915 0.027 Uiso 1 1 calc R . . C22' C 0.8931(3) 1.0303(2) 0.53606(19) 0.0163(10) Uani 1 1 d . . . C23' C 0.8468(3) 0.9581(2) 0.5295(2) 0.0162(10) Uani 1 1 d . . . C24' C 0.8472(4) 0.9304(3) 0.5841(2) 0.0239(11) Uani 1 1 d . . . H24E H 0.9153 0.9221 0.5915 0.036 Uiso 1 1 calc R . . H24D H 0.7903 0.8865 0.5765 0.036 Uiso 1 1 calc R . . H24F H 0.8363 0.9650 0.6188 0.036 Uiso 1 1 calc R . . C25' C 0.7993(3) 0.9117(2) 0.4721(2) 0.0157(10) Uani 1 1 d . . . C26' C 0.7479(3) 0.8338(2) 0.4655(2) 0.0193(11) Uani 1 1 d . . . H26D H 0.7369 0.8066 0.4232 0.023 Uiso 1 1 calc R . . H26C H 0.7956 0.8165 0.4870 0.023 Uiso 1 1 calc R . . N27' N 0.6445(3) 0.82300(19) 0.48946(16) 0.0167(9) Uani 1 1 d . . . H27' H 0.6162 0.8575 0.4992 0.020 Uiso 1 1 calc R . . C28' C 0.5944(4) 0.7601(2) 0.49611(19) 0.0178(11) Uani 1 1 d . . . O29' O 0.6259(3) 0.70678(16) 0.47980(14) 0.0243(8) Uani 1 1 d . . . C30' C 0.4951(4) 0.7570(2) 0.5273(2) 0.0206(11) Uani 1 1 d . . . C31' C 0.4138(4) 0.7837(2) 0.5110(2) 0.0261(12) Uani 1 1 d . . . H31' H 0.4204 0.8057 0.4804 0.031 Uiso 1 1 calc R . . C32' C 0.3228(4) 0.7774(3) 0.5407(3) 0.0372(14) Uani 1 1 d . . . H32' H 0.2681 0.7949 0.5298 0.045 Uiso 1 1 calc R . . C33' C 0.3128(4) 0.7452(3) 0.5865(3) 0.0412(15) Uani 1 1 d . . . H33' H 0.2521 0.7423 0.6066 0.049 Uiso 1 1 calc R . . C34' C 0.3919(4) 0.7172(3) 0.6028(3) 0.0385(14) Uani 1 1 d . . . H34' H 0.3847 0.6945 0.6330 0.046 Uiso 1 1 calc R . . C35' C 0.4806(4) 0.7239(3) 0.5731(2) 0.0291(12) Uani 1 1 d . . . N36' N 0.5697(4) 0.6991(3) 0.5932(2) 0.0363(11) Uani 1 1 d . . . O37' O 0.6569(3) 0.7424(2) 0.61349(17) 0.0496(11) Uani 1 1 d . . . O38' O 0.5469(4) 0.6346(3) 0.5876(2) 0.0668(14) Uani 1 1 d . . . C39' C 0.7983(3) 0.9379(2) 0.42222(19) 0.0151(10) Uani 1 1 d . . . C40' C 0.7479(4) 0.8890(2) 0.3600(2) 0.0214(11) Uani 1 1 d . . . H40D H 0.7124 0.9134 0.3393 0.032 Uiso 1 1 calc R . . H40F H 0.6964 0.8470 0.3636 0.032 Uiso 1 1 calc R . . H40E H 0.8031 0.8756 0.3374 0.032 Uiso 1 1 calc R . . C41' C 0.8443(3) 1.0109(2) 0.4303(2) 0.0163(10) Uani 1 1 d . . . C42' C 0.8429(3) 1.0386(2) 0.3762(2) 0.0200(11) Uani 1 1 d . . . H42D H 0.9048 1.0801 0.3821 0.024 Uiso 1 1 calc R . . H42C H 0.8488 1.0022 0.3405 0.024 Uiso 1 1 calc R . . N43' N 0.7444(3) 1.05780(19) 0.36635(17) 0.0200(9) Uani 1 1 d . . . H43' H 0.7038 1.0636 0.3945 0.024 Uiso 1 1 calc R . . C44' C 0.7184(4) 1.0663(2) 0.3130(2) 0.0201(11) Uani 1 1 d . . . O45' O 0.7731(3) 1.05742(17) 0.27090(15) 0.0289(8) Uani 1 1 d . . . C46' C 0.6170(4) 1.0884(2) 0.3053(2) 0.0222(11) Uani 1 1 d . . . C47' C 0.5266(4) 1.0675(2) 0.3332(2) 0.0224(11) Uani 1 1 d . . . H47' H 0.5275 1.0401 0.3594 0.027 Uiso 1 1 calc R . . C48' C 0.4352(4) 1.0871(3) 0.3224(2) 0.0298(12) Uani 1 1 d . . . H48' H 0.3755 1.0734 0.3419 0.036 Uiso 1 1 calc R . . C49' C 0.4317(4) 1.1268(3) 0.2831(2) 0.0373(14) Uani 1 1 d . . . H49' H 0.3696 1.1393 0.2758 0.045 Uiso 1 1 calc R . . C50' C 0.5204(4) 1.1479(3) 0.2545(2) 0.0340(13) Uani 1 1 d . . . H50' H 0.5187 1.1743 0.2275 0.041 Uiso 1 1 calc R . . C51' C 0.6115(4) 1.1292(3) 0.2667(2) 0.0264(12) Uani 1 1 d . . . N52' N 0.7077(4) 1.1584(3) 0.2397(2) 0.0380(12) Uani 1 1 d . . . O53' O 0.7012(3) 1.1433(2) 0.18484(19) 0.0497(11) Uani 1 1 d . . . O54' O 0.7867(3) 1.1992(2) 0.27463(19) 0.0417(10) Uani 1 1 d . . . C55' C 0.9305(4) 1.1372(2) 0.4969(2) 0.0256(12) Uani 1 1 d . . . H55E H 1.0073 1.1511 0.4969 0.038 Uiso 1 1 calc R . . H55F H 0.9132 1.1621 0.5350 0.038 Uiso 1 1 calc R . . H55D H 0.8970 1.1490 0.4649 0.038 Uiso 1 1 calc R . . C56' C 0.8896(3) 1.0578(2) 0.4876(2) 0.0174(11) Uani 1 1 d . . . N57' N 0.4203(3) 0.46764(19) 0.65161(16) 0.0206(9) Uani 1 1 d . . . C58' C 0.3705(4) 0.3943(2) 0.6580(2) 0.0253(12) Uani 1 1 d . . . H58A H 0.3293 0.3641 0.6196 0.030 Uiso 1 1 calc R . . H58B H 0.4285 0.3748 0.6655 0.030 Uiso 1 1 calc R . . C59' C 0.2980(4) 0.3884(3) 0.7064(2) 0.0273(12) Uani 1 1 d . . . H59A H 0.2495 0.4171 0.7056 0.033 Uiso 1 1 calc R . . H59B H 0.3414 0.4069 0.7457 0.033 Uiso 1 1 calc R . . C60' C 0.2331(4) 0.3120(3) 0.6974(2) 0.0297(12) Uani 1 1 d . . . H60B H 0.2070 0.3079 0.7352 0.036 Uiso 1 1 calc R . . H60A H 0.2805 0.2820 0.6878 0.036 Uiso 1 1 calc R . . C61' C 0.1379(4) 0.2837(3) 0.6484(3) 0.0409(14) Uani 1 1 d . . . H61B H 0.0897 0.3124 0.6577 0.061 Uiso 1 1 calc R . . H61A H 0.1007 0.2352 0.6462 0.061 Uiso 1 1 calc R . . H61C H 0.1629 0.2853 0.6104 0.061 Uiso 1 1 calc R . . C62' C 0.3321(4) 0.5001(3) 0.6369(2) 0.0352(13) Uani 1 1 d . . . H62A H 0.2935 0.5085 0.6717 0.042 Uiso 1 1 calc R . . H62B H 0.3672 0.5463 0.6316 0.042 Uiso 1 1 calc R . . C63' C 0.2517(5) 0.4584(3) 0.5830(3) 0.0455(15) Uani 1 1 d . . . H63A H 0.2215 0.4101 0.5848 0.055 Uiso 1 1 calc R . . H63B H 0.2867 0.4563 0.5467 0.055 Uiso 1 1 calc R . . C64' C 0.1613(5) 0.4933(3) 0.5805(3) 0.061(2) Uani 1 1 d . . . H64A H 0.1221 0.4749 0.5401 0.074 Uiso 1 1 calc R . . H64B H 0.1928 0.5444 0.5887 0.074 Uiso 1 1 calc R . . C65' C 0.0810(5) 0.4791(4) 0.6268(4) 0.075(2) Uani 1 1 d . . . H65A H 0.0487 0.4286 0.6185 0.113 Uiso 1 1 calc R . . H65B H 0.0257 0.5016 0.6235 0.113 Uiso 1 1 calc R . . H65C H 0.1191 0.4983 0.6670 0.113 Uiso 1 1 calc R . . C66' C 0.4881(4) 0.4611(3) 0.6002(2) 0.0330(13) Uani 1 1 d . . . H66B H 0.4446 0.4243 0.5652 0.040 Uiso 1 1 calc R . . H66A H 0.5057 0.5058 0.5901 0.040 Uiso 1 1 calc R . . C67' C 0.5916(4) 0.4438(3) 0.6114(2) 0.0403(14) Uani 1 1 d . . . H67B H 0.6359 0.4796 0.6466 0.048 Uiso 1 1 calc R . . H67A H 0.5754 0.3979 0.6194 0.048 Uiso 1 1 calc R . . C68' C 0.6530(5) 0.4414(3) 0.5576(3) 0.0547(18) Uani 1 1 d . . . H68B H 0.6087 0.4048 0.5227 0.066 Uiso 1 1 calc R . . H68A H 0.6666 0.4868 0.5490 0.066 Uiso 1 1 calc R . . C69' C 0.7578(5) 0.4263(4) 0.5666(4) 0.081(2) Uani 1 1 d . . . H69B H 0.8019 0.4619 0.6014 0.121 Uiso 1 1 calc R . . H69A H 0.7943 0.4273 0.5316 0.121 Uiso 1 1 calc R . . H69C H 0.7448 0.3800 0.5726 0.121 Uiso 1 1 calc R . . C70' C 0.4859(4) 0.5161(3) 0.7106(2) 0.0286(12) Uani 1 1 d . . . H70B H 0.4379 0.5191 0.7415 0.034 Uiso 1 1 calc R . . H70A H 0.5381 0.4940 0.7218 0.034 Uiso 1 1 calc R . . C71' C 0.5450(5) 0.5902(3) 0.7112(3) 0.0521(17) Uani 1 1 d . . . H71B H 0.4933 0.6162 0.7083 0.063 Uiso 1 1 calc R . . H71A H 0.5836 0.5883 0.6762 0.063 Uiso 1 1 calc R . . C72' C 0.6246(6) 0.6302(3) 0.7682(3) 0.0562(19) Uani 1 1 d . . . H72A H 0.5860 0.6356 0.8032 0.067 Uiso 1 1 calc R . . H72B H 0.6739 0.6031 0.7727 0.067 Uiso 1 1 calc R . . C73' C 0.6880(7) 0.7033(4) 0.7646(4) 0.088(3) Uani 1 1 d . . . H73A H 0.7180 0.6983 0.7271 0.132 Uiso 1 1 calc R . . H73B H 0.7452 0.7251 0.7977 0.132 Uiso 1 1 calc R . . H73C H 0.6409 0.7328 0.7669 0.132 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 F1 0.0195(14) 0.0308(16) 0.0209(15) 0.0073(12) 0.0061(11) 0.0115(12) F2 0.0186(14) 0.0289(16) 0.0228(15) 0.0076(12) 0.0044(12) 0.0083(12) O3 0.023(2) 0.032(2) 0.035(2) -0.0001(19) 0.0058(17) 0.0112(18) O4 0.023(2) 0.026(2) 0.044(2) 0.0139(18) 0.0134(18) 0.0152(17) O5 0.020(2) 0.034(2) 0.020(2) -0.0016(19) -0.0001(18) 0.0099(17) O6 0.021(2) 0.025(2) 0.042(2) 0.0129(17) 0.0111(17) 0.0116(16) O7 0.019(2) 0.036(2) 0.020(2) 0.001(2) 0.0011(18) 0.0121(17) O8 0.021(2) 0.030(2) 0.030(2) -0.003(2) 0.0000(17) 0.010(2) O9 0.040(2) 0.037(2) 0.054(3) 0.025(2) 0.014(2) 0.012(2) N10 0.040(3) 0.032(3) 0.042(3) 0.022(2) 0.022(3) 0.021(2) O11 0.070(3) 0.056(3) 0.035(3) 0.029(2) 0.027(2) 0.035(2) C12 0.034(3) 0.025(3) 0.030(3) 0.015(2) 0.012(2) 0.015(2) C13 0.047(3) 0.035(3) 0.028(3) 0.019(3) 0.007(3) 0.023(3) C14 0.031(3) 0.042(3) 0.037(3) 0.016(3) 0.003(3) 0.018(3) C15 0.025(3) 0.036(3) 0.030(3) 0.013(3) 0.008(2) 0.015(2) C16 0.027(3) 0.024(3) 0.020(3) 0.013(2) 0.006(2) 0.010(2) C17 0.023(3) 0.023(3) 0.016(3) 0.007(2) 0.006(2) 0.009(2) C18 0.023(3) 0.018(3) 0.021(3) 0.006(2) 0.010(2) 0.010(2) O19 0.039(2) 0.038(2) 0.026(2) 0.0177(17) 0.0173(17) 0.0258(17) N20 0.018(2) 0.025(2) 0.019(2) 0.0101(18) 0.0104(17) 0.0125(17) C21 0.015(2) 0.024(3) 0.024(3) 0.007(2) 0.006(2) 0.006(2) C22 0.007(2) 0.025(3) 0.019(3) 0.007(2) 0.0051(19) 0.009(2) C23 0.008(2) 0.023(3) 0.019(3) 0.003(2) 0.0043(19) 0.009(2) C24 0.018(3) 0.023(3) 0.022(3) 0.007(2) 0.002(2) 0.007(2) C25 0.014(2) 0.023(3) 0.021(3) 0.004(2) 0.005(2) 0.011(2) C26 0.024(3) 0.019(3) 0.023(3) 0.005(2) 0.005(2) 0.012(2) N27 0.021(2) 0.020(2) 0.021(2) 0.0084(18) 0.0064(17) 0.0111(18) C28 0.026(3) 0.024(3) 0.010(3) 0.006(2) 0.002(2) 0.008(2) O29 0.040(2) 0.0191(19) 0.0224(19) 0.0055(15) 0.0075(16) 0.0141(16) C30 0.025(3) 0.017(3) 0.022(3) 0.004(2) 0.005(2) 0.002(2) C31 0.030(3) 0.027(3) 0.032(3) 0.007(2) 0.011(2) 0.012(2) C32 0.035(3) 0.037(3) 0.051(4) 0.007(3) 0.018(3) 0.014(3) C33 0.036(3) 0.041(4) 0.056(4) 0.007(3) 0.024(3) 0.005(3) C34 0.058(4) 0.043(4) 0.040(4) 0.020(3) 0.028(3) 0.001(3) C35 0.034(3) 0.030(3) 0.037(3) 0.017(3) 0.010(3) 0.008(2) N36 0.068(4) 0.072(4) 0.051(4) 0.048(3) 0.018(3) 0.016(3) O37 0.059(3) 0.090(4) 0.031(2) 0.011(2) 0.004(2) 0.033(3) O38 0.106(5) 0.135(6) 0.244(8) 0.169(6) 0.024(5) 0.030(4) C39 0.011(2) 0.027(3) 0.019(3) 0.008(2) 0.007(2) 0.013(2) C40 0.026(3) 0.036(3) 0.018(3) 0.011(2) 0.003(2) 0.016(2) C41 0.010(2) 0.028(3) 0.021(3) 0.001(2) 0.006(2) 0.014(2) C42 0.012(2) 0.030(3) 0.024(3) 0.001(2) -0.001(2) 0.010(2) N43 0.014(2) 0.026(2) 0.018(2) -0.0021(18) -0.0006(17) 0.0131(17) C44 0.021(3) 0.018(3) 0.020(3) 0.002(2) 0.001(2) 0.004(2) O45 0.028(2) 0.041(2) 0.0214(19) 0.0065(16) -0.0033(16) 0.0210(17) C46 0.020(3) 0.018(3) 0.023(3) 0.006(2) 0.002(2) 0.008(2) C47 0.022(3) 0.022(3) 0.023(3) 0.000(2) 0.001(2) 0.005(2) C48 0.018(3) 0.034(3) 0.037(3) 0.007(3) 0.005(2) 0.003(2) C49 0.025(3) 0.036(3) 0.034(3) 0.009(3) 0.009(2) 0.015(2) C50 0.028(3) 0.022(3) 0.025(3) 0.002(2) 0.005(2) 0.009(2) C51 0.017(3) 0.025(3) 0.022(3) 0.008(2) 0.002(2) 0.009(2) N52 0.020(2) 0.023(2) 0.028(3) -0.001(2) -0.001(2) 0.0096(18) O53 0.036(2) 0.047(2) 0.024(2) -0.0022(18) -0.0090(17) 0.0115(18) O54 0.0210(19) 0.038(2) 0.033(2) 0.0090(18) 0.0018(17) 0.0027(16) C55 0.008(2) 0.018(3) 0.026(3) 0.002(2) 0.007(2) 0.0078(19) C56 0.016(3) 0.028(3) 0.031(3) 0.006(2) 0.004(2) 0.006(2) O74 0.050(3) 0.062(3) 0.058(3) 0.028(2) -0.016(2) 0.012(2) C75 0.046(4) 0.055(4) 0.046(4) 0.015(3) 0.002(3) 0.012(3) C76 0.050(4) 0.044(4) 0.052(4) 0.019(3) -0.010(3) 0.015(3) O77 0.050(3) 0.064(3) 0.057(3) 0.029(2) 0.002(2) 0.016(2) C78 0.035(4) 0.065(5) 0.079(5) 0.038(4) -0.010(3) 0.009(3) C79 0.042(4) 0.057(4) 0.076(5) 0.027(4) -0.009(4) 0.013(3) O80 0.071(4) 0.142(5) 0.078(4) 0.063(4) 0.005(3) 0.043(3) C81 0.048(5) 0.126(8) 0.102(7) 0.058(6) 0.007(5) 0.020(5) C82 0.060(5) 0.076(5) 0.083(6) 0.030(5) -0.016(4) 0.026(4) O83 0.059(3) 0.118(5) 0.076(4) 0.052(3) 0.000(3) 0.034(3) C84 0.058(4) 0.083(5) 0.060(5) 0.037(4) -0.001(4) 0.026(4) C85 0.067(5) 0.080(5) 0.059(5) 0.024(4) 0.006(4) 0.035(4) O9' 0.026(2) 0.043(2) 0.029(2) 0.0099(18) 0.0071(17) 0.0054(17) N10' 0.025(2) 0.022(2) 0.023(3) -0.003(2) -0.004(2) 0.0080(19) O11' 0.028(2) 0.038(2) 0.024(2) 0.0009(17) -0.0048(17) 0.0052(17) C12' 0.019(3) 0.021(3) 0.021(3) 0.006(2) 0.000(2) 0.005(2) C13' 0.029(3) 0.030(3) 0.020(3) 0.004(2) 0.009(2) 0.017(2) C14' 0.025(3) 0.036(3) 0.033(3) 0.012(3) 0.013(2) 0.020(2) C15' 0.015(3) 0.035(3) 0.036(3) 0.008(3) 0.002(2) 0.007(2) C16' 0.020(3) 0.023(3) 0.022(3) 0.001(2) -0.002(2) 0.008(2) C17' 0.021(3) 0.018(3) 0.022(3) 0.007(2) 0.002(2) 0.006(2) C18' 0.017(3) 0.016(3) 0.024(3) 0.002(2) 0.001(2) 0.005(2) O19' 0.0236(19) 0.040(2) 0.024(2) 0.0052(17) -0.0016(16) 0.0171(16) N20' 0.016(2) 0.025(2) 0.019(2) 0.0000(18) 0.0013(17) 0.0111(17) C21' 0.017(2) 0.026(3) 0.020(3) -0.001(2) 0.003(2) 0.007(2) C22' 0.008(2) 0.024(3) 0.015(3) -0.003(2) 0.0027(19) 0.009(2) C23' 0.011(2) 0.023(3) 0.018(3) 0.006(2) 0.002(2) 0.011(2) C24' 0.021(3) 0.029(3) 0.023(3) 0.006(2) 0.003(2) 0.011(2) C25' 0.011(2) 0.020(3) 0.020(3) 0.004(2) 0.006(2) 0.011(2) C26' 0.017(2) 0.022(3) 0.023(3) 0.009(2) 0.005(2) 0.010(2) N27' 0.019(2) 0.015(2) 0.020(2) 0.0068(17) 0.0049(17) 0.0095(17) C28' 0.025(3) 0.020(3) 0.008(2) 0.004(2) -0.001(2) 0.006(2) O29' 0.035(2) 0.0202(19) 0.0209(19) 0.0052(15) 0.0089(15) 0.0139(16) C30' 0.026(3) 0.013(3) 0.019(3) 0.002(2) 0.005(2) 0.001(2) C31' 0.026(3) 0.022(3) 0.027(3) 0.006(2) 0.007(2) 0.001(2) C32' 0.030(3) 0.029(3) 0.051(4) 0.007(3) 0.018(3) 0.008(2) C33' 0.035(3) 0.038(3) 0.041(4) 0.003(3) 0.021(3) 0.002(3) C34' 0.040(3) 0.037(3) 0.041(4) 0.017(3) 0.021(3) 0.007(3) C35' 0.035(3) 0.027(3) 0.026(3) 0.011(2) 0.006(2) 0.005(2) N36' 0.051(3) 0.041(3) 0.031(3) 0.029(2) 0.014(2) 0.017(3) O37' 0.047(3) 0.064(3) 0.034(2) 0.008(2) 0.002(2) 0.016(2) O38' 0.082(3) 0.063(3) 0.080(3) 0.056(3) 0.016(3) 0.025(3) C39' 0.010(2) 0.020(3) 0.017(3) 0.004(2) 0.0018(19) 0.0093(19) C40' 0.022(3) 0.025(3) 0.020(3) 0.005(2) 0.003(2) 0.011(2) C41' 0.010(2) 0.023(3) 0.020(3) 0.007(2) 0.004(2) 0.009(2) C42' 0.017(2) 0.022(3) 0.024(3) 0.008(2) 0.007(2) 0.009(2) N43' 0.018(2) 0.025(2) 0.024(2) 0.0095(19) 0.0104(18) 0.0125(17) C44' 0.023(3) 0.016(3) 0.026(3) 0.012(2) 0.008(2) 0.008(2) O45' 0.036(2) 0.037(2) 0.029(2) 0.0204(17) 0.0198(17) 0.0223(17) C46' 0.024(3) 0.021(3) 0.023(3) 0.007(2) 0.003(2) 0.010(2) C47' 0.023(3) 0.024(3) 0.028(3) 0.017(2) 0.006(2) 0.010(2) C48' 0.024(3) 0.038(3) 0.030(3) 0.012(3) 0.010(2) 0.011(2) C49' 0.039(3) 0.046(4) 0.037(3) 0.015(3) 0.003(3) 0.026(3) C50' 0.047(3) 0.037(3) 0.034(3) 0.023(3) 0.009(3) 0.025(3) C51' 0.031(3) 0.031(3) 0.027(3) 0.016(2) 0.013(2) 0.017(2) N52' 0.051(3) 0.037(3) 0.046(3) 0.027(3) 0.021(3) 0.028(3) O53' 0.068(3) 0.067(3) 0.039(3) 0.037(2) 0.031(2) 0.036(2) O54' 0.038(2) 0.039(2) 0.060(3) 0.028(2) 0.019(2) 0.015(2) C55' 0.017(3) 0.020(3) 0.037(3) 0.005(2) 0.007(2) 0.003(2) C56' 0.007(2) 0.020(3) 0.026(3) 0.005(2) 0.007(2) 0.0054(19) N57' 0.029(2) 0.019(2) 0.017(2) 0.0075(18) 0.0051(18) 0.0086(18) C58' 0.031(3) 0.024(3) 0.022(3) 0.007(2) 0.002(2) 0.010(2) C59' 0.028(3) 0.029(3) 0.026(3) 0.007(2) 0.004(2) 0.009(2) C60' 0.032(3) 0.023(3) 0.030(3) 0.007(2) 0.012(2) 0.003(2) C61' 0.030(3) 0.041(3) 0.044(4) 0.003(3) 0.008(3) 0.006(3) C62' 0.037(3) 0.027(3) 0.046(4) 0.016(3) 0.004(3) 0.011(2) C63' 0.050(4) 0.054(4) 0.040(4) 0.018(3) -0.005(3) 0.025(3) C64' 0.066(5) 0.047(4) 0.067(5) 0.010(4) -0.033(4) 0.023(3) C65' 0.051(4) 0.068(5) 0.113(7) 0.036(5) -0.005(4) 0.023(4) C66' 0.042(3) 0.027(3) 0.028(3) 0.010(2) 0.011(3) 0.004(2) C67' 0.038(3) 0.051(4) 0.037(3) 0.017(3) 0.017(3) 0.016(3) C68' 0.047(4) 0.041(4) 0.065(5) 0.005(3) 0.033(3) 0.001(3) C69' 0.055(5) 0.084(6) 0.108(7) 0.027(5) 0.051(5) 0.025(4) C70' 0.030(3) 0.027(3) 0.023(3) 0.001(2) 0.001(2) 0.005(2) C71' 0.068(4) 0.042(4) 0.036(4) 0.015(3) -0.002(3) -0.003(3) C72' 0.097(5) 0.026(3) 0.027(3) 0.010(3) -0.008(3) -0.014(3) C73' 0.094(6) 0.069(6) 0.087(6) 0.020(5) -0.014(5) 0.007(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 O3 H3A 0.87(2) . ? O3 H3B 0.88(2) . ? O4 H4A 0.88(2) . ? O4 H4B 0.87(2) . ? O5 H5A 0.87(7) . ? O5 H5B 0.79(6) . ? O6 H6A 0.89(2) . ? O6 H6B 0.88(2) . ? O7 H7A 0.80(7) . ? O7 H7B 0.74(6) . ? O8 H8A 0.80(5) . ? O8 H8B 0.88(6) . ? O9 N10 1.218(6) . ? N10 O11 1.227(6) . ? N10 C12 1.471(6) . ? C12 C13 1.378(7) . ? C12 C17 1.403(6) . ? C13 C14 1.372(7) . ? C13 H13 0.9300 . ? C14 C15 1.381(7) . ? C14 H14 0.9300 . ? C15 C16 1.381(6) . ? C15 H15 0.9300 . ? C16 C17 1.386(6) . ? C16 H16 0.9300 . ? C17 C18 1.496(6) . ? C18 O19 1.237(5) . ? C18 N20 1.328(6) . ? N20 C21 1.463(6) . ? N20 H20 0.8600 . ? C21 C22 1.506(6) . ? C21 H21B 0.9700 . ? C21 H21A 0.9700 . ? C22 C55 1.394(6) . ? C22 C23 1.405(6) . ? C23 C25 1.402(6) . ? C23 C24 1.519(6) . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C24 H24A 0.9600 . ? C25 C39 1.405(6) . ? C25 C26 1.509(6) . ? C26 N27 1.457(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? N27 C28 1.332(6) . ? N27 H27 0.8600 . ? C28 O29 1.233(5) . ? C28 C30 1.504(6) . ? C30 C35 1.381(7) . ? C30 C31 1.392(7) . ? C31 C32 1.388(7) . ? C31 H31 0.9300 . ? C32 C33 1.357(8) . ? C32 H32 0.9300 . ? C33 C34 1.387(8) . ? C33 H33 0.9300 . ? C34 C35 1.376(7) . ? C34 H34 0.9300 . ? C35 N36 1.477(7) . ? N36 O38 1.204(7) . ? N36 O37 1.220(6) . ? C39 C41 1.397(6) . ? C39 C40 1.514(6) . ? C40 H40A 0.9600 . ? C40 H40C 0.9600 . ? C40 H40B 0.9600 . ? C41 C55 1.397(6) . ? C41 C42 1.514(6) . ? C42 N43 1.468(5) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? N43 C44 1.320(6) . ? N43 H43 0.8600 . ? C44 O45 1.235(5) . ? C44 C46 1.502(6) . ? C46 C51 1.389(6) . ? C46 C47 1.393(6) . ? C47 C48 1.383(7) . ? C47 H47 0.9300 . ? C48 C49 1.377(7) . ? C48 H48 0.9300 . ? C49 C50 1.389(7) . ? C49 H49 0.9300 . ? C50 C51 1.374(6) . ? C50 H50 0.9300 . ? C51 N52 1.473(6) . ? N52 O54 1.214(5) . ? N52 O53 1.232(5) . ? C55 C56 1.524(6) . ? C56 H56C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? N57 C70B 1.458(12) . ? N57 C62 1.479(9) . ? N57 C58B 1.518(10) . ? N57 C66 1.531(8) . ? N57 C58 1.541(8) . ? N57 C70 1.549(8) . ? N57 C66B 1.549(12) . ? N57 C62B 1.552(13) . ? C58 C58B 1.048(12) . ? C58 C59B 1.060(12) . ? C58 C59 1.529(11) . ? C58B C59 1.173(12) . ? C58B C59B 1.546(13) . ? C58B C66 1.886(13) . ? C59 C59B 1.156(14) . ? C59 C60B 1.497(12) . ? C59 C60 1.561(12) . ? C59 C61B 2.02(2) . ? C59B C60B 1.535(12) . ? C59B C60 1.543(16) . ? C60 C60B 0.726(13) . ? C60 C61B 1.165(18) . ? C60 C61 1.520(13) . ? C60B C61B 1.505(15) . ? C60B C61 1.697(14) . ? C61 C61B 0.640(19) . ? C62 C62B 1.108(15) . ? C62 C63B 1.294(17) . ? C62 C63 1.533(12) . ? C62 C66B 1.719(15) . ? C62B C63 1.095(14) . ? C62B C63B 1.515(16) . ? C62B C70 1.983(15) . ? C63 C63B 0.817(17) . ? C63 C64B 1.398(17) . ? C63 C64 1.563(13) . ? C63B C64 1.40(2) . ? C63B C64B 1.485(16) . ? C64 C64B 0.790(15) . ? C64 C65 1.536(15) . ? C64B C65 1.158(19) . ? C64B C65B 1.520(16) . ? C65 C65B 1.66(2) . ? C66 C67B 1.227(16) . ? C66 C66B 1.270(15) . ? C66 C67 1.524(12) . ? C66B C67 1.286(16) . ? C66B C67B 1.516(16) . ? C67 C67B 0.636(19) . ? C67 C68B 1.400(18) . ? C67 C68 1.576(13) . ? C67B C68 1.324(18) . ? C67B C68B 1.522(16) . ? C68 C68B 0.983(17) . ? C68 C69B 1.376(17) . ? C68 C69 1.437(18) . ? C68B C69B 1.468(15) . ? C69 C69B 1.59(3) . ? C70 C70B 0.862(13) . ? C70 C71B 1.222(17) . ? C70 C71 1.502(10) . ? C70B C71 1.168(13) . ? C70B C71B 1.522(16) . ? C71 C71B 1.187(17) . ? C71 C72 1.524(18) . ? C71 C72B 1.532(11) . ? C71B C72B 1.550(15) . ? C71B C72 1.85(3) . ? C72 C73 1.451(18) . ? C72 C73B 1.78(4) . ? C72B C73B 1.430(16) . ? C72B C73 1.543(12) . ? C73 C73B 1.71(2) . ? O74 C75 1.427(7) . ? O74 C79 1.433(8) . ? C75 C76 1.504(8) . ? C75 H75B 0.9700 . ? C75 H75A 0.9700 . ? C76 O77 1.430(7) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? O77 C78 1.429(7) . ? C78 C79 1.489(8) . ? C78 H78B 0.9700 . ? C78 H78A 0.9700 . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? O80 C81 1.397(8) . ? O80 C85 1.425(8) . ? C81 C82 1.483(10) . ? C81 H81B 0.9700 . ? C81 H81A 0.9700 . ? C82 O83 1.435(8) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? O83 C84 1.412(7) . ? C84 C85 1.481(9) . ? C84 H84B 0.9700 . ? C84 H84A 0.9700 . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? O9' N10' 1.219(5) . ? N10' O11' 1.231(5) . ? N10' C12' 1.475(6) . ? C12' C17' 1.384(6) . ? C12' C13' 1.391(6) . ? C13' C14' 1.390(7) . ? C13' H13' 0.9300 . ? C14' C15' 1.381(7) . ? C14' H14' 0.9300 . ? C15' C16' 1.387(6) . ? C15' H15' 0.9300 . ? C16' C17' 1.390(6) . ? C16' H16' 0.9300 . ? C17' C18' 1.505(6) . ? C18' O19' 1.229(5) . ? C18' N20' 1.326(6) . ? N20' C21' 1.467(5) . ? N20' H20' 0.8600 . ? C21' C22' 1.506(6) . ? C21' H21C 0.9700 . ? C21' H21D 0.9700 . ? C22' C56' 1.388(6) . ? C22' C23' 1.393(6) . ? C23' C25' 1.406(6) . ? C23' C24' 1.516(6) . ? C24' H24E 0.9600 . ? C24' H24D 0.9600 . ? C24' H24F 0.9600 . ? C25' C39' 1.397(6) . ? C25' C26' 1.508(6) . ? C26' N27' 1.459(5) . ? C26' H26D 0.9700 . ? C26' H26C 0.9700 . ? N27' C28' 1.323(6) . ? N27' H27' 0.8600 . ? C28' O29' 1.234(5) . ? C28' C30' 1.501(6) . ? C30' C31' 1.391(7) . ? C30' C35' 1.397(6) . ? C31' C32' 1.388(7) . ? C31' H31' 0.9300 . ? C32' C33' 1.383(8) . ? C32' H32' 0.9300 . ? C33' C34' 1.386(8) . ? C33' H33' 0.9300 . ? C34' C35' 1.362(7) . ? C34' H34' 0.9300 . ? C35' N36' 1.485(7) . ? N36' O37' 1.213(6) . ? N36' O38' 1.234(6) . ? C39' C41' 1.401(6) . ? C39' C40' 1.513(6) . ? C40' H40D 0.9600 . ? C40' H40F 0.9600 . ? C40' H40E 0.9600 . ? C41' C56' 1.401(6) . ? C41' C42' 1.507(6) . ? C42' N43' 1.460(5) . ? C42' H42D 0.9700 . ? C42' H42C 0.9700 . ? N43' C44' 1.334(6) . ? N43' H43' 0.8600 . ? C44' O45' 1.235(5) . ? C44' C46' 1.520(6) . ? C46' C47' 1.385(6) . ? C46' C51' 1.386(6) . ? C47' C48' 1.383(7) . ? C47' H47' 0.9300 . ? C48' C49' 1.377(7) . ? C48' H48' 0.9300 . ? C49' C50' 1.381(7) . ? C49' H49' 0.9300 . ? C50' C51' 1.377(7) . ? C50' H50' 0.9300 . ? C51' N52' 1.476(6) . ? N52' O53' 1.218(6) . ? N52' O54' 1.224(6) . ? C55' C56' 1.510(6) . ? C55' H55E 0.9600 . ? C55' H55F 0.9600 . ? C55' H55D 0.9600 . ? N57' C58' 1.509(6) . ? N57' C70' 1.510(6) . ? N57' C66' 1.511(6) . ? N57' C62' 1.536(6) . ? C58' C59' 1.504(6) . ? C58' H58A 0.9700 . ? C58' H58B 0.9700 . ? C59' C60' 1.509(6) . ? C59' H59A 0.9700 . ? C59' H59B 0.9700 . ? C60' C61' 1.510(7) . ? C60' H60B 0.9700 . ? C60' H60A 0.9700 . ? C61' H61B 0.9600 . ? C61' H61A 0.9600 . ? C61' H61C 0.9600 . ? C62' C63' 1.483(7) . ? C62' H62A 0.9700 . ? C62' H62B 0.9700 . ? C63' C64' 1.534(8) . ? C63' H63A 0.9700 . ? C63' H63B 0.9700 . ? C64' C65' 1.558(10) . ? C64' H64A 0.9700 . ? C64' H64B 0.9700 . ? C65' H65A 0.9600 . ? C65' H65B 0.9600 . ? C65' H65C 0.9600 . ? C66' C67' 1.507(7) . ? C66' H66B 0.9700 . ? C66' H66A 0.9700 . ? C67' C68' 1.506(7) . ? C67' H67B 0.9700 . ? C67' H67A 0.9700 . ? C68' C69' 1.491(9) . ? C68' H68B 0.9700 . ? C68' H68A 0.9700 . ? C69' H69B 0.9600 . ? C69' H69A 0.9600 . ? C69' H69C 0.9600 . ? C70' C71' 1.492(7) . ? C70' H70B 0.9700 . ? C70' H70A 0.9700 . ? C71' C72' 1.522(8) . ? C71' H71B 0.9700 . ? C71' H71A 0.9700 . ? C72' C73' 1.520(9) . ? C72' H72A 0.9700 . ? C72' H72B 0.9700 . ? C73' H73A 0.9600 . ? C73' H73B 0.9600 . ? C73' H73C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H3A O3 H3B 109(6) . . ? H4A O4 H4B 104(6) . . ? H5A O5 H5B 98(5) . . ? H6A O6 H6B 107(6) . . ? H7A O7 H7B 102(6) . . ? H8A O8 H8B 97(5) . . ? O9 N10 O11 124.9(4) . . ? O9 N10 C12 117.7(4) . . ? O11 N10 C12 117.2(5) . . ? C13 C12 C17 122.7(4) . . ? C13 C12 N10 117.4(4) . . ? C17 C12 N10 119.9(4) . . ? C14 C13 C12 118.4(5) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 121.0(5) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 119.7(5) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.4(4) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C12 116.7(4) . . ? C16 C17 C18 123.6(4) . . ? C12 C17 C18 119.5(4) . . ? O19 C18 N20 122.1(4) . . ? O19 C18 C17 119.4(4) . . ? N20 C18 C17 118.5(4) . . ? C18 N20 C21 119.1(4) . . ? C18 N20 H20 120.4 . . ? C21 N20 H20 120.4 . . ? N20 C21 C22 111.7(3) . . ? N20 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? N20 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? H21B C21 H21A 107.9 . . ? C55 C22 C23 120.6(4) . . ? C55 C22 C21 120.6(4) . . ? C23 C22 C21 118.7(4) . . ? C25 C23 C22 119.5(4) . . ? C25 C23 C24 121.4(4) . . ? C22 C23 C24 119.0(4) . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? H24C C24 H24A 109.5 . . ? C23 C25 C39 120.0(4) . . ? C23 C25 C26 121.2(4) . . ? C39 C25 C26 118.8(4) . . ? N27 C26 C25 110.5(3) . . ? N27 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? N27 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C28 N27 C26 120.5(4) . . ? C28 N27 H27 119.8 . . ? C26 N27 H27 119.8 . . ? O29 C28 N27 123.9(4) . . ? O29 C28 C30 120.6(4) . . ? N27 C28 C30 115.5(4) . . ? C35 C30 C31 116.7(4) . . ? C35 C30 C28 121.4(4) . . ? C31 C30 C28 121.7(4) . . ? C32 C31 C30 119.9(5) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 121.6(6) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C32 C33 C34 120.0(5) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 117.7(5) . . ? C35 C34 H34 121.1 . . ? C33 C34 H34 121.1 . . ? C34 C35 C30 123.9(5) . . ? C34 C35 N36 117.8(5) . . ? C30 C35 N36 118.1(4) . . ? O38 N36 O37 123.9(6) . . ? O38 N36 C35 118.1(6) . . ? O37 N36 C35 118.0(5) . . ? C41 C39 C25 119.7(4) . . ? C41 C39 C40 120.0(4) . . ? C25 C39 C40 120.3(4) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? H40C C40 H40B 109.5 . . ? C55 C41 C39 120.7(4) . . ? C55 C41 C42 119.5(4) . . ? C39 C41 C42 119.8(4) . . ? N43 C42 C41 112.2(3) . . ? N43 C42 H42A 109.2 . . ? C41 C42 H42A 109.2 . . ? N43 C42 H42B 109.2 . . ? C41 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C44 N43 C42 120.9(4) . . ? C44 N43 H43 119.6 . . ? C42 N43 H43 119.6 . . ? O45 C44 N43 123.4(4) . . ? O45 C44 C46 119.7(4) . . ? N43 C44 C46 116.8(4) . . ? C51 C46 C47 117.1(4) . . ? C51 C46 C44 121.7(4) . . ? C47 C46 C44 120.9(4) . . ? C48 C47 C46 120.7(5) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C49 C48 C47 120.4(5) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C48 C49 C50 120.4(5) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C51 C50 C49 118.1(5) . . ? C51 C50 H50 121.0 . . ? C49 C50 H50 121.0 . . ? C50 C51 C46 123.3(4) . . ? C50 C51 N52 116.9(4) . . ? C46 C51 N52 119.6(4) . . ? O54 N52 O53 123.6(4) . . ? O54 N52 C51 119.0(4) . . ? O53 N52 C51 117.3(4) . . ? C22 C55 C41 119.4(4) . . ? C22 C55 C56 120.3(4) . . ? C41 C55 C56 120.2(4) . . ? C55 C56 H56C 109.5 . . ? C55 C56 H56A 109.5 . . ? H56C C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56C C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C70B N57 C62 141.7(7) . . ? C70B N57 C58B 114.0(7) . . ? C62 N57 C58B 100.0(6) . . ? C70B N57 C66 93.7(7) . . ? C62 N57 C66 111.6(5) . . ? C58B N57 C66 76.4(5) . . ? C70B N57 C58 85.8(6) . . ? C62 N57 C58 112.2(5) . . ? C58B N57 C58 40.1(5) . . ? C66 N57 C58 106.3(5) . . ? C70B N57 C70 33.1(5) . . ? C62 N57 C70 108.8(5) . . ? C58B N57 C70 143.7(6) . . ? C66 N57 C70 111.3(5) . . ? C58 N57 C70 106.6(5) . . ? C70B N57 C66B 114.4(8) . . ? C62 N57 C66B 69.1(6) . . ? C58B N57 C66B 106.3(7) . . ? C66 N57 C66B 48.7(6) . . ? C58 N57 C66B 146.2(7) . . ? C70 N57 C66B 104.4(6) . . ? C70B N57 C62B 106.1(8) . . ? C62 N57 C62B 42.8(6) . . ? C58B N57 C62B 109.7(7) . . ? C66 N57 C62B 153.7(7) . . ? C58 N57 C62B 92.6(6) . . ? C70 N57 C62B 79.5(6) . . ? C66B N57 C62B 106.1(8) . . ? C58B C58 C59B 94.3(10) . . ? C58B C58 C59 50.0(7) . . ? C59B C58 C59 49.1(8) . . ? C58B C58 N57 68.8(7) . . ? C59B C58 N57 162.2(10) . . ? C59 C58 N57 113.2(6) . . ? C58 C58B C59 86.8(9) . . ? C58 C58B N57 71.1(7) . . ? C59 C58B N57 144.2(10) . . ? C58 C58B C59B 43.1(7) . . ? C59 C58B C59B 48.0(7) . . ? N57 C58B C59B 114.1(8) . . ? C58 C58B C66 110.5(9) . . ? C59 C58B C66 161.6(10) . . ? N57 C58B C66 52.1(4) . . ? C59B C58B C66 144.7(9) . . ? C59B C59 C58B 83.2(9) . . ? C59B C59 C60B 69.3(8) . . ? C58B C59 C60B 141.8(10) . . ? C59B C59 C58 43.8(6) . . ? C58B C59 C58 43.2(6) . . ? C60B C59 C58 112.9(7) . . ? C59B C59 C60 67.3(8) . . ? C58B C59 C60 150.3(10) . . ? C60B C59 C60 27.4(5) . . ? C58 C59 C60 108.0(7) . . ? C59B C59 C61B 101.9(9) . . ? C58B C59 C61B 169.9(10) . . ? C60B C59 C61B 48.0(6) . . ? C58 C59 C61B 137.6(8) . . ? C60 C59 C61B 35.2(7) . . ? C58 C59B C59 87.1(10) . . ? C58 C59B C60B 152.3(12) . . ? C59 C59B C60B 65.9(8) . . ? C58 C59B C60 147.1(13) . . ? C59 C59B C60 69.0(8) . . ? C60B C59B C60 27.3(5) . . ? C58 C59B C58B 42.5(7) . . ? C59 C59B C58B 48.9(7) . . ? C60B C59B C58B 110.1(9) . . ? C60 C59B C58B 117.8(10) . . ? C60B C60 C61B 103.0(17) . . ? C60B C60 C61 91.2(14) . . ? C61B C60 C61 23.1(10) . . ? C60B C60 C59B 75.8(13) . . ? C61B C60 C59B 136.9(14) . . ? C61 C60 C59B 152.6(10) . . ? C60B C60 C59 71.4(12) . . ? C61B C60 C59 94.2(13) . . ? C61 C60 C59 109.4(9) . . ? C59B C60 C59 43.8(6) . . ? C60 C60B C59 81.2(12) . . ? C60 C60B C61B 49.0(13) . . ? C59 C60B C61B 84.3(10) . . ? C60 C60B C59B 76.9(13) . . ? C59 C60B C59B 44.8(6) . . ? C61B C60B C59B 112.1(11) . . ? C60 C60B C61 63.5(12) . . ? C59 C60B C61 103.6(7) . . ? C61B C60B C61 22.0(8) . . ? C59B C60B C61 133.9(9) . . ? C61B C61 C60 45.6(17) . . ? C61B C61 C60B 61.8(17) . . ? C60 C61 C60B 25.3(5) . . ? C61 C61B C60 111(2) . . ? C61 C61B C60B 96(2) . . ? C60 C61B C60B 28.0(7) . . ? C61 C61B C59 136(2) . . ? C60 C61B C59 50.6(9) . . ? C60B C61B C59 47.7(7) . . ? C62B C62 C63B 77.8(10) . . ? C62B C62 N57 72.1(8) . . ? C63B C62 N57 139.7(11) . . ? C62B C62 C63 45.5(8) . . ? C63B C62 C63 32.2(8) . . ? N57 C62 C63 112.9(7) . . ? C62B C62 C66B 121.0(10) . . ? C63B C62 C66B 160.8(12) . . ? N57 C62 C66B 57.4(5) . . ? C63 C62 C66B 166.2(9) . . ? C63 C62B C62 88.2(12) . . ? C63 C62B C63B 31.6(8) . . ? C62 C62B C63B 56.6(9) . . ? C63 C62B N57 142.3(13) . . ? C62 C62B N57 65.1(8) . . ? C63B C62B N57 116.2(11) . . ? C63 C62B C70 167.5(13) . . ? C62 C62B C70 101.8(10) . . ? C63B C62B C70 157.3(12) . . ? N57 C62B C70 50.2(5) . . ? C63B C63 C62B 103.8(16) . . ? C63B C63 C64B 79.5(14) . . ? C62B C63 C64B 162.2(14) . . ? C63B C63 C62 57.6(13) . . ? C62B C63 C62 46.3(8) . . ? C64B C63 C62 133.9(10) . . ? C63B C63 C64 63.0(14) . . ? C62B C63 C64 136.2(13) . . ? C64B C63 C64 30.3(6) . . ? C62 C63 C64 107.0(9) . . ? C63 C63B C62 90.2(15) . . ? C63 C63B C64 85.6(16) . . ? C62 C63B C64 135.3(16) . . ? C63 C63B C64B 67.7(15) . . ? C62 C63B C64B 152.1(16) . . ? C64 C63B C64B 31.6(7) . . ? C63 C63B C62B 44.6(11) . . ? C62 C63B C62B 45.6(8) . . ? C64 C63B C62B 116.2(14) . . ? C64B C63B C62B 110.4(14) . . ? C64B C64 C63B 80.4(15) . . ? C64B C64 C65 47.4(14) . . ? C63B C64 C65 127.2(14) . . ? C64B C64 C63 63.2(14) . . ? C63B C64 C63 31.4(7) . . ? C65 C64 C63 108.4(11) . . ? C64 C64B C65 102.4(18) . . ? C64 C64B C63 86.5(15) . . ? C65 C64B C63 159.1(17) . . ? C64 C64B C63B 68.0(15) . . ? C65 C64B C63B 167.3(17) . . ? C63 C64B C63B 32.8(7) . . ? C64 C64B C65B 177(2) . . ? C65 C64B C65B 75.1(13) . . ? C63 C64B C65B 96.6(12) . . ? C63B C64B C65B 114.1(14) . . ? C64B C65 C64 30.2(8) . . ? C64B C65 C65B 62.4(11) . . ? C64 C65 C65B 92.5(12) . . ? C64B C65B C65 42.5(8) . . ? C67B C66 C66B 74.8(9) . . ? C67B C66 C67 23.7(9) . . ? C66B C66 C67 53.9(7) . . ? C67B C66 N57 135.6(10) . . ? C66B C66 N57 66.4(6) . . ? C67 C66 N57 111.8(6) . . ? C67B C66 C58B 162.1(11) . . ? C66B C66 C58B 100.2(8) . . ? C67 C66 C58B 153.7(8) . . ? N57 C66 C58B 51.5(4) . . ? C66 C66B C67 73.2(9) . . ? C66 C66B C67B 51.3(8) . . ? C67 C66B C67B 24.5(8) . . ? C66 C66B N57 64.9(7) . . ? C67 C66B N57 126.1(11) . . ? C67B C66B N57 113.0(10) . . ? C66 C66B C62 111.9(9) . . ? C67 C66B C62 170.6(13) . . ? C67B C66B C62 162.8(12) . . ? N57 C66B C62 53.5(5) . . ? C67B C67 C66B 98(2) . . ? C67B C67 C68B 88.5(19) . . ? C66B C67 C68B 137.4(13) . . ? C67B C67 C66 50.9(16) . . ? C66B C67 C66 52.9(7) . . ? C68B C67 C66 136.4(11) . . ? C67B C67 C68 55.5(17) . . ? C66B C67 C68 147.2(12) . . ? C68B C67 C68 38.0(7) . . ? C66 C67 C68 106.4(9) . . ? C67 C67B C66 105(2) . . ? C67 C67B C68 101(2) . . ? C66 C67B C68 153.4(18) . . ? C67 C67B C66B 57.0(17) . . ? C66 C67B C66B 53.9(8) . . ? C68 C67B C66B 150.3(15) . . ? C67 C67B C68B 66.8(18) . . ? C66 C67B C68B 162.0(16) . . ? C68 C67B C68B 39.7(8) . . ? C66B C67B C68B 110.9(13) . . ? C68B C68 C67B 81.1(12) . . ? C68B C68 C69B 74.9(12) . . ? C67B C68 C69B 153.7(14) . . ? C68B C68 C69 114(2) . . ? C67B C68 C69 112.9(18) . . ? C69B C68 C69 68.8(15) . . ? C68B C68 C67 61.2(11) . . ? C67B C68 C67 23.3(8) . . ? C69B C68 C67 130.4(11) . . ? C69 C68 C67 108.0(16) . . ? C68 C68B C67 80.7(12) . . ? C68 C68B C69B 64.8(12) . . ? C67 C68B C69B 138.4(15) . . ? C68 C68B C67B 59.3(11) . . ? C67 C68B C67B 24.7(8) . . ? C69B C68B C67B 123.1(14) . . ? C68 C69 C69B 53.8(11) . . ? C68 C69B C68B 40.3(8) . . ? C68 C69B C69 57.4(10) . . ? C68B C69B C69 83.8(14) . . ? C70B C70 C71B 92.2(13) . . ? C70B C70 C71 50.8(9) . . ? C71B C70 C71 50.4(8) . . ? C70B C70 N57 67.6(9) . . ? C71B C70 N57 131.7(10) . . ? C71 C70 N57 117.1(6) . . ? C70B C70 C62B 109.0(11) . . ? C71B C70 C62B 153.6(11) . . ? C71 C70 C62B 155.9(7) . . ? N57 C70 C62B 50.3(5) . . ? C70 C70B C71 94.3(12) . . ? C70 C70B N57 79.2(10) . . ? C71 C70B N57 164.7(12) . . ? C70 C70B C71B 53.3(11) . . ? C71 C70B C71B 50.3(8) . . ? N57 C70B C71B 116.3(10) . . ? C70B C71 C71B 80.5(10) . . ? C70B C71 C70 34.9(7) . . ? C71B C71 C70 52.5(9) . . ? C70B C71 C72 146.0(13) . . ? C71B C71 C72 85.2(16) . . ? C70 C71 C72 114.4(11) . . ? C70B C71 C72B 141.4(10) . . ? C71B C71 C72B 68.2(8) . . ? C70 C71 C72B 106.6(6) . . ? C72 C71 C72B 18.7(14) . . ? C71 C71B C70 77.2(10) . . ? C71 C71B C70B 49.2(8) . . ? C70 C71B C70B 34.5(7) . . ? C71 C71B C72B 66.5(9) . . ? C70 C71B C72B 122.2(13) . . ? C70B C71B C72B 112.2(11) . . ? C71 C71B C72 55.1(11) . . ? C70 C71B C72 110.1(15) . . ? C70B C71B C72 99.1(13) . . ? C72B C71B C72 13.3(11) . . ? C73 C72 C71 118.6(16) . . ? C73 C72 C73B 62.8(13) . . ? C71 C72 C73B 118(2) . . ? C73 C72 C71B 96.5(16) . . ? C71 C72 C71B 39.7(8) . . ? C73B C72 C71B 78.9(18) . . ? C73B C72B C71 146.8(13) . . ? C73B C72B C73 69.9(11) . . ? C71 C72B C73 112.6(7) . . ? C73B C72B C71B 101.5(13) . . ? C71 C72B C71B 45.3(7) . . ? C73 C72B C71B 106.5(9) . . ? C72 C73 C72B 18.7(15) . . ? C72 C73 C73B 68.1(16) . . ? C72B C73 C73B 51.9(7) . . ? C72B C73B C73 58.2(9) . . ? C72B C73B C72 12.6(9) . . ? C73 C73B C72 49.1(9) . . ? C75 O74 C79 109.6(5) . . ? O74 C75 C76 111.3(5) . . ? O74 C75 H75B 109.4 . . ? C76 C75 H75B 109.4 . . ? O74 C75 H75A 109.4 . . ? C76 C75 H75A 109.4 . . ? H75B C75 H75A 108.0 . . ? O77 C76 C75 110.5(5) . . ? O77 C76 H76A 109.6 . . ? C75 C76 H76A 109.6 . . ? O77 C76 H76B 109.6 . . ? C75 C76 H76B 109.6 . . ? H76A C76 H76B 108.1 . . ? C78 O77 C76 109.3(5) . . ? O77 C78 C79 111.2(5) . . ? O77 C78 H78B 109.4 . . ? C79 C78 H78B 109.4 . . ? O77 C78 H78A 109.4 . . ? C79 C78 H78A 109.4 . . ? H78B C78 H78A 108.0 . . ? O74 C79 C78 110.5(5) . . ? O74 C79 H79A 109.6 . . ? C78 C79 H79A 109.6 . . ? O74 C79 H79B 109.6 . . ? C78 C79 H79B 109.6 . . ? H79A C79 H79B 108.1 . . ? C81 O80 C85 110.1(6) . . ? O80 C81 C82 112.3(6) . . ? O80 C81 H81B 109.1 . . ? C82 C81 H81B 109.1 . . ? O80 C81 H81A 109.1 . . ? C82 C81 H81A 109.1 . . ? H81B C81 H81A 107.9 . . ? O83 C82 C81 110.8(6) . . ? O83 C82 H82A 109.5 . . ? C81 C82 H82A 109.5 . . ? O83 C82 H82B 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 108.1 . . ? C84 O83 C82 110.1(5) . . ? O83 C84 C85 110.6(6) . . ? O83 C84 H84B 109.5 . . ? C85 C84 H84B 109.5 . . ? O83 C84 H84A 109.5 . . ? C85 C84 H84A 109.5 . . ? H84B C84 H84A 108.1 . . ? O80 C85 C84 110.8(6) . . ? O80 C85 H85A 109.5 . . ? C84 C85 H85A 109.5 . . ? O80 C85 H85B 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 108.1 . . ? O9' N10' O11' 124.1(4) . . ? O9' N10' C12' 118.4(4) . . ? O11' N10' C12' 117.5(4) . . ? C17' C12' C13' 123.7(4) . . ? C17' C12' N10' 119.9(4) . . ? C13' C12' N10' 116.4(4) . . ? C14' C13' C12' 117.6(4) . . ? C14' C13' H13' 121.2 . . ? C12' C13' H13' 121.2 . . ? C15' C14' C13' 120.5(4) . . ? C15' C14' H14' 119.8 . . ? C13' C14' H14' 119.8 . . ? C14' C15' C16' 120.0(4) . . ? C14' C15' H15' 120.0 . . ? C16' C15' H15' 120.0 . . ? C15' C16' C17' 121.5(4) . . ? C15' C16' H16' 119.3 . . ? C17' C16' H16' 119.3 . . ? C12' C17' C16' 116.7(4) . . ? C12' C17' C18' 121.6(4) . . ? C16' C17' C18' 121.4(4) . . ? O19' C18' N20' 123.8(4) . . ? O19' C18' C17' 120.1(4) . . ? N20' C18' C17' 116.1(4) . . ? C18' N20' C21' 121.3(4) . . ? C18' N20' H20' 119.3 . . ? C21' N20' H20' 119.3 . . ? N20' C21' C22' 112.7(4) . . ? N20' C21' H21C 109.1 . . ? C22' C21' H21C 109.1 . . ? N20' C21' H21D 109.1 . . ? C22' C21' H21D 109.1 . . ? H21C C21' H21D 107.8 . . ? C56' C22' C23' 121.3(4) . . ? C56' C22' C21' 120.0(4) . . ? C23' C22' C21' 118.6(4) . . ? C22' C23' C25' 119.2(4) . . ? C22' C23' C24' 120.0(4) . . ? C25' C23' C24' 120.8(4) . . ? C23' C24' H24E 109.5 . . ? C23' C24' H24D 109.5 . . ? H24E C24' H24D 109.5 . . ? C23' C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? C39' C25' C23' 120.3(4) . . ? C39' C25' C26' 120.8(4) . . ? C23' C25' C26' 118.9(4) . . ? N27' C26' C25' 110.8(3) . . ? N27' C26' H26D 109.5 . . ? C25' C26' H26D 109.5 . . ? N27' C26' H26C 109.5 . . ? C25' C26' H26C 109.5 . . ? H26D C26' H26C 108.1 . . ? C28' N27' C26' 119.9(4) . . ? C28' N27' H27' 120.0 . . ? C26' N27' H27' 120.0 . . ? O29' C28' N27' 124.2(4) . . ? O29' C28' C30' 120.2(4) . . ? N27' C28' C30' 115.6(4) . . ? C31' C30' C35' 117.9(4) . . ? C31' C30' C28' 122.6(4) . . ? C35' C30' C28' 119.5(4) . . ? C32' C31' C30' 119.5(5) . . ? C32' C31' H31' 120.2 . . ? C30' C31' H31' 120.2 . . ? C33' C32' C31' 120.5(5) . . ? C33' C32' H32' 119.7 . . ? C31' C32' H32' 119.7 . . ? C32' C33' C34' 121.0(5) . . ? C32' C33' H33' 119.5 . . ? C34' C33' H33' 119.5 . . ? C35' C34' C33' 117.6(5) . . ? C35' C34' H34' 121.2 . . ? C33' C34' H34' 121.2 . . ? C34' C35' C30' 123.5(5) . . ? C34' C35' N36' 118.2(4) . . ? C30' C35' N36' 118.2(4) . . ? O37' N36' O38' 125.6(5) . . ? O37' N36' C35' 118.9(4) . . ? O38' N36' C35' 115.6(5) . . ? C25' C39' C41' 119.2(4) . . ? C25' C39' C40' 121.3(4) . . ? C41' C39' C40' 119.4(4) . . ? C39' C40' H40D 109.5 . . ? C39' C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? C39' C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? H40F C40' H40E 109.5 . . ? C56' C41' C39' 120.8(4) . . ? C56' C41' C42' 120.4(4) . . ? C39' C41' C42' 118.8(4) . . ? N43' C42' C41' 111.9(3) . . ? N43' C42' H42D 109.2 . . ? C41' C42' H42D 109.2 . . ? N43' C42' H42C 109.2 . . ? C41' C42' H42C 109.2 . . ? H42D C42' H42C 107.9 . . ? C44' N43' C42' 118.9(4) . . ? C44' N43' H43' 120.5 . . ? C42' N43' H43' 120.5 . . ? O45' C44' N43' 122.9(4) . . ? O45' C44' C46' 119.9(4) . . ? N43' C44' C46' 117.2(4) . . ? C47' C46' C51' 117.4(4) . . ? C47' C46' C44' 123.4(4) . . ? C51' C46' C44' 119.1(4) . . ? C48' C47' C46' 120.6(4) . . ? C48' C47' H47' 119.7 . . ? C46' C47' H47' 119.7 . . ? C49' C48' C47' 120.6(5) . . ? C49' C48' H48' 119.7 . . ? C47' C48' H48' 119.7 . . ? C48' C49' C50' 119.9(5) . . ? C48' C49' H49' 120.0 . . ? C50' C49' H49' 120.0 . . ? C51' C50' C49' 118.6(5) . . ? C51' C50' H50' 120.7 . . ? C49' C50' H50' 120.7 . . ? C50' C51' C46' 122.8(4) . . ? C50' C51' N52' 116.9(4) . . ? C46' C51' N52' 120.2(4) . . ? O53' N52' O54' 124.9(5) . . ? O53' N52' C51' 118.0(5) . . ? O54' N52' C51' 116.9(5) . . ? C56' C55' H55E 109.5 . . ? C56' C55' H55F 109.5 . . ? H55E C55' H55F 109.5 . . ? C56' C55' H55D 109.5 . . ? H55E C55' H55D 109.5 . . ? H55F C55' H55D 109.5 . . ? C22' C56' C41' 119.0(4) . . ? C22' C56' C55' 120.4(4) . . ? C41' C56' C55' 120.6(4) . . ? C58' N57' C70' 109.5(3) . . ? C58' N57' C66' 108.7(3) . . ? C70' N57' C66' 112.0(4) . . ? C58' N57' C62' 110.5(4) . . ? C70' N57' C62' 107.7(4) . . ? C66' N57' C62' 108.4(4) . . ? C59' C58' N57' 117.5(4) . . ? C59' C58' H58A 107.9 . . ? N57' C58' H58A 107.9 . . ? C59' C58' H58B 107.9 . . ? N57' C58' H58B 107.9 . . ? H58A C58' H58B 107.2 . . ? C58' C59' C60' 111.2(4) . . ? C58' C59' H59A 109.4 . . ? C60' C59' H59A 109.4 . . ? C58' C59' H59B 109.4 . . ? C60' C59' H59B 109.4 . . ? H59A C59' H59B 108.0 . . ? C59' C60' C61' 115.0(4) . . ? C59' C60' H60B 108.5 . . ? C61' C60' H60B 108.5 . . ? C59' C60' H60A 108.5 . . ? C61' C60' H60A 108.5 . . ? H60B C60' H60A 107.5 . . ? C60' C61' H61B 109.5 . . ? C60' C61' H61A 109.5 . . ? H61B C61' H61A 109.5 . . ? C60' C61' H61C 109.5 . . ? H61B C61' H61C 109.5 . . ? H61A C61' H61C 109.5 . . ? C63' C62' N57' 117.4(4) . . ? C63' C62' H62A 108.0 . . ? N57' C62' H62A 108.0 . . ? C63' C62' H62B 108.0 . . ? N57' C62' H62B 108.0 . . ? H62A C62' H62B 107.2 . . ? C62' C63' C64' 110.2(5) . . ? C62' C63' H63A 109.6 . . ? C64' C63' H63A 109.6 . . ? C62' C63' H63B 109.6 . . ? C64' C63' H63B 109.6 . . ? H63A C63' H63B 108.1 . . ? C63' C64' C65' 112.3(5) . . ? C63' C64' H64A 109.1 . . ? C65' C64' H64A 109.1 . . ? C63' C64' H64B 109.1 . . ? C65' C64' H64B 109.1 . . ? H64A C64' H64B 107.9 . . ? C64' C65' H65A 109.5 . . ? C64' C65' H65B 109.5 . . ? H65A C65' H65B 109.5 . . ? C64' C65' H65C 109.5 . . ? H65A C65' H65C 109.5 . . ? H65B C65' H65C 109.5 . . ? C67' C66' N57' 116.4(4) . . ? C67' C66' H66B 108.2 . . ? N57' C66' H66B 108.2 . . ? C67' C66' H66A 108.2 . . ? N57' C66' H66A 108.2 . . ? H66B C66' H66A 107.3 . . ? C68' C67' C66' 110.9(5) . . ? C68' C67' H67B 109.5 . . ? C66' C67' H67B 109.5 . . ? C68' C67' H67A 109.5 . . ? C66' C67' H67A 109.5 . . ? H67B C67' H67A 108.0 . . ? C69' C68' C67' 113.4(6) . . ? C69' C68' H68B 108.9 . . ? C67' C68' H68B 108.9 . . ? C69' C68' H68A 108.9 . . ? C67' C68' H68A 108.9 . . ? H68B C68' H68A 107.7 . . ? C68' C69' H69B 109.5 . . ? C68' C69' H69A 109.5 . . ? H69B C69' H69A 109.5 . . ? C68' C69' H69C 109.5 . . ? H69B C69' H69C 109.5 . . ? H69A C69' H69C 109.5 . . ? C71' C70' N57' 116.5(4) . . ? C71' C70' H70B 108.2 . . ? N57' C70' H70B 108.2 . . ? C71' C70' H70A 108.2 . . ? N57' C70' H70A 108.2 . . ? H70B C70' H70A 107.3 . . ? C70' C71' C72' 112.4(5) . . ? C70' C71' H71B 109.1 . . ? C72' C71' H71B 109.1 . . ? C70' C71' H71A 109.1 . . ? C72' C71' H71A 109.1 . . ? H71B C71' H71A 107.9 . . ? C73' C72' C71' 110.3(5) . . ? C73' C72' H72A 109.6 . . ? C71' C72' H72A 109.6 . . ? C73' C72' H72B 109.6 . . ? C71' C72' H72B 109.6 . . ? H72A C72' H72B 108.1 . . ? C72' C73' H73A 109.5 . . ? C72' C73' H73B 109.5 . . ? H73A C73' H73B 109.5 . . ? C72' C73' H73C 109.5 . . ? H73A C73' H73C 109.5 . . ? H73B C73' H73C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3B F1 0.88(2) 1.78(2) 2.655(4) 171(8) 1 O4 H4A F1 0.88(2) 1.79(2) 2.673(4) 179(6) 1_455 O4 H4B F1 0.87(2) 2.09(3) 2.912(4) 157(6) 2_665 O5 H5A O8 0.87(7) 1.95(7) 2.808(5) 172(6) 1 O5 H5B F2 0.79(6) 1.90(6) 2.675(5) 169(5) 1 O6 H6A F2 0.89(2) 2.10(3) 2.941(4) 158(5) 2_656 O6 H6B F2 0.88(2) 1.82(2) 2.694(4) 172(7) 1 O7 H7A O3 0.80(7) 2.01(7) 2.809(5) 177(6) 2_766 O7 H7B F1 0.74(6) 1.97(6) 2.690(5) 166(6) 1_556 O8 H8A F2 0.80(5) 1.88(5) 2.669(5) 168(5) 2_656 N20 H20 F1 0.86 1.95 2.763(4) 157.6 1_556 N27 H27 O4 0.86 1.96 2.807(5) 168.6 2_666 N43 H43 O7 0.86 2.03 2.884(5) 170.5 1 N20' H20' O5 0.86 2.05 2.905(5) 170.9 1_565 N27' H27' O6 0.86 2.01 2.845(5) 165.0 2_666 N43' H43' F2 0.86 1.96 2.773(4) 157.7 1_565 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.67 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.694 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.079 # Attachment 'Complex_2.cif' data_tonacl _database_code_depnum_ccdc_archive 'CCDC 733119' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H68 Cl N7 O10' _chemical_formula_weight 950.55 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' Cl Cl 0.1484 0.1585 '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 12.945(2) _cell_length_b 14.4605(10) _cell_length_c 15.5879(12) _cell_angle_alpha 117.393(2) _cell_angle_beta 95.911(2) _cell_angle_gamma 101.767(2) _cell_volume 2470.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4097 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 22.40 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9456 _exptl_absorpt_correction_T_max 0.9750 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'BRUKER CCD AREA DETECTOR' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19525 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 22.95 _reflns_number_total 6810 _reflns_number_gt 5194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'MERCURY 1.4' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+1.4252P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6810 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.18004(6) 0.78107(5) 0.40388(5) 0.03209(18) Uani 1 1 d . . . O2 O 0.9367(2) 0.7752(2) 0.34301(17) 0.0605(7) Uani 1 1 d . . . H2B H 0.933(4) 0.823(4) 0.392(3) 0.111(19) Uiso 1 1 d . . . H2A H 1.002(4) 0.767(3) 0.352(3) 0.117(17) Uiso 1 1 d . . . C3 C 0.0435(2) 0.7817(2) 0.07971(18) 0.0277(6) Uani 1 1 d . . . H3A H 0.0669 0.8522 0.1380 0.042 Uiso 1 1 calc R . . H3B H -0.0317 0.7655 0.0515 0.042 Uiso 1 1 calc R . . H3C H 0.0854 0.7811 0.0322 0.042 Uiso 1 1 calc R . . C4 C 0.05940(19) 0.69706(18) 0.10724(16) 0.0194(6) Uani 1 1 d . . . C5 C 0.16450(19) 0.69655(19) 0.13988(16) 0.0205(6) Uani 1 1 d . . . C6 C 0.2602(2) 0.7909(2) 0.16267(17) 0.0266(6) Uani 1 1 d . . . H6A H 0.3223 0.7652 0.1439 0.032 Uiso 1 1 calc R . . H6B H 0.2425 0.8266 0.1259 0.032 Uiso 1 1 calc R . . N7 N 0.28498(17) 0.86707(17) 0.26964(15) 0.0246(5) Uani 1 1 d . . . H7 H 0.256(2) 0.844(2) 0.3091(19) 0.035(8) Uiso 1 1 d . . . C8 C 0.34265(19) 0.9700(2) 0.30741(18) 0.0228(6) Uani 1 1 d . . . O9 O 0.38857(14) 1.00423(13) 0.25796(12) 0.0302(4) Uani 1 1 d . . . C10 C 0.35780(19) 1.04527(19) 0.41705(17) 0.0221(6) Uani 1 1 d . . . C11 C 0.4628(2) 1.0874(2) 0.47397(19) 0.0289(6) Uani 1 1 d . . . H11 H 0.5186 1.0667 0.4434 0.035 Uiso 1 1 calc R . . C12 C 0.4870(2) 1.1592(2) 0.5749(2) 0.0349(7) Uani 1 1 d . . . H12 H 0.5582 1.1860 0.6112 0.042 Uiso 1 1 calc R . . C13 C 0.4058(2) 1.1908(2) 0.6212(2) 0.0378(7) Uani 1 1 d . . . H13 H 0.4220 1.2388 0.6891 0.045 Uiso 1 1 calc R . . C14 C 0.3001(2) 1.1517(2) 0.56735(19) 0.0346(7) Uani 1 1 d . . . H14 H 0.2448 1.1730 0.5984 0.042 Uiso 1 1 calc R . . C15 C 0.2776(2) 1.0800(2) 0.46627(18) 0.0264(6) Uani 1 1 d . . . N16 N 0.16432(17) 1.04412(17) 0.41087(16) 0.0305(5) Uani 1 1 d . . . O17 O 0.14835(14) 1.01623(15) 0.32242(13) 0.0375(5) Uani 1 1 d . . . O18 O 0.09222(15) 1.04560(16) 0.45651(14) 0.0424(5) Uani 1 1 d . . . C19 C 0.2929(2) 0.6147(2) 0.19607(19) 0.0311(7) Uani 1 1 d . . . H19B H 0.3015 0.6213 0.2608 0.047 Uiso 1 1 calc R . . H19C H 0.3453 0.6737 0.1984 0.047 Uiso 1 1 calc R . . H19A H 0.3034 0.5470 0.1498 0.047 Uiso 1 1 calc R . . C20 C 0.18014(19) 0.61765(19) 0.16352(16) 0.0209(6) Uani 1 1 d . . . C21 C 0.09039(19) 0.54254(19) 0.16075(16) 0.0198(6) Uani 1 1 d . . . C22 C 0.1093(2) 0.46537(19) 0.19715(16) 0.0237(6) Uani 1 1 d . . . H22B H 0.0489 0.3998 0.1646 0.028 Uiso 1 1 calc R . . H22A H 0.1746 0.4453 0.1808 0.028 Uiso 1 1 calc R . . N23 N 0.12014(16) 0.51774(17) 0.30486(14) 0.0222(5) Uani 1 1 d . . . H23 H 0.1357(19) 0.592(2) 0.3408(18) 0.029(7) Uiso 1 1 d . . . C24 C 0.12850(18) 0.4610(2) 0.35168(17) 0.0215(6) Uani 1 1 d . . . O25 O 0.12652(16) 0.36524(14) 0.30722(12) 0.0369(5) Uani 1 1 d . . . C26 C 0.13573(18) 0.51777(19) 0.46199(17) 0.0204(6) Uani 1 1 d . . . C27 C 0.11187(19) 0.61616(19) 0.51266(17) 0.0228(6) Uani 1 1 d . . . H27 H 0.0949 0.6514 0.4785 0.027 Uiso 1 1 calc R . . C28 C 0.11295(19) 0.6627(2) 0.61307(18) 0.0260(6) Uani 1 1 d . . . H28 H 0.0974 0.7288 0.6457 0.031 Uiso 1 1 calc R . . C29 C 0.1371(2) 0.6109(2) 0.66423(18) 0.0274(6) Uani 1 1 d . . . H29 H 0.1378 0.6423 0.7315 0.033 Uiso 1 1 calc R . . C30 C 0.16029(19) 0.5127(2) 0.61662(18) 0.0271(6) Uani 1 1 d . . . H30 H 0.1760 0.4771 0.6510 0.033 Uiso 1 1 calc R . . C31 C 0.15966(19) 0.46852(19) 0.51713(17) 0.0231(6) Uani 1 1 d . . . N32 N 0.1875(2) 0.36460(19) 0.47279(15) 0.0326(6) Uani 1 1 d . . . O33 O 0.27999(17) 0.36780(17) 0.46139(15) 0.0499(6) Uani 1 1 d . . . O34 O 0.11924(17) 0.28280(16) 0.45598(14) 0.0451(5) Uani 1 1 d . . . C35 C -0.1114(2) 0.4716(2) 0.13929(19) 0.0287(6) Uani 1 1 d . . . H35A H -0.1452 0.4107 0.0744 0.043 Uiso 1 1 calc R . . H35B H -0.1626 0.5111 0.1647 0.043 Uiso 1 1 calc R . . H35C H -0.0878 0.4461 0.1828 0.043 Uiso 1 1 calc R . . C36 C -0.01482(19) 0.54544(19) 0.13298(16) 0.0199(6) Uani 1 1 d . . . C37 C -0.02992(18) 0.61987(18) 0.10246(16) 0.0173(5) Uani 1 1 d . . . C38 C -0.14325(19) 0.62110(19) 0.06822(17) 0.0225(6) Uani 1 1 d . . . H38B H -0.1482 0.6241 0.0071 0.027 Uiso 1 1 calc R . . H38A H -0.1949 0.5546 0.0548 0.027 Uiso 1 1 calc R . . N39 N -0.17059(17) 0.71441(16) 0.14322(16) 0.0212(5) Uani 1 1 d . . . H39 H -0.1451(19) 0.7354(19) 0.1991(18) 0.019(7) Uiso 1 1 d . . . C40 C -0.23013(19) 0.76701(19) 0.11826(18) 0.0216(6) Uani 1 1 d . . . O41 O -0.27091(14) 0.73763(14) 0.03163(12) 0.0315(4) Uani 1 1 d . . . C42 C -0.24196(19) 0.86878(19) 0.20173(17) 0.0202(6) Uani 1 1 d . . . C43 C -0.1535(2) 0.9465(2) 0.27676(18) 0.0263(6) Uani 1 1 d . . . H43 H -0.0866 0.9325 0.2789 0.032 Uiso 1 1 calc R . . C44 C -0.1633(2) 1.0444(2) 0.34818(18) 0.0294(6) Uani 1 1 d . . . H44 H -0.1037 1.0947 0.3988 0.035 Uiso 1 1 calc R . . C45 C -0.2615(2) 1.0675(2) 0.34455(19) 0.0298(6) Uani 1 1 d . . . H45 H -0.2675 1.1337 0.3925 0.036 Uiso 1 1 calc R . . C46 C -0.3510(2) 0.9930(2) 0.27007(18) 0.0258(6) Uani 1 1 d . . . H46 H -0.4170 1.0086 0.2666 0.031 Uiso 1 1 calc R . . C47 C -0.33972(19) 0.89494(19) 0.20125(17) 0.0208(6) Uani 1 1 d . . . N48 N -0.43909(16) 0.81413(18) 0.12796(14) 0.0253(5) Uani 1 1 d . . . O49 O -0.46173(14) 0.72296(15) 0.11809(14) 0.0379(5) Uani 1 1 d . . . O50 O -0.49527(13) 0.84516(14) 0.08437(12) 0.0316(4) Uani 1 1 d . . . N51 N 0.37498(14) 0.21569(15) 0.18188(13) 0.0191(5) Uani 1 1 d . . . C52 C 0.46942(18) 0.22111(19) 0.25283(16) 0.0205(6) Uani 1 1 d . . . H52B H 0.4595 0.1497 0.2465 0.025 Uiso 1 1 calc R . . H52A H 0.5357 0.2382 0.2324 0.025 Uiso 1 1 calc R . . C53 C 0.48361(19) 0.3030(2) 0.36108(17) 0.0268(6) Uani 1 1 d . . . H53B H 0.4192 0.2851 0.3836 0.032 Uiso 1 1 calc R . . H53A H 0.4928 0.3749 0.3687 0.032 Uiso 1 1 calc R . . C54 C 0.58163(19) 0.3035(2) 0.42407(17) 0.0270(6) Uani 1 1 d . . . H54A H 0.6464 0.3259 0.4041 0.032 Uiso 1 1 calc R . . H54B H 0.5745 0.2305 0.4127 0.032 Uiso 1 1 calc R . . C55 C 0.5936(2) 0.3797(2) 0.53391(18) 0.0352(7) Uani 1 1 d . . . H55A H 0.6087 0.4532 0.5466 0.053 Uiso 1 1 calc R . . H55C H 0.6520 0.3728 0.5717 0.053 Uiso 1 1 calc R . . H55B H 0.5275 0.3611 0.5528 0.053 Uiso 1 1 calc R . . C56 C 0.38800(18) 0.32517(18) 0.18664(18) 0.0212(6) Uani 1 1 d . . . H56B H 0.3311 0.3170 0.1359 0.025 Uiso 1 1 calc R . . H56A H 0.3780 0.3762 0.2505 0.025 Uiso 1 1 calc R . . C57 C 0.49670(19) 0.3729(2) 0.1727(2) 0.0275(6) Uani 1 1 d . . . H57A H 0.5531 0.3936 0.2296 0.033 Uiso 1 1 calc R . . H57B H 0.5127 0.3183 0.1143 0.033 Uiso 1 1 calc R . . C58 C 0.4967(2) 0.4716(2) 0.1614(2) 0.0338(7) Uani 1 1 d . . . H58A H 0.4812 0.5264 0.2200 0.041 Uiso 1 1 calc R . . H58B H 0.4400 0.4511 0.1048 0.041 Uiso 1 1 calc R . . C59 C 0.6055(2) 0.5189(3) 0.1467(3) 0.0566(10) Uani 1 1 d . . . H59A H 0.6613 0.5416 0.2037 0.085 Uiso 1 1 calc R . . H59C H 0.6027 0.5803 0.1385 0.085 Uiso 1 1 calc R . . H59B H 0.6210 0.4647 0.0887 0.085 Uiso 1 1 calc R . . C60 C 0.27040(17) 0.18454(19) 0.21062(17) 0.0204(6) Uani 1 1 d . . . H60B H 0.2727 0.2418 0.2764 0.024 Uiso 1 1 calc R . . H60A H 0.2674 0.1191 0.2146 0.024 Uiso 1 1 calc R . . C61 C 0.16681(18) 0.16482(19) 0.14167(17) 0.0212(6) Uani 1 1 d . . . H61A H 0.1678 0.1163 0.0736 0.025 Uiso 1 1 calc R . . H61B H 0.1607 0.2329 0.1471 0.025 Uiso 1 1 calc R . . C62 C 0.07052(18) 0.1143(2) 0.17031(18) 0.0248(6) Uani 1 1 d . . . H62A H 0.0689 0.0399 0.1511 0.030 Uiso 1 1 calc R . . H62B H 0.0800 0.1540 0.2418 0.030 Uiso 1 1 calc R . . C63 C -0.03673(19) 0.1152(2) 0.1219(2) 0.0325(7) Uani 1 1 d . . . H63B H -0.0382 0.1890 0.1454 0.049 Uiso 1 1 calc R . . H63C H -0.0949 0.0782 0.1384 0.049 Uiso 1 1 calc R . . H63A H -0.0450 0.0791 0.0512 0.049 Uiso 1 1 calc R . . C64 C 0.37362(19) 0.13171(18) 0.07654(16) 0.0214(6) Uani 1 1 d . . . H64B H 0.3261 0.1413 0.0309 0.026 Uiso 1 1 calc R . . H64A H 0.4460 0.1469 0.0654 0.026 Uiso 1 1 calc R . . C65 C 0.33769(19) 0.01348(18) 0.05059(17) 0.0222(6) Uani 1 1 d . . . H65B H 0.2646 -0.0041 0.0595 0.027 Uiso 1 1 calc R . . H65A H 0.3850 0.0016 0.0946 0.027 Uiso 1 1 calc R . . C66 C 0.34107(19) -0.06002(19) -0.05646(17) 0.0234(6) Uani 1 1 d . . . H66B H 0.2965 -0.0451 -0.0998 0.028 Uiso 1 1 calc R . . H66A H 0.4149 -0.0439 -0.0642 0.028 Uiso 1 1 calc R . . C67 C 0.3009(2) -0.17954(19) -0.08715(18) 0.0291(6) Uani 1 1 d . . . H67A H 0.3449 -0.1947 -0.0445 0.044 Uiso 1 1 calc R . . H67C H 0.3055 -0.2230 -0.1545 0.044 Uiso 1 1 calc R . . H67B H 0.2270 -0.1964 -0.0819 0.044 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 Cl1 0.0491(4) 0.0248(4) 0.0213(4) 0.0101(3) 0.0121(3) 0.0095(3) O2 0.0616(17) 0.092(2) 0.0241(13) 0.0157(14) 0.0090(11) 0.0481(15) C3 0.0347(16) 0.0275(15) 0.0247(15) 0.0150(13) 0.0078(12) 0.0100(12) C4 0.0258(15) 0.0199(14) 0.0119(12) 0.0059(11) 0.0070(11) 0.0088(11) C5 0.0230(14) 0.0218(14) 0.0111(13) 0.0039(11) 0.0054(11) 0.0051(11) C6 0.0280(15) 0.0284(15) 0.0174(14) 0.0074(12) 0.0058(11) 0.0051(12) N7 0.0287(13) 0.0262(13) 0.0160(12) 0.0104(11) 0.0042(10) 0.0027(10) C8 0.0206(14) 0.0265(16) 0.0226(14) 0.0131(13) 0.0027(12) 0.0077(12) O9 0.0352(11) 0.0295(10) 0.0255(10) 0.0148(9) 0.0097(9) 0.0043(8) C10 0.0254(15) 0.0204(14) 0.0215(14) 0.0134(12) 0.0031(12) 0.0023(11) C11 0.0295(16) 0.0270(15) 0.0300(16) 0.0155(13) 0.0027(13) 0.0060(12) C12 0.0354(17) 0.0280(16) 0.0300(17) 0.0137(14) -0.0080(14) -0.0040(13) C13 0.053(2) 0.0311(17) 0.0201(15) 0.0110(13) 0.0002(15) 0.0016(15) C14 0.0450(19) 0.0299(16) 0.0259(16) 0.0122(14) 0.0125(14) 0.0064(14) C15 0.0283(15) 0.0237(15) 0.0236(15) 0.0119(13) 0.0017(12) 0.0020(12) N16 0.0324(14) 0.0300(13) 0.0259(14) 0.0101(11) 0.0092(11) 0.0109(11) O17 0.0369(11) 0.0476(13) 0.0225(11) 0.0114(9) 0.0054(9) 0.0165(10) O18 0.0339(12) 0.0522(13) 0.0383(12) 0.0174(10) 0.0182(10) 0.0139(10) C19 0.0265(15) 0.0341(16) 0.0275(15) 0.0113(13) 0.0010(12) 0.0106(13) C20 0.0230(14) 0.0257(14) 0.0089(12) 0.0031(11) 0.0021(10) 0.0113(12) C21 0.0283(15) 0.0196(13) 0.0080(12) 0.0025(11) 0.0033(11) 0.0108(12) C22 0.0301(15) 0.0247(14) 0.0136(13) 0.0055(12) 0.0035(11) 0.0131(12) N23 0.0316(13) 0.0185(13) 0.0137(11) 0.0049(10) 0.0031(9) 0.0098(10) C24 0.0180(14) 0.0242(15) 0.0203(14) 0.0102(13) 0.0026(11) 0.0052(11) O25 0.0665(14) 0.0252(11) 0.0242(10) 0.0129(9) 0.0126(9) 0.0209(10) C26 0.0173(13) 0.0219(14) 0.0175(13) 0.0072(12) 0.0035(11) 0.0030(11) C27 0.0231(14) 0.0202(14) 0.0197(14) 0.0074(12) 0.0035(11) 0.0020(11) C28 0.0262(15) 0.0207(14) 0.0235(15) 0.0065(12) 0.0070(12) 0.0020(12) C29 0.0267(15) 0.0298(16) 0.0142(13) 0.0052(12) 0.0027(11) 0.0001(12) C30 0.0267(15) 0.0360(17) 0.0205(15) 0.0162(13) 0.0043(12) 0.0074(13) C31 0.0206(14) 0.0251(15) 0.0229(15) 0.0106(12) 0.0054(11) 0.0081(12) N32 0.0440(16) 0.0425(16) 0.0234(13) 0.0211(12) 0.0119(11) 0.0220(13) O33 0.0442(14) 0.0623(15) 0.0534(14) 0.0276(12) 0.0217(11) 0.0327(11) O34 0.0647(15) 0.0340(12) 0.0472(13) 0.0245(11) 0.0229(11) 0.0193(11) C35 0.0309(16) 0.0318(16) 0.0268(15) 0.0167(13) 0.0072(12) 0.0098(13) C36 0.0234(14) 0.0207(14) 0.0109(12) 0.0044(11) 0.0044(11) 0.0051(11) C37 0.0212(14) 0.0204(13) 0.0083(12) 0.0033(11) 0.0050(10) 0.0104(11) C38 0.0251(14) 0.0238(14) 0.0155(13) 0.0055(12) 0.0044(11) 0.0113(12) N39 0.0249(12) 0.0256(13) 0.0118(12) 0.0072(11) 0.0020(10) 0.0106(10) C40 0.0194(14) 0.0249(14) 0.0198(15) 0.0102(12) 0.0035(11) 0.0077(12) O41 0.0392(11) 0.0359(11) 0.0179(10) 0.0094(9) 0.0013(8) 0.0205(9) C42 0.0231(14) 0.0238(14) 0.0157(13) 0.0109(12) 0.0047(11) 0.0080(12) C43 0.0240(15) 0.0278(15) 0.0270(15) 0.0118(13) 0.0051(12) 0.0120(12) C44 0.0293(16) 0.0257(15) 0.0238(15) 0.0060(13) 0.0004(12) 0.0074(12) C45 0.0404(17) 0.0249(15) 0.0230(15) 0.0083(13) 0.0093(13) 0.0152(13) C46 0.0280(15) 0.0306(16) 0.0266(15) 0.0168(13) 0.0099(12) 0.0157(13) C47 0.0220(14) 0.0243(15) 0.0167(13) 0.0113(12) 0.0025(11) 0.0062(12) N48 0.0243(12) 0.0327(14) 0.0215(12) 0.0135(11) 0.0084(10) 0.0117(11) O49 0.0348(11) 0.0289(12) 0.0444(12) 0.0181(10) -0.0014(9) 0.0028(9) O50 0.0268(10) 0.0461(12) 0.0293(10) 0.0218(10) 0.0056(8) 0.0174(9) N51 0.0153(11) 0.0224(11) 0.0188(11) 0.0095(9) 0.0032(9) 0.0062(9) C52 0.0170(13) 0.0249(14) 0.0214(14) 0.0120(12) 0.0032(11) 0.0082(11) C53 0.0236(15) 0.0301(15) 0.0205(14) 0.0080(12) 0.0007(11) 0.0087(12) C54 0.0200(14) 0.0336(16) 0.0248(15) 0.0143(13) 0.0013(11) 0.0049(12) C55 0.0279(16) 0.0446(18) 0.0260(16) 0.0171(14) -0.0022(12) 0.0012(13) C56 0.0233(14) 0.0190(14) 0.0203(14) 0.0076(11) 0.0032(11) 0.0098(11) C57 0.0219(14) 0.0253(15) 0.0366(16) 0.0155(13) 0.0069(12) 0.0087(12) C58 0.0244(15) 0.0309(16) 0.0542(19) 0.0254(15) 0.0111(14) 0.0117(13) C59 0.0387(19) 0.048(2) 0.110(3) 0.057(2) 0.0283(19) 0.0174(16) C60 0.0190(13) 0.0226(14) 0.0175(13) 0.0085(11) 0.0047(11) 0.0050(11) C61 0.0213(14) 0.0212(14) 0.0186(13) 0.0075(12) 0.0035(11) 0.0077(11) C62 0.0214(14) 0.0237(14) 0.0249(14) 0.0096(12) 0.0018(11) 0.0050(11) C63 0.0215(15) 0.0366(17) 0.0355(16) 0.0168(14) 0.0022(12) 0.0051(12) C64 0.0243(14) 0.0240(14) 0.0154(13) 0.0075(11) 0.0061(11) 0.0107(11) C65 0.0215(14) 0.0238(14) 0.0194(14) 0.0084(12) 0.0033(11) 0.0089(11) C66 0.0189(14) 0.0269(15) 0.0205(14) 0.0087(12) 0.0036(11) 0.0067(11) C67 0.0231(15) 0.0280(16) 0.0251(15) 0.0046(13) 0.0012(12) 0.0086(12) _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 O2 H2B 0.77(5) . ? O2 H2A 0.89(5) . ? C3 C4 1.514(3) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C37 1.403(3) . ? C4 C5 1.405(3) . ? C5 C20 1.394(3) . ? C5 C6 1.515(3) . ? C6 N7 1.467(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N7 C8 1.330(3) . ? N7 H7 0.90(3) . ? C8 O9 1.232(3) . ? C8 C10 1.509(3) . ? C10 C11 1.386(3) . ? C10 C15 1.393(3) . ? C11 C12 1.383(4) . ? C11 H11 0.9300 . ? C12 C13 1.373(4) . ? C12 H12 0.9300 . ? C13 C14 1.381(4) . ? C13 H13 0.9300 . ? C14 C15 1.386(3) . ? C14 H14 0.9300 . ? C15 N16 1.477(3) . ? N16 O17 1.226(3) . ? N16 O18 1.228(3) . ? C19 C20 1.511(3) . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C19 H19A 0.9600 . ? C20 C21 1.401(3) . ? C21 C36 1.401(3) . ? C21 C22 1.514(3) . ? C22 N23 1.466(3) . ? C22 H22B 0.9700 . ? C22 H22A 0.9700 . ? N23 C24 1.337(3) . ? N23 H23 0.92(3) . ? C24 O25 1.224(3) 1 ? C24 O25 1.224(3) . ? C24 C26 1.509(3) . ? C26 C27 1.392(3) . ? C26 C31 1.393(3) . ? C27 C28 1.388(3) . ? C27 H27 0.9300 . ? C28 C29 1.374(3) . ? C28 H28 0.9300 . ? C29 C30 1.382(3) . ? C29 H29 0.9300 . ? C30 C31 1.377(3) . ? C30 H30 0.9300 . ? C31 N32 1.477(3) . ? N32 O34 1.221(3) . ? N32 O33 1.223(3) 1 ? N32 O33 1.223(3) . ? C35 C36 1.514(3) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.400(3) . ? C37 C38 1.515(3) . ? C38 N39 1.463(3) . ? C38 H38B 0.9700 . ? C38 H38A 0.9700 . ? N39 C40 1.332(3) . ? N39 H39 0.78(2) . ? C40 O41 1.231(3) . ? C40 C42 1.501(3) . ? C42 C43 1.390(3) . ? C42 C47 1.393(3) . ? C43 C44 1.382(3) . ? C43 H43 0.9300 . ? C44 C45 1.380(3) . ? C44 H44 0.9300 . ? C45 C46 1.384(3) . ? C45 H45 0.9300 . ? C46 C47 1.378(3) . ? C46 H46 0.9300 . ? C47 N48 1.477(3) . ? N48 O49 1.222(2) . ? N48 O50 1.226(2) . ? N51 C60 1.516(3) . ? N51 C56 1.523(3) . ? N51 C64 1.524(3) . ? N51 C52 1.525(3) . ? C52 C53 1.514(3) . ? C52 H52B 0.9700 . ? C52 H52A 0.9700 . ? C53 C54 1.519(3) . ? C53 H53B 0.9700 . ? C53 H53A 0.9700 . ? C54 C55 1.520(3) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 H55A 0.9600 . ? C55 H55C 0.9600 . ? C55 H55B 0.9600 . ? C56 C57 1.519(3) . ? C56 H56B 0.9700 . ? C56 H56A 0.9700 . ? C57 C58 1.516(3) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.524(4) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9600 . ? C59 H59C 0.9600 . ? C59 H59B 0.9600 . ? C60 C61 1.517(3) . ? C60 H60B 0.9700 . ? C60 H60A 0.9700 . ? C61 C62 1.527(3) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.516(3) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C63 H63A 0.9600 . ? C64 C65 1.518(3) . ? C64 H64B 0.9700 . ? C64 H64A 0.9700 . ? C65 C66 1.522(3) . ? C65 H65B 0.9700 . ? C65 H65A 0.9700 . ? C66 C67 1.519(3) . ? C66 H66B 0.9700 . ? C66 H66A 0.9700 . ? C67 H67A 0.9600 . ? C67 H67C 0.9600 . ? C67 H67B 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H2B O2 H2A 108(4) . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C37 C4 C5 119.2(2) . . ? C37 C4 C3 120.8(2) . . ? C5 C4 C3 120.0(2) . . ? C20 C5 C4 120.5(2) . . ? C20 C5 C6 119.6(2) . . ? C4 C5 C6 119.4(2) . . ? N7 C6 C5 107.66(19) . . ? N7 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? N7 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C8 N7 C6 121.1(2) . . ? C8 N7 H7 120.0(17) . . ? C6 N7 H7 118.8(17) . . ? O9 C8 N7 122.8(2) . . ? O9 C8 C10 119.2(2) . . ? N7 C8 C10 117.9(2) . . ? C11 C10 C15 116.7(2) . . ? C11 C10 C8 116.7(2) . . ? C15 C10 C8 126.6(2) . . ? C12 C11 C10 121.9(3) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 118.9(3) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C14 C15 C10 122.4(2) . . ? C14 C15 N16 117.1(2) . . ? C10 C15 N16 120.5(2) . . ? O17 N16 O18 124.1(2) . . ? O17 N16 C15 117.8(2) . . ? O18 N16 C15 118.1(2) . . ? C20 C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20 C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? C5 C20 C21 119.7(2) . . ? C5 C20 C19 120.9(2) . . ? C21 C20 C19 119.3(2) . . ? C36 C21 C20 120.3(2) . . ? C36 C21 C22 120.6(2) . . ? C20 C21 C22 118.9(2) . . ? N23 C22 C21 109.75(19) . . ? N23 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? N23 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? H22B C22 H22A 108.2 . . ? C24 N23 C22 119.9(2) . . ? C24 N23 H23 119.8(15) . . ? C22 N23 H23 119.0(15) . . ? O25 C24 N23 122.0(2) 1 . ? O25 C24 N23 122.0(2) . . ? O25 C24 C26 120.3(2) 1 . ? O25 C24 C26 120.3(2) . . ? N23 C24 C26 117.7(2) . . ? C27 C26 C31 116.5(2) . . ? C27 C26 C24 123.0(2) . . ? C31 C26 C24 120.3(2) . . ? C28 C27 C26 121.4(2) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C29 C28 C27 119.8(2) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.6(2) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 118.5(2) . . ? C31 C30 H30 120.8 . . ? C29 C30 H30 120.8 . . ? C30 C31 C26 123.1(2) . . ? C30 C31 N32 114.8(2) . . ? C26 C31 N32 122.1(2) . . ? O34 N32 O33 124.4(2) . 1 ? O34 N32 O33 124.4(2) . . ? O34 N32 C31 118.0(2) . . ? O33 N32 C31 117.4(2) 1 . ? O33 N32 C31 117.4(2) . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C21 119.5(2) . . ? C37 C36 C35 120.1(2) . . ? C21 C36 C35 120.4(2) . . ? C36 C37 C4 120.5(2) . . ? C36 C37 C38 120.2(2) . . ? C4 C37 C38 119.2(2) . . ? N39 C38 C37 111.24(19) . . ? N39 C38 H38B 109.4 . . ? C37 C38 H38B 109.4 . . ? N39 C38 H38A 109.4 . . ? C37 C38 H38A 109.4 . . ? H38B C38 H38A 108.0 . . ? C40 N39 C38 121.6(2) . . ? C40 N39 H39 120.7(18) . . ? C38 N39 H39 117.5(18) . . ? O41 C40 N39 123.0(2) . . ? O41 C40 C42 120.5(2) . . ? N39 C40 C42 116.5(2) . . ? C43 C42 C47 116.9(2) . . ? C43 C42 C40 121.6(2) . . ? C47 C42 C40 121.1(2) . . ? C44 C43 C42 121.1(2) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C45 C44 C43 120.1(2) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.5(2) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C47 C46 C45 118.2(2) . . ? C47 C46 H46 120.9 . . ? C45 C46 H46 120.9 . . ? C46 C47 C42 123.1(2) . . ? C46 C47 N48 116.6(2) . . ? C42 C47 N48 120.3(2) . . ? O49 N48 O50 124.8(2) . . ? O49 N48 C47 118.0(2) . . ? O50 N48 C47 117.2(2) . . ? C60 N51 C56 109.31(17) . . ? C60 N51 C64 110.79(17) . . ? C56 N51 C64 108.43(17) . . ? C60 N51 C52 108.93(17) . . ? C56 N51 C52 110.72(17) . . ? C64 N51 C52 108.67(17) . . ? C53 C52 N51 115.33(18) . . ? C53 C52 H52B 108.4 . . ? N51 C52 H52B 108.4 . . ? C53 C52 H52A 108.4 . . ? N51 C52 H52A 108.4 . . ? H52B C52 H52A 107.5 . . ? C52 C53 C54 110.7(2) . . ? C52 C53 H53B 109.5 . . ? C54 C53 H53B 109.5 . . ? C52 C53 H53A 109.5 . . ? C54 C53 H53A 109.5 . . ? H53B C53 H53A 108.1 . . ? C53 C54 C55 111.8(2) . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54B 109.3 . . ? C55 C54 H54B 109.3 . . ? H54A C54 H54B 107.9 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? H55C C55 H55B 109.5 . . ? C57 C56 N51 114.61(18) . . ? C57 C56 H56B 108.6 . . ? N51 C56 H56B 108.6 . . ? C57 C56 H56A 108.6 . . ? N51 C56 H56A 108.6 . . ? H56B C56 H56A 107.6 . . ? C58 C57 C56 111.3(2) . . ? C58 C57 H57A 109.4 . . ? C56 C57 H57A 109.4 . . ? C58 C57 H57B 109.4 . . ? C56 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? C57 C58 C59 111.3(2) . . ? C57 C58 H58A 109.4 . . ? C59 C58 H58A 109.4 . . ? C57 C58 H58B 109.4 . . ? C59 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? H59C C59 H59B 109.5 . . ? N51 C60 C61 116.02(18) . . ? N51 C60 H60B 108.3 . . ? C61 C60 H60B 108.3 . . ? N51 C60 H60A 108.3 . . ? C61 C60 H60A 108.3 . . ? H60B C60 H60A 107.4 . . ? C60 C61 C62 108.86(19) . . ? C60 C61 H61A 109.9 . . ? C62 C61 H61A 109.9 . . ? C60 C61 H61B 109.9 . . ? C62 C61 H61B 109.9 . . ? H61A C61 H61B 108.3 . . ? C63 C62 C61 112.6(2) . . ? C63 C62 H62A 109.1 . . ? C61 C62 H62A 109.1 . . ? C63 C62 H62B 109.1 . . ? C61 C62 H62B 109.1 . . ? H62A C62 H62B 107.8 . . ? C62 C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C63 H63A 109.5 . . ? H63B C63 H63A 109.5 . . ? H63C C63 H63A 109.5 . . ? C65 C64 N51 116.46(18) . . ? C65 C64 H64B 108.2 . . ? N51 C64 H64B 108.2 . . ? C65 C64 H64A 108.2 . . ? N51 C64 H64A 108.2 . . ? H64B C64 H64A 107.3 . . ? C64 C65 C66 110.20(19) . . ? C64 C65 H65B 109.6 . . ? C66 C65 H65B 109.6 . . ? C64 C65 H65A 109.6 . . ? C66 C65 H65A 109.6 . . ? H65B C65 H65A 108.1 . . ? C67 C66 C65 112.0(2) . . ? C67 C66 H66B 109.2 . . ? C65 C66 H66B 109.2 . . ? C67 C66 H66A 109.2 . . ? C65 C66 H66A 109.2 . . ? H66B C66 H66A 107.9 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? H67C C67 H67B 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A Cl1 0.89(5) 2.29(5) 3.167(3) 168(4) 1_655 C59 H59C O49 0.96 2.51 3.441(3) 163.1 1_655 C52 H52B O9 0.97 2.21 3.138(3) 159.1 1_545 C65 H65A O9 0.97 2.52 3.301(3) 137.0 1_545 C67 H67A O50 0.96 2.50 3.394(3) 155.4 1_645 O2 H2B O18 0.77(5) 2.36(5) 3.132(3) 174(5) 2_676 N7 H7 Cl1 0.90(3) 2.27(3) 3.172(2) 178(2) 1 N23 H23 Cl1 0.92(3) 2.35(3) 3.260(2) 169(2) 1 C27 H27 Cl1 0.93 2.74 3.537(2) 144.3 1 C53 H53B O33 0.97 2.48 3.283(3) 140.2 1 C60 H60B O33 0.97 2.58 3.543(3) 169.5 1 C61 H61B O25 0.97 2.50 3.057(3) 116.1 1 N39 H39 O2 0.78(2) 2.14(2) 2.914(3) 172(2) 1_455 C46 H46 O9 0.93 2.49 3.399(3) 164.6 1_455 C45 H45 Cl1 0.93 2.82 3.404(3) 121.7 2_576 C56 H56B O41 0.97 2.34 3.199(3) 147.1 2_565 C64 H64A O50 0.97 2.53 3.202(3) 126.5 2_565 C64 H64B O41 0.97 2.54 3.417(3) 150.2 2_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.95 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.177 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.044 # Attachment 'Complex_3.cif' data_nis31_0m _database_code_depnum_ccdc_archive 'CCDC 733120' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H66 N8 O12' _chemical_formula_weight 959.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.922(6) _cell_length_b 14.152(7) _cell_length_c 15.351(7) _cell_angle_alpha 116.614(6) _cell_angle_beta 92.811(7) _cell_angle_gamma 101.864(7) _cell_volume 2424(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1808 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 19.04 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9666 _exptl_absorpt_correction_T_max 0.9850 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'BRUKER CCD AREA DETECTOR' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21099 _diffrn_reflns_av_R_equivalents 0.0963 _diffrn_reflns_av_sigmaI/netI 0.1193 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 23.89 _reflns_number_total 7484 _reflns_number_gt 4320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'MERCURY 2.2' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7484 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1287 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.2086 _refine_ls_wR_factor_gt 0.1747 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _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 N1 N 0.0233(3) 0.2572(3) 0.3596(3) 0.0303(9) Uani 1 1 d . . . O2 O -0.0101(3) 0.3149(2) 0.3285(2) 0.0382(8) Uani 1 1 d . . . O3 O 0.1217(2) 0.2831(2) 0.3944(2) 0.0337(8) Uani 1 1 d . . . O4 O -0.0383(2) 0.1757(2) 0.3575(2) 0.0341(8) Uani 1 1 d . . . C5 C 0.2768(3) 0.1276(4) 0.2314(3) 0.0352(12) Uani 1 1 d . . . H5B H 0.3319 0.1353 0.1936 0.053 Uiso 1 1 calc R . . H5C H 0.2709 0.0610 0.2356 0.053 Uiso 1 1 calc R . . H5A H 0.2947 0.1885 0.2967 0.053 Uiso 1 1 calc R . . C6 C 0.1706(3) 0.1242(3) 0.1816(3) 0.0236(10) Uani 1 1 d . . . C7 C 0.0784(3) 0.0431(3) 0.1654(3) 0.0217(10) Uani 1 1 d . . . C8 C 0.0866(4) -0.0418(3) 0.1967(3) 0.0263(10) Uani 1 1 d . . . H8A H 0.0268 -0.1055 0.1612 0.032 Uiso 1 1 calc R . . H8B H 0.1523 -0.0642 0.1809 0.032 Uiso 1 1 calc R . . N9 N 0.0861(3) 0.0025(3) 0.3034(2) 0.0258(9) Uani 1 1 d . . . H9 H 0.039(4) 0.049(4) 0.329(3) 0.046(14) Uiso 1 1 d . . . C10 C 0.1458(3) -0.0242(3) 0.3585(3) 0.0226(10) Uani 1 1 d . . . O11 O 0.2024(2) -0.0877(2) 0.3245(2) 0.0317(8) Uani 1 1 d . . . C12 C 0.1417(3) 0.0299(4) 0.4680(3) 0.0263(10) Uani 1 1 d . . . C13 C 0.1167(3) 0.1294(3) 0.5160(3) 0.0274(10) Uani 1 1 d . . . H13 H 0.0981 0.1630 0.4798 0.033 Uiso 1 1 calc R . . C14 C 0.1191(4) 0.1797(4) 0.6173(3) 0.0318(11) Uani 1 1 d . . . H14 H 0.1023 0.2468 0.6483 0.038 Uiso 1 1 calc R . . C15 C 0.1462(4) 0.1316(4) 0.6723(3) 0.0333(11) Uani 1 1 d . . . H15 H 0.1477 0.1661 0.7403 0.040 Uiso 1 1 calc R . . C16 C 0.1711(3) 0.0320(4) 0.6270(3) 0.0313(11) Uani 1 1 d . . . H16 H 0.1893 -0.0013 0.6636 0.038 Uiso 1 1 calc R . . C17 C 0.1683(3) -0.0171(4) 0.5255(3) 0.0289(11) Uani 1 1 d . . . N18 N 0.1934(4) -0.1237(3) 0.4827(3) 0.0351(10) Uani 1 1 d . . . O19 O 0.2832(3) -0.1271(3) 0.5068(3) 0.0510(10) Uani 1 1 d . . . O20 O 0.1211(3) -0.2041(3) 0.4288(3) 0.0450(9) Uani 1 1 d . . . C21 C -0.0217(3) 0.0460(3) 0.1276(3) 0.0242(10) Uani 1 1 d . . . C22 C -0.1218(3) -0.0343(4) 0.1193(3) 0.0306(11) Uani 1 1 d . . . H22C H -0.1516 -0.0812 0.0509 0.046 Uiso 1 1 calc R . . H22A H -0.1727 0.0041 0.1526 0.046 Uiso 1 1 calc R . . H22B H -0.1054 -0.0776 0.1490 0.046 Uiso 1 1 calc R . . C23 C -0.0264(3) 0.1305(3) 0.1045(3) 0.0254(10) Uani 1 1 d . . . C24 C -0.1343(3) 0.1390(4) 0.0679(3) 0.0307(11) Uani 1 1 d . . . H24A H -0.1289 0.1527 0.0116 0.037 Uiso 1 1 calc R . . H24B H -0.1879 0.0708 0.0473 0.037 Uiso 1 1 calc R . . N25 N -0.1661(3) 0.2284(3) 0.1477(3) 0.0269(9) Uani 1 1 d . . . H25 H -0.134(3) 0.248(3) 0.203(3) 0.014(11) Uiso 1 1 d . . . C26 C -0.2288(3) 0.2835(3) 0.1291(3) 0.0251(10) Uani 1 1 d . . . O27 O -0.2707(3) 0.2567(3) 0.0445(2) 0.0392(9) Uani 1 1 d . . . C28 C -0.2441(3) 0.3827(3) 0.2154(3) 0.0225(10) Uani 1 1 d . . . C29 C -0.1608(4) 0.4555(3) 0.2920(3) 0.0282(11) Uani 1 1 d . . . H29 H -0.0938 0.4408 0.2918 0.034 Uiso 1 1 calc R . . C30 C -0.1758(4) 0.5479(4) 0.3674(3) 0.0324(11) Uani 1 1 d . . . H30 H -0.1190 0.5951 0.4180 0.039 Uiso 1 1 calc R . . C31 C -0.2741(4) 0.5728(4) 0.3701(3) 0.0340(11) Uani 1 1 d . . . H31 H -0.2836 0.6354 0.4227 0.041 Uiso 1 1 calc R . . C32 C -0.3585(3) 0.5038(3) 0.2939(3) 0.0286(11) Uani 1 1 d . . . H32 H -0.4245 0.5203 0.2930 0.034 Uiso 1 1 calc R . . C33 C -0.3417(3) 0.4103(3) 0.2198(3) 0.0253(10) Uani 1 1 d . . . N34 N -0.4366(3) 0.3345(3) 0.1462(3) 0.0290(9) Uani 1 1 d . . . O35 O -0.4854(2) 0.3705(3) 0.1028(2) 0.0375(8) Uani 1 1 d . . . O36 O -0.4655(3) 0.2419(3) 0.1364(2) 0.0453(9) Uani 1 1 d . . . C37 C 0.0649(3) 0.2103(3) 0.1189(3) 0.0244(10) Uani 1 1 d . . . C38 C 0.0598(4) 0.3058(4) 0.1003(3) 0.0366(12) Uani 1 1 d . . . H38A H -0.0102 0.2927 0.0664 0.055 Uiso 1 1 calc R . . H38B H 0.1125 0.3137 0.0605 0.055 Uiso 1 1 calc R . . H38C H 0.0737 0.3715 0.1622 0.055 Uiso 1 1 calc R . . C39 C 0.1645(3) 0.2094(3) 0.1610(3) 0.0255(10) Uani 1 1 d . . . C40 C 0.2595(4) 0.3030(4) 0.1909(3) 0.0323(11) Uani 1 1 d . . . H40A H 0.3238 0.2769 0.1807 0.039 Uiso 1 1 calc R . . H40B H 0.2532 0.3389 0.1505 0.039 Uiso 1 1 calc R . . N41 N 0.2672(3) 0.3809(3) 0.2949(3) 0.0293(9) Uani 1 1 d . . . H41 H 0.223(4) 0.361(4) 0.326(4) 0.055(17) Uiso 1 1 d . . . C42 C 0.3284(3) 0.4816(4) 0.3307(3) 0.0270(10) Uani 1 1 d . . . O43 O 0.3906(2) 0.5100(2) 0.2844(2) 0.0350(8) Uani 1 1 d . . . C44 C 0.3289(4) 0.5616(4) 0.4374(3) 0.0322(11) Uani 1 1 d . . . C45 C 0.4280(4) 0.6003(4) 0.5028(4) 0.0395(12) Uani 1 1 d . . . H45 H 0.4869 0.5742 0.4798 0.047 Uiso 1 1 calc R . . C46 C 0.4359(4) 0.6759(4) 0.5992(4) 0.0473(14) Uani 1 1 d . . . H46 H 0.5005 0.7011 0.6416 0.057 Uiso 1 1 calc R . . C47 C 0.3484(4) 0.7155(4) 0.6348(4) 0.0400(12) Uani 1 1 d . . . H47 H 0.3557 0.7669 0.7007 0.048 Uiso 1 1 calc R . . C48 C 0.2513(4) 0.6802(4) 0.5742(3) 0.0391(12) Uani 1 1 d . . . H48 H 0.1925 0.7062 0.5976 0.047 Uiso 1 1 calc R . . C49 C 0.2457(4) 0.6029(4) 0.4755(3) 0.0354(12) Uani 1 1 d . . . N50 N 0.1441(3) 0.5714(3) 0.4133(3) 0.0359(10) Uani 1 1 d . . . O51 O 0.0622(3) 0.5786(3) 0.4506(3) 0.0511(10) Uani 1 1 d . . . O52 O 0.1444(3) 0.5412(3) 0.3233(2) 0.0434(9) Uani 1 1 d . . . N53 N 0.3640(2) 0.7120(3) 0.1764(2) 0.0208(8) Uani 1 1 d . . . C54 C 0.3782(3) 0.8204(3) 0.1754(3) 0.0234(10) Uani 1 1 d . . . H54B H 0.3703 0.8747 0.2399 0.028 Uiso 1 1 calc R . . H54A H 0.3209 0.8133 0.1278 0.028 Uiso 1 1 calc R . . C55 C 0.4845(3) 0.8625(3) 0.1505(3) 0.0263(10) Uani 1 1 d . . . H55B H 0.5421 0.8787 0.2021 0.032 Uiso 1 1 calc R . . H55A H 0.4967 0.8062 0.0891 0.032 Uiso 1 1 calc R . . C56 C 0.4861(3) 0.9642(3) 0.1405(3) 0.0315(11) Uani 1 1 d . . . H56A H 0.4261 0.9489 0.0914 0.038 Uiso 1 1 calc R . . H56B H 0.4775 1.0216 0.2030 0.038 Uiso 1 1 calc R . . C57 C 0.5890(4) 1.0038(4) 0.1105(4) 0.0424(13) Uani 1 1 d . . . H57B H 0.6482 1.0230 0.1608 0.064 Uiso 1 1 calc R . . H57C H 0.5859 1.0667 0.1025 0.064 Uiso 1 1 calc R . . H57A H 0.5984 0.9468 0.0493 0.064 Uiso 1 1 calc R . . C58 C 0.4552(3) 0.7165(3) 0.2468(3) 0.0224(10) Uani 1 1 d . . . H58A H 0.4420 0.6465 0.2468 0.027 Uiso 1 1 calc R . . H58B H 0.5214 0.7262 0.2210 0.027 Uiso 1 1 calc R . . C59 C 0.4709(3) 0.8048(3) 0.3517(3) 0.0279(10) Uani 1 1 d . . . H59A H 0.4044 0.7984 0.3777 0.033 Uiso 1 1 calc R . . H59B H 0.4901 0.8757 0.3536 0.033 Uiso 1 1 calc R . . C60 C 0.5584(3) 0.7962(4) 0.4154(3) 0.0284(11) Uani 1 1 d . . . H60B H 0.6254 0.8063 0.3910 0.034 Uiso 1 1 calc R . . H60A H 0.5410 0.7234 0.4096 0.034 Uiso 1 1 calc R . . C61 C 0.5732(4) 0.8797(4) 0.5237(3) 0.0396(12) Uani 1 1 d . . . H61B H 0.5967 0.9520 0.5306 0.059 Uiso 1 1 calc R . . H61C H 0.6260 0.8676 0.5611 0.059 Uiso 1 1 calc R . . H61A H 0.5064 0.8722 0.5477 0.059 Uiso 1 1 calc R . . C62 C 0.3659(3) 0.6235(3) 0.0730(3) 0.0233(10) Uani 1 1 d . . . H62A H 0.3197 0.6314 0.0262 0.028 Uiso 1 1 calc R . . H62B H 0.4382 0.6366 0.0586 0.028 Uiso 1 1 calc R . . C63 C 0.3318(3) 0.5073(3) 0.0551(3) 0.0253(10) Uani 1 1 d . . . H63A H 0.2580 0.4909 0.0647 0.030 Uiso 1 1 calc R . . H63B H 0.3760 0.4979 0.1021 0.030 Uiso 1 1 calc R . . C64 C 0.3428(3) 0.4289(3) -0.0498(3) 0.0272(10) Uani 1 1 d . . . H64A H 0.3010 0.4411 -0.0963 0.033 Uiso 1 1 calc R . . H64B H 0.4172 0.4443 -0.0583 0.033 Uiso 1 1 calc R . . C65 C 0.3052(4) 0.3103(4) -0.0726(3) 0.0336(11) Uani 1 1 d . . . H65A H 0.3472 0.2976 -0.0275 0.050 Uiso 1 1 calc R . . H65C H 0.3136 0.2640 -0.1390 0.050 Uiso 1 1 calc R . . H65B H 0.2311 0.2943 -0.0658 0.050 Uiso 1 1 calc R . . C66 C 0.2591(3) 0.6858(3) 0.2102(3) 0.0236(10) Uani 1 1 d . . . H66A H 0.2600 0.7449 0.2751 0.028 Uiso 1 1 calc R . . H66B H 0.2541 0.6201 0.2169 0.028 Uiso 1 1 calc R . . C67 C 0.1586(3) 0.6687(3) 0.1421(3) 0.0252(10) Uani 1 1 d . . . H67A H 0.1563 0.7373 0.1431 0.030 Uiso 1 1 calc R . . H67B H 0.1608 0.6164 0.0749 0.030 Uiso 1 1 calc R . . C68 C 0.0596(3) 0.6272(4) 0.1758(3) 0.0309(11) Uani 1 1 d . . . H68A H 0.0631 0.6746 0.2457 0.037 Uiso 1 1 calc R . . H68B H 0.0583 0.5546 0.1670 0.037 Uiso 1 1 calc R . . C69 C -0.0427(3) 0.6224(4) 0.1202(3) 0.0367(12) Uani 1 1 d . . . H69A H -0.0447 0.6949 0.1332 0.055 Uiso 1 1 calc R . . H69C H -0.1031 0.5912 0.1414 0.055 Uiso 1 1 calc R . . H69B H -0.0453 0.5780 0.0507 0.055 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 N1 0.039(3) 0.037(2) 0.017(2) 0.0118(19) 0.0052(18) 0.015(2) O2 0.058(2) 0.0388(19) 0.0305(19) 0.0223(16) 0.0058(16) 0.0234(17) O3 0.035(2) 0.043(2) 0.0267(18) 0.0190(16) 0.0028(15) 0.0119(16) O4 0.0380(19) 0.0350(19) 0.0301(19) 0.0183(16) 0.0079(15) 0.0032(16) C5 0.033(3) 0.045(3) 0.032(3) 0.020(2) 0.003(2) 0.014(2) C6 0.027(2) 0.033(3) 0.012(2) 0.010(2) 0.0060(18) 0.012(2) C7 0.028(2) 0.026(2) 0.014(2) 0.0102(19) 0.0049(19) 0.011(2) C8 0.035(3) 0.029(3) 0.016(2) 0.011(2) 0.001(2) 0.011(2) N9 0.030(2) 0.037(2) 0.017(2) 0.0155(18) 0.0027(17) 0.0140(18) C10 0.028(2) 0.027(2) 0.014(2) 0.011(2) 0.0026(19) 0.006(2) O11 0.0431(19) 0.0386(19) 0.0203(17) 0.0137(15) 0.0066(14) 0.0241(16) C12 0.022(2) 0.037(3) 0.022(2) 0.016(2) 0.0030(19) 0.006(2) C13 0.032(3) 0.033(3) 0.018(2) 0.014(2) 0.002(2) 0.007(2) C14 0.037(3) 0.034(3) 0.026(3) 0.015(2) 0.006(2) 0.010(2) C15 0.037(3) 0.041(3) 0.019(2) 0.013(2) 0.003(2) 0.007(2) C16 0.032(3) 0.045(3) 0.024(3) 0.023(2) 0.001(2) 0.006(2) C17 0.030(3) 0.037(3) 0.025(3) 0.017(2) 0.005(2) 0.013(2) N18 0.046(3) 0.042(3) 0.030(2) 0.025(2) 0.013(2) 0.017(2) O19 0.051(2) 0.077(3) 0.053(2) 0.044(2) 0.0151(19) 0.040(2) O20 0.061(2) 0.039(2) 0.039(2) 0.0202(18) 0.0094(19) 0.0144(19) C21 0.031(3) 0.029(2) 0.015(2) 0.010(2) 0.0038(19) 0.011(2) C22 0.032(3) 0.040(3) 0.027(3) 0.022(2) 0.002(2) 0.008(2) C23 0.034(3) 0.035(3) 0.011(2) 0.011(2) 0.0050(19) 0.015(2) C24 0.039(3) 0.035(3) 0.023(3) 0.013(2) 0.003(2) 0.021(2) N25 0.035(2) 0.036(2) 0.016(2) 0.0152(19) 0.0034(18) 0.0170(18) C26 0.021(2) 0.030(3) 0.030(3) 0.018(2) 0.007(2) 0.009(2) O27 0.053(2) 0.055(2) 0.0126(17) 0.0126(16) -0.0053(15) 0.0282(17) C28 0.028(2) 0.029(2) 0.016(2) 0.014(2) 0.0017(19) 0.010(2) C29 0.032(3) 0.034(3) 0.028(3) 0.020(2) 0.003(2) 0.015(2) C30 0.035(3) 0.031(3) 0.026(3) 0.009(2) -0.002(2) 0.011(2) C31 0.036(3) 0.037(3) 0.030(3) 0.014(2) 0.007(2) 0.013(2) C32 0.028(3) 0.033(3) 0.031(3) 0.019(2) 0.005(2) 0.013(2) C33 0.030(3) 0.034(3) 0.018(2) 0.016(2) 0.0008(19) 0.011(2) N34 0.027(2) 0.040(3) 0.022(2) 0.0163(19) 0.0025(17) 0.0093(19) O35 0.0324(18) 0.061(2) 0.0278(18) 0.0245(17) 0.0018(15) 0.0220(17) O36 0.048(2) 0.038(2) 0.041(2) 0.0167(18) -0.0110(17) 0.0016(17) C37 0.035(3) 0.028(2) 0.016(2) 0.012(2) 0.010(2) 0.013(2) C38 0.050(3) 0.040(3) 0.028(3) 0.020(2) 0.010(2) 0.017(2) C39 0.029(3) 0.033(3) 0.017(2) 0.013(2) 0.0088(19) 0.010(2) C40 0.036(3) 0.043(3) 0.024(3) 0.021(2) 0.012(2) 0.009(2) N41 0.031(2) 0.035(2) 0.024(2) 0.017(2) 0.0045(18) 0.0037(19) C42 0.024(2) 0.035(3) 0.031(3) 0.023(2) 0.001(2) 0.006(2) O43 0.0316(18) 0.044(2) 0.0340(19) 0.0245(17) 0.0067(15) 0.0037(15) C44 0.040(3) 0.035(3) 0.028(3) 0.023(2) 0.001(2) 0.003(2) C45 0.046(3) 0.041(3) 0.034(3) 0.026(3) -0.002(2) -0.001(2) C46 0.045(3) 0.057(4) 0.039(3) 0.032(3) -0.016(3) -0.008(3) C47 0.050(3) 0.046(3) 0.026(3) 0.020(2) 0.004(3) 0.008(3) C48 0.053(3) 0.046(3) 0.023(3) 0.023(2) 0.003(2) 0.002(3) C49 0.038(3) 0.048(3) 0.026(3) 0.025(2) 0.000(2) 0.005(2) N50 0.041(3) 0.046(3) 0.022(2) 0.016(2) 0.004(2) 0.011(2) O51 0.038(2) 0.072(3) 0.043(2) 0.025(2) 0.0105(18) 0.0170(19) O52 0.054(2) 0.048(2) 0.031(2) 0.0209(17) -0.0009(17) 0.0141(17) N53 0.0191(19) 0.028(2) 0.0153(19) 0.0104(16) -0.0001(15) 0.0058(15) C54 0.030(2) 0.023(2) 0.017(2) 0.009(2) -0.0002(19) 0.0076(19) C55 0.028(2) 0.030(3) 0.023(2) 0.014(2) 0.003(2) 0.009(2) C56 0.031(3) 0.030(3) 0.035(3) 0.018(2) 0.000(2) 0.007(2) C57 0.041(3) 0.043(3) 0.051(3) 0.029(3) 0.011(3) 0.009(2) C58 0.022(2) 0.030(2) 0.019(2) 0.014(2) 0.0014(18) 0.0086(19) C59 0.030(3) 0.033(3) 0.018(2) 0.011(2) -0.0002(19) 0.008(2) C60 0.027(2) 0.040(3) 0.023(2) 0.019(2) 0.000(2) 0.006(2) C61 0.037(3) 0.050(3) 0.025(3) 0.016(2) -0.006(2) 0.004(2) C62 0.026(2) 0.034(3) 0.009(2) 0.009(2) 0.0021(18) 0.011(2) C63 0.027(2) 0.031(3) 0.021(2) 0.013(2) 0.0019(19) 0.010(2) C64 0.026(2) 0.033(3) 0.021(2) 0.011(2) 0.0008(19) 0.009(2) C65 0.031(3) 0.039(3) 0.026(3) 0.011(2) -0.001(2) 0.011(2) C66 0.024(2) 0.034(3) 0.014(2) 0.012(2) -0.0002(18) 0.009(2) C67 0.021(2) 0.031(3) 0.021(2) 0.012(2) -0.0025(19) 0.005(2) C68 0.023(2) 0.049(3) 0.022(2) 0.019(2) -0.0016(19) 0.007(2) C69 0.028(3) 0.049(3) 0.033(3) 0.020(2) 0.000(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 O4 1.246(5) 1 ? N1 O4 1.246(5) . ? N1 O2 1.247(4) 1 ? N1 O2 1.247(4) . ? N1 O3 1.266(4) 1 ? N1 O3 1.266(4) . ? C5 C6 1.519(6) . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C5 H5A 0.9600 . ? C6 C39 1.392(6) . ? C6 C7 1.398(6) . ? C7 C21 1.407(6) . ? C7 C8 1.501(5) . ? C8 N9 1.469(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N9 C10 1.339(5) . ? N9 H9 0.95(5) . ? C10 O11 1.225(5) . ? C10 C12 1.512(6) . ? C12 C13 1.382(6) . ? C12 C17 1.390(6) . ? C13 C14 1.385(6) . ? C13 H13 0.9300 . ? C14 C15 1.373(6) . ? C14 H14 0.9300 . ? C15 C16 1.379(6) . ? C15 H15 0.9300 . ? C16 C17 1.387(6) . ? C16 H16 0.9300 . ? C17 N18 1.465(6) . ? N18 O19 1.218(5) . ? N18 O20 1.223(5) . ? C21 C23 1.403(6) . ? C21 C22 1.494(6) . ? C22 H22C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C23 C37 1.385(6) . ? C23 C24 1.525(6) . ? C24 N25 1.465(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? N25 C26 1.336(5) . ? N25 H25 0.83(4) . ? C26 O27 1.236(5) . ? C26 C28 1.496(6) . ? C28 C33 1.392(6) . ? C28 C29 1.392(6) . ? C29 C30 1.364(6) . ? C29 H29 0.9300 . ? C30 C31 1.384(6) . ? C30 H30 0.9300 . ? C31 C32 1.388(6) . ? C31 H31 0.9300 . ? C32 C33 1.372(6) . ? C32 H32 0.9300 . ? C33 N34 1.473(5) . ? N34 O36 1.222(4) . ? N34 O35 1.223(4) . ? C37 C39 1.416(6) . ? C37 C38 1.515(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.485(6) . ? C40 N41 1.462(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? N41 C42 1.323(5) . ? N41 H41 0.85(5) . ? C42 O43 1.221(5) 1 ? C42 O43 1.221(5) . ? C42 C44 1.517(6) . ? C44 C49 1.361(6) . ? C44 C45 1.428(6) . ? C45 C46 1.367(7) . ? C45 H45 0.9300 . ? C46 C47 1.392(7) . ? C46 H46 0.9300 . ? C47 C48 1.379(7) . ? C47 H47 0.9300 . ? C48 C49 1.403(6) . ? C48 H48 0.9300 . ? C49 N50 1.446(6) . ? N50 O51 1.229(5) . ? N50 O52 1.250(5) . ? N53 C66 1.510(5) . ? N53 C54 1.514(5) . ? N53 C62 1.524(5) . ? N53 C58 1.531(5) . ? C54 C55 1.519(6) . ? C54 H54B 0.9700 . ? C54 H54A 0.9700 . ? C55 C56 1.512(6) . ? C55 H55B 0.9700 . ? C55 H55A 0.9700 . ? C56 C57 1.509(6) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C57 H57A 0.9600 . ? C58 C59 1.503(6) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.518(6) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.520(6) . ? C60 H60B 0.9700 . ? C60 H60A 0.9700 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C61 H61A 0.9600 . ? C62 C63 1.504(6) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.527(6) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.515(6) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9600 . ? C65 H65C 0.9600 . ? C65 H65B 0.9600 . ? C66 C67 1.533(5) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.509(6) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.510(6) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 H69A 0.9600 . ? C69 H69C 0.9600 . ? C69 H69B 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 N1 O2 121.3(4) 1 1 ? O4 N1 O2 121.3(4) . 1 ? O4 N1 O2 121.3(4) 1 . ? O4 N1 O2 121.3(4) . . ? O4 N1 O3 119.9(4) 1 1 ? O4 N1 O3 119.9(4) . 1 ? O2 N1 O3 118.8(4) 1 1 ? O2 N1 O3 118.8(4) . 1 ? O4 N1 O3 119.9(4) 1 . ? O4 N1 O3 119.9(4) . . ? O2 N1 O3 118.8(4) 1 . ? O2 N1 O3 118.8(4) . . ? C6 C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 C5 H5A 109.5 . . ? H5B C5 H5A 109.5 . . ? H5C C5 H5A 109.5 . . ? C39 C6 C7 120.3(4) . . ? C39 C6 C5 118.7(4) . . ? C7 C6 C5 120.7(4) . . ? C6 C7 C21 120.5(4) . . ? C6 C7 C8 118.7(4) . . ? C21 C7 C8 120.6(4) . . ? N9 C8 C7 110.1(3) . . ? N9 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? N9 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? C10 N9 C8 121.2(4) . . ? C10 N9 H9 124(3) . . ? C8 N9 H9 115(3) . . ? O11 C10 N9 123.4(4) . . ? O11 C10 C12 120.3(4) . . ? N9 C10 C12 116.3(4) . . ? C13 C12 C17 117.1(4) . . ? C13 C12 C10 122.3(4) . . ? C17 C12 C10 120.6(4) . . ? C12 C13 C14 121.0(4) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 120.6(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.1(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 118.4(4) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C16 C17 C12 122.7(4) . . ? C16 C17 N18 115.2(4) . . ? C12 C17 N18 122.1(4) . . ? O19 N18 O20 124.2(4) . . ? O19 N18 C17 118.0(4) . . ? O20 N18 C17 117.7(4) . . ? C23 C21 C7 118.7(4) . . ? C23 C21 C22 120.6(4) . . ? C7 C21 C22 120.6(4) . . ? C21 C22 H22C 109.5 . . ? C21 C22 H22A 109.5 . . ? H22C C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C37 C23 C21 121.1(4) . . ? C37 C23 C24 118.9(4) . . ? C21 C23 C24 119.9(4) . . ? N25 C24 C23 109.2(3) . . ? N25 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? N25 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? C26 N25 C24 121.6(4) . . ? C26 N25 H25 123(3) . . ? C24 N25 H25 114(3) . . ? O27 C26 N25 122.3(4) . . ? O27 C26 C28 120.6(4) . . ? N25 C26 C28 117.0(4) . . ? C33 C28 C29 116.5(4) . . ? C33 C28 C26 121.1(4) . . ? C29 C28 C26 122.3(4) . . ? C30 C29 C28 121.0(4) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 121.2(4) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C30 C31 C32 119.6(4) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C33 C32 C31 118.0(4) . . ? C33 C32 H32 121.0 . . ? C31 C32 H32 121.0 . . ? C32 C33 C28 123.7(4) . . ? C32 C33 N34 115.8(4) . . ? C28 C33 N34 120.3(4) . . ? O36 N34 O35 124.0(4) . . ? O36 N34 C33 118.4(4) . . ? O35 N34 C33 117.4(4) . . ? C23 C37 C39 119.8(4) . . ? C23 C37 C38 121.6(4) . . ? C39 C37 C38 118.3(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C6 C39 C37 119.5(4) . . ? C6 C39 C40 120.0(4) . . ? C37 C39 C40 120.4(4) . . ? N41 C40 C39 109.9(4) . . ? N41 C40 H40A 109.7 . . ? C39 C40 H40A 109.7 . . ? N41 C40 H40B 109.7 . . ? C39 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C42 N41 C40 119.9(4) . . ? C42 N41 H41 124(4) . . ? C40 N41 H41 116(4) . . ? O43 C42 N41 122.9(4) 1 . ? O43 C42 N41 122.9(4) . . ? O43 C42 C44 118.7(4) 1 . ? O43 C42 C44 118.7(4) . . ? N41 C42 C44 118.1(4) . . ? C49 C44 C45 117.3(4) . . ? C49 C44 C42 126.3(4) . . ? C45 C44 C42 116.3(4) . . ? C46 C45 C44 119.7(5) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 120.9(5) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C48 C47 C46 121.3(5) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C47 C48 C49 116.6(5) . . ? C47 C48 H48 121.7 . . ? C49 C48 H48 121.7 . . ? C44 C49 C48 124.3(4) . . ? C44 C49 N50 120.7(4) . . ? C48 C49 N50 114.9(4) . . ? O51 N50 O52 122.8(4) . . ? O51 N50 C49 119.4(4) . . ? O52 N50 C49 117.8(4) . . ? C66 N53 C54 109.1(3) . . ? C66 N53 C62 110.8(3) . . ? C54 N53 C62 109.2(3) . . ? C66 N53 C58 108.8(3) . . ? C54 N53 C58 111.0(3) . . ? C62 N53 C58 108.0(3) . . ? N53 C54 C55 115.3(3) . . ? N53 C54 H54B 108.4 . . ? C55 C54 H54B 108.4 . . ? N53 C54 H54A 108.4 . . ? C55 C54 H54A 108.4 . . ? H54B C54 H54A 107.5 . . ? C56 C55 C54 111.2(3) . . ? C56 C55 H55B 109.4 . . ? C54 C55 H55B 109.4 . . ? C56 C55 H55A 109.4 . . ? C54 C55 H55A 109.4 . . ? H55B C55 H55A 108.0 . . ? C57 C56 C55 111.9(4) . . ? C57 C56 H56A 109.2 . . ? C55 C56 H56A 109.2 . . ? C57 C56 H56B 109.2 . . ? C55 C56 H56B 109.2 . . ? H56A C56 H56B 107.9 . . ? C56 C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C57 H57A 109.5 . . ? H57B C57 H57A 109.5 . . ? H57C C57 H57A 109.5 . . ? C59 C58 N53 115.8(3) . . ? C59 C58 H58A 108.3 . . ? N53 C58 H58A 108.3 . . ? C59 C58 H58B 108.3 . . ? N53 C58 H58B 108.3 . . ? H58A C58 H58B 107.4 . . ? C58 C59 C60 110.8(3) . . ? C58 C59 H59A 109.5 . . ? C60 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 108.1 . . ? C59 C60 C61 113.0(4) . . ? C59 C60 H60B 109.0 . . ? C61 C60 H60B 109.0 . . ? C59 C60 H60A 109.0 . . ? C61 C60 H60A 109.0 . . ? H60B C60 H60A 107.8 . . ? C60 C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C61 H61A 109.5 . . ? H61B C61 H61A 109.5 . . ? H61C C61 H61A 109.5 . . ? C63 C62 N53 116.5(3) . . ? C63 C62 H62A 108.2 . . ? N53 C62 H62A 108.2 . . ? C63 C62 H62B 108.2 . . ? N53 C62 H62B 108.2 . . ? H62A C62 H62B 107.3 . . ? C62 C63 C64 110.3(3) . . ? C62 C63 H63A 109.6 . . ? C64 C63 H63A 109.6 . . ? C62 C63 H63B 109.6 . . ? C64 C63 H63B 109.6 . . ? H63A C63 H63B 108.1 . . ? C65 C64 C63 112.2(4) . . ? C65 C64 H64A 109.2 . . ? C63 C64 H64A 109.2 . . ? C65 C64 H64B 109.2 . . ? C63 C64 H64B 109.2 . . ? H64A C64 H64B 107.9 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? H65C C65 H65B 109.5 . . ? N53 C66 C67 115.3(3) . . ? N53 C66 H66A 108.5 . . ? C67 C66 H66A 108.5 . . ? N53 C66 H66B 108.5 . . ? C67 C66 H66B 108.5 . . ? H66A C66 H66B 107.5 . . ? C68 C67 C66 110.0(3) . . ? C68 C67 H67A 109.7 . . ? C66 C67 H67A 109.7 . . ? C68 C67 H67B 109.7 . . ? C66 C67 H67B 109.7 . . ? H67A C67 H67B 108.2 . . ? C67 C68 C69 112.8(4) . . ? C67 C68 H68A 109.0 . . ? C69 C68 H68A 109.0 . . ? C67 C68 H68B 109.0 . . ? C69 C68 H68B 109.0 . . ? H68A C68 H68B 107.8 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? H69C C69 H69B 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N9 H9 O4 0.95(5) 2.12(5) 3.036(5) 161(4) 1 N25 H25 O2 0.83(4) 2.14(4) 2.943(5) 162(4) 1 N41 H41 O3 0.85(5) 2.14(6) 2.982(5) 169(5) 1 C13 H13 O3 0.93 2.55 3.437(5) 158.8 1 C29 H29 O2 0.93 2.51 3.247(5) 136.5 1 C32 H32 O43 0.93 2.36 3.260(5) 163.3 1_455 C54 H54A O27 0.97 2.37 3.183(5) 141.0 2_565 C62 H62A O27 0.97 2.44 3.319(5) 150.0 2_565 C62 H62B O35 0.97 2.54 3.199(5) 124.8 2_565 C58 H58A O43 0.97 2.24 3.182(5) 163.7 1 C65 H65A O35 0.96 2.56 3.403(5) 146.6 1_655 C59 H59A O19 0.97 2.57 3.457(6) 152.2 1_565 C66 H66A O11 0.97 2.43 3.154(5) 130.9 1_565 C68 H68A O20 0.97 2.52 3.468(6) 165.5 1_565 C57 H57C O36 0.96 2.53 3.438(6) 157.0 1_665 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.89 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.425 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.078 # Attachment 'complex-4.cif' data_tonaac_0m _database_code_depnum_ccdc_archive 'CCDC 733121' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H71 N7 O12' _chemical_formula_weight 974.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9277(19) _cell_length_b 14.647(2) _cell_length_c 15.513(2) _cell_angle_alpha 62.355(2) _cell_angle_beta 73.693(2) _cell_angle_gamma 77.867(2) _cell_volume 2486.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6213 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 23.98 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9780 _exptl_absorpt_correction_T_max 0.9871 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'BRUKER CCD AREA DETECTOR' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23294 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 24.96 _reflns_number_total 8696 _reflns_number_gt 6356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'MERCURY 1.4' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0844P)^2^+0.7370P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8696 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1523 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 1.03869(15) 0.68242(13) 0.61349(13) 0.0368(4) Uani 1 1 d . . . C2 C 0.9717(2) 0.6176(2) 0.63816(18) 0.0318(6) Uani 1 1 d . . . O3 O 0.87408(14) 0.62469(14) 0.68027(13) 0.0362(4) Uani 1 1 d . . . C4 C 1.0137(2) 0.5253(2) 0.6157(2) 0.0407(7) Uani 1 1 d . . . H4C H 1.0447 0.4715 0.6694 0.061 Uiso 1 1 calc R . . H4A H 1.0680 0.5450 0.5551 0.061 Uiso 1 1 calc R . . H4B H 0.9552 0.5005 0.6082 0.061 Uiso 1 1 calc R . . O5A O 0.75321(18) 0.39277(15) 0.42303(15) 0.0282(5) Uiso 0.81 1 d P . . O5B O 0.8165(9) 0.3803(7) 0.4078(7) 0.038(2) Uiso 0.19 1 d P . . C6 C 0.71273(19) 0.4101(2) 0.21057(19) 0.0329(6) Uani 1 1 d . . . H6A H 0.6600 0.4640 0.2188 0.049 Uiso 1 1 calc R . . H6B H 0.7095 0.3500 0.2733 0.049 Uiso 1 1 calc R . . H6C H 0.6977 0.3930 0.1629 0.049 Uiso 1 1 calc R . . C7 C 0.82459(18) 0.44709(18) 0.17396(16) 0.0234(5) Uani 1 1 d . . . C8 C 0.83849(18) 0.54901(17) 0.14944(16) 0.0224(5) Uani 1 1 d . . . C9 C 0.74144(19) 0.62081(18) 0.16750(17) 0.0263(5) Uani 1 1 d . . . H9A H 0.7575 0.6922 0.1268 0.032 Uiso 1 1 calc R . . H9B H 0.6803 0.6104 0.1495 0.032 Uiso 1 1 calc R . . N10 N 0.71481(16) 0.59901(16) 0.27321(15) 0.0257(5) Uani 1 1 d . . . H10 H 0.739(2) 0.536(2) 0.319(2) 0.042(8) Uiso 1 1 d . . . C11 C 0.65867(18) 0.66926(17) 0.30470(17) 0.0240(5) Uani 1 1 d . . . O12 O 0.61482(13) 0.75123(13) 0.25077(12) 0.0321(4) Uani 1 1 d . . . C13 C 0.64489(18) 0.64053(17) 0.41316(17) 0.0248(5) Uani 1 1 d . . . C14 C 0.5452(2) 0.61114(19) 0.47487(19) 0.0320(6) Uani 1 1 d . . . H14 H 0.4899 0.6103 0.4478 0.038 Uiso 1 1 calc R . . C15 C 0.5263(2) 0.5832(2) 0.57567(19) 0.0374(6) Uani 1 1 d . . . H15 H 0.4590 0.5629 0.6156 0.045 Uiso 1 1 calc R . . C16 C 0.6061(2) 0.5850(2) 0.61745(19) 0.0360(6) Uani 1 1 d . . . H16 H 0.5928 0.5655 0.6855 0.043 Uiso 1 1 calc R . . C17 C 0.7060(2) 0.61568(18) 0.55840(18) 0.0324(6) Uani 1 1 d . . . H17 H 0.7604 0.6179 0.5857 0.039 Uiso 1 1 calc R . . C18 C 0.72341(19) 0.64300(18) 0.45761(17) 0.0260(5) Uani 1 1 d . . . N19 N 0.82960(16) 0.67829(16) 0.39624(16) 0.0301(5) Uani 1 1 d . . . O20 O 0.83804(14) 0.72797(13) 0.30612(12) 0.0333(4) Uani 1 1 d . . . O21 O 0.90433(14) 0.65657(15) 0.43831(14) 0.0411(5) Uani 1 1 d . . . C22 C 0.9564(2) 0.69401(18) 0.08647(18) 0.0286(5) Uani 1 1 d . . . H22A H 1.0312 0.7063 0.0585 0.043 Uiso 1 1 calc R . . H22B H 0.9327 0.7067 0.1447 0.043 Uiso 1 1 calc R . . H22C H 0.9137 0.7396 0.0383 0.043 Uiso 1 1 calc R . . C23 C 0.94295(18) 0.58233(17) 0.11467(16) 0.0219(5) Uani 1 1 d . . . C24 C 1.03313(18) 0.51300(17) 0.10677(15) 0.0204(5) Uani 1 1 d . . . C25 C 1.14563(18) 0.54812(18) 0.07220(17) 0.0247(5) Uani 1 1 d . . . H25A H 1.1977 0.4952 0.0594 0.030 Uiso 1 1 calc R . . H25B H 1.1493 0.6108 0.0104 0.030 Uiso 1 1 calc R . . N26 N 1.17404(15) 0.56802(15) 0.14670(15) 0.0232(4) Uani 1 1 d . . . H26 H 1.164(2) 0.521(2) 0.208(2) 0.037(8) Uiso 1 1 d . . . C27 C 1.22584(18) 0.65004(18) 0.12011(17) 0.0260(5) Uani 1 1 d . . . O28 O 1.25574(16) 0.71214(14) 0.03319(12) 0.0419(5) Uani 1 1 d . . . C29 C 1.24059(18) 0.67096(17) 0.20152(17) 0.0245(5) Uani 1 1 d . . . C30 C 1.1523(2) 0.68657(18) 0.26975(18) 0.0303(6) Uani 1 1 d . . . H30 H 1.0844 0.6730 0.2716 0.036 Uiso 1 1 calc R . . C31 C 1.1627(2) 0.7221(2) 0.33554(19) 0.0348(6) Uani 1 1 d . . . H31 H 1.1023 0.7316 0.3811 0.042 Uiso 1 1 calc R . . C32 C 1.2630(2) 0.7434(2) 0.33325(19) 0.0334(6) Uani 1 1 d . . . H32 H 1.2699 0.7671 0.3774 0.040 Uiso 1 1 calc R . . C33 C 1.3532(2) 0.72943(18) 0.26531(18) 0.0296(6) Uani 1 1 d . . . H33 H 1.4209 0.7440 0.2628 0.035 Uiso 1 1 calc R . . C34 C 1.34007(18) 0.69352(17) 0.20162(17) 0.0250(5) Uani 1 1 d . . . N35 N 1.43736(16) 0.67874(16) 0.13182(15) 0.0299(5) Uani 1 1 d . . . O36 O 1.49993(13) 0.74624(13) 0.08830(13) 0.0354(4) Uani 1 1 d . . . O37 O 1.45360(16) 0.59809(15) 0.12244(16) 0.0507(5) Uani 1 1 d . . . C38 C 1.11854(19) 0.33437(18) 0.12836(18) 0.0283(5) Uani 1 1 d . . . H38A H 1.0964 0.2679 0.1471 0.042 Uiso 1 1 calc R . . H38B H 1.1606 0.3280 0.1733 0.042 Uiso 1 1 calc R . . H38C H 1.1615 0.3594 0.0618 0.042 Uiso 1 1 calc R . . C39 C 1.01973(18) 0.40942(17) 0.13300(15) 0.0216(5) Uani 1 1 d . . . C40 C 0.91550(19) 0.37796(17) 0.16539(16) 0.0227(5) Uani 1 1 d . . . C41 C 0.8983(2) 0.26625(18) 0.19805(17) 0.0266(5) Uani 1 1 d . . . H41A H 0.8292 0.2636 0.1866 0.032 Uiso 1 1 calc R . . H41B H 0.9547 0.2376 0.1586 0.032 Uiso 1 1 calc R . . N42 N 0.90026(17) 0.20418(15) 0.30356(15) 0.0260(5) Uani 1 1 d . . . H42 H 0.927(2) 0.226(2) 0.330(2) 0.039(8) Uiso 1 1 d . . . C43 C 0.85754(18) 0.11334(17) 0.35381(17) 0.0234(5) Uani 1 1 d . . . O44 O 0.81513(15) 0.07983(13) 0.31421(13) 0.0370(4) Uani 1 1 d . . . C45 C 0.86065(18) 0.05274(18) 0.46215(17) 0.0244(5) Uani 1 1 d . . . C46 C 0.87971(19) 0.09478(18) 0.51939(17) 0.0270(5) Uani 1 1 d . . . H46 H 0.8948 0.1635 0.4895 0.032 Uiso 1 1 calc R . . C47 C 0.8767(2) 0.0364(2) 0.62018(19) 0.0337(6) Uani 1 1 d . . . H47 H 0.8893 0.0664 0.6571 0.040 Uiso 1 1 calc R . . C48 C 0.8552(2) -0.06564(19) 0.66623(18) 0.0330(6) Uani 1 1 d . . . H48 H 0.8534 -0.1041 0.7340 0.040 Uiso 1 1 calc R . . C49 C 0.83639(19) -0.11108(19) 0.61222(18) 0.0303(6) Uani 1 1 d . . . H49 H 0.8220 -0.1800 0.6425 0.036 Uiso 1 1 calc R . . C50 C 0.83953(19) -0.05111(18) 0.51208(18) 0.0282(5) Uani 1 1 d . . . N51 N 0.8258(2) -0.10831(17) 0.45828(18) 0.0430(6) Uani 1 1 d . . . O52 O 0.9069(2) -0.13201(17) 0.40682(18) 0.0608(6) Uani 1 1 d . . . O53 O 0.7365(2) -0.13255(17) 0.47291(17) 0.0695(7) Uani 1 1 d . . . N54 N 0.62909(14) 0.03925(14) 0.17661(13) 0.0210(4) Uani 1 1 d . . . C55 C 0.62769(18) 0.05992(17) 0.07177(16) 0.0230(5) Uani 1 1 d . . . H55A H 0.6744 0.1142 0.0254 0.028 Uiso 1 1 calc R . . H55B H 0.5547 0.0861 0.0610 0.028 Uiso 1 1 calc R . . C56 C 0.66306(18) -0.03217(17) 0.04655(17) 0.0238(5) Uani 1 1 d . . . H56A H 0.7367 -0.0583 0.0550 0.029 Uiso 1 1 calc R . . H56B H 0.6167 -0.0871 0.0917 0.029 Uiso 1 1 calc R . . C57 C 0.65691(18) -0.00098(18) -0.06009(17) 0.0255(5) Uani 1 1 d . . . H57A H 0.5829 0.0240 -0.0679 0.031 Uiso 1 1 calc R . . H57B H 0.7019 0.0551 -0.1048 0.031 Uiso 1 1 calc R . . C58 C 0.6939(2) -0.0905(2) -0.08819(18) 0.0315(6) Uani 1 1 d . . . H58A H 0.7681 -0.1134 -0.0834 0.047 Uiso 1 1 calc R . . H58B H 0.6871 -0.0684 -0.1553 0.047 Uiso 1 1 calc R . . H58C H 0.6498 -0.1464 -0.0438 0.047 Uiso 1 1 calc R . . C59 C 0.61436(18) 0.14221(17) 0.18240(17) 0.0237(5) Uani 1 1 d . . . H59A H 0.6252 0.1293 0.2466 0.028 Uiso 1 1 calc R . . H59B H 0.6701 0.1847 0.1317 0.028 Uiso 1 1 calc R . . C60 C 0.50522(18) 0.20260(18) 0.16901(19) 0.0282(6) Uani 1 1 d . . . H60A H 0.4500 0.1667 0.2260 0.034 Uiso 1 1 calc R . . H60B H 0.4883 0.2066 0.1102 0.034 Uiso 1 1 calc R . . C61 C 0.5043(2) 0.31155(19) 0.1582(2) 0.0347(6) Uani 1 1 d . . . H61A H 0.5191 0.3076 0.2179 0.042 Uiso 1 1 calc R . . H61B H 0.5610 0.3468 0.1024 0.042 Uiso 1 1 calc R . . C62 C 0.3962(2) 0.3728(2) 0.1418(3) 0.0508(8) Uani 1 1 d . . . H62A H 0.3803 0.3748 0.0840 0.076 Uiso 1 1 calc R . . H62B H 0.3988 0.4421 0.1319 0.076 Uiso 1 1 calc R . . H62C H 0.3407 0.3404 0.1990 0.076 Uiso 1 1 calc R . . C63 C 0.53796(18) -0.02707(18) 0.24887(17) 0.0240(5) Uani 1 1 d . . . H63A H 0.4707 0.0074 0.2277 0.029 Uiso 1 1 calc R . . H63B H 0.5510 -0.0924 0.2441 0.029 Uiso 1 1 calc R . . C64 C 0.52324(19) -0.0497(2) 0.35665(17) 0.0301(6) Uani 1 1 d . . . H64A H 0.5082 0.0148 0.3632 0.036 Uiso 1 1 calc R . . H64B H 0.5894 -0.0851 0.3796 0.036 Uiso 1 1 calc R . . C65 C 0.4302(2) -0.1170(2) 0.42040(18) 0.0319(6) Uani 1 1 d . . . H65A H 0.3636 -0.0795 0.3995 0.038 Uiso 1 1 calc R . . H65B H 0.4433 -0.1790 0.4098 0.038 Uiso 1 1 calc R . . C66 C 0.4167(2) -0.1474(2) 0.52993(19) 0.0426(7) Uani 1 1 d . . . H66A H 0.4827 -0.1838 0.5508 0.064 Uiso 1 1 calc R . . H66B H 0.3589 -0.1913 0.5673 0.064 Uiso 1 1 calc R . . H66C H 0.3999 -0.0863 0.5413 0.064 Uiso 1 1 calc R . . C67 C 0.73582(17) -0.01868(17) 0.20353(17) 0.0227(5) Uani 1 1 d . . . H67A H 0.7351 -0.0284 0.2699 0.027 Uiso 1 1 calc R . . H67B H 0.7408 -0.0868 0.2059 0.027 Uiso 1 1 calc R . . C68 C 0.83656(18) 0.03276(18) 0.13380(17) 0.0249(5) Uani 1 1 d . . . H68A H 0.8397 0.0955 0.1391 0.030 Uiso 1 1 calc R . . H68B H 0.8345 0.0513 0.0656 0.030 Uiso 1 1 calc R . . C69 C 0.93586(19) -0.04187(19) 0.16158(19) 0.0320(6) Uani 1 1 d . . . H69A H 0.9276 -0.0739 0.2334 0.038 Uiso 1 1 calc R . . H69B H 0.9409 -0.0963 0.1411 0.038 Uiso 1 1 calc R . . C70 C 1.0395(2) 0.0111(2) 0.1136(2) 0.0385(6) Uani 1 1 d . . . H70A H 1.0462 0.0460 0.0427 0.058 Uiso 1 1 calc R . . H70B H 1.1002 -0.0396 0.1292 0.058 Uiso 1 1 calc R . . H70C H 1.0378 0.0606 0.1384 0.058 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 O1 0.0465(11) 0.0307(10) 0.0367(10) -0.0126(8) -0.0088(8) -0.0155(8) C2 0.0376(15) 0.0341(14) 0.0238(13) -0.0106(11) -0.0064(11) -0.0082(12) O3 0.0403(11) 0.0371(10) 0.0312(10) -0.0134(8) -0.0055(8) -0.0094(8) C4 0.0519(17) 0.0306(15) 0.0428(16) -0.0154(13) -0.0113(13) -0.0092(13) C6 0.0284(13) 0.0368(15) 0.0342(14) -0.0148(12) -0.0003(11) -0.0142(11) C7 0.0269(13) 0.0282(13) 0.0174(11) -0.0091(10) -0.0028(9) -0.0114(10) C8 0.0226(12) 0.0248(12) 0.0200(12) -0.0086(10) -0.0036(9) -0.0065(9) C9 0.0274(13) 0.0293(13) 0.0224(12) -0.0096(10) -0.0050(10) -0.0071(10) N10 0.0291(11) 0.0220(11) 0.0233(11) -0.0078(9) -0.0039(9) -0.0039(9) C11 0.0194(12) 0.0226(13) 0.0307(13) -0.0111(11) -0.0027(10) -0.0078(10) O12 0.0367(10) 0.0267(9) 0.0317(10) -0.0119(8) -0.0100(8) 0.0015(8) C13 0.0259(12) 0.0186(12) 0.0306(13) -0.0115(10) -0.0047(10) -0.0028(9) C14 0.0287(14) 0.0321(14) 0.0354(15) -0.0140(12) -0.0028(11) -0.0101(11) C15 0.0362(15) 0.0395(15) 0.0338(15) -0.0162(12) 0.0045(12) -0.0133(12) C16 0.0456(16) 0.0337(14) 0.0261(14) -0.0134(11) 0.0006(12) -0.0086(12) C17 0.0390(15) 0.0265(13) 0.0334(14) -0.0121(11) -0.0098(12) -0.0053(11) C18 0.0275(13) 0.0224(12) 0.0269(13) -0.0101(10) -0.0021(10) -0.0058(10) N19 0.0302(12) 0.0305(11) 0.0333(13) -0.0151(10) -0.0069(10) -0.0071(9) O20 0.0387(10) 0.0358(10) 0.0252(10) -0.0102(8) -0.0018(8) -0.0166(8) O21 0.0344(11) 0.0469(12) 0.0453(11) -0.0176(9) -0.0141(9) -0.0079(9) C22 0.0344(14) 0.0222(12) 0.0281(13) -0.0083(10) -0.0062(11) -0.0072(10) C23 0.0292(13) 0.0209(12) 0.0173(11) -0.0067(9) -0.0051(9) -0.0092(10) C24 0.0253(12) 0.0219(12) 0.0150(11) -0.0066(9) -0.0034(9) -0.0087(9) C25 0.0267(13) 0.0255(12) 0.0226(12) -0.0102(10) -0.0006(10) -0.0107(10) N26 0.0260(11) 0.0231(11) 0.0203(11) -0.0068(9) -0.0024(8) -0.0117(8) C27 0.0251(12) 0.0256(13) 0.0266(13) -0.0092(11) -0.0014(10) -0.0114(10) O28 0.0614(13) 0.0405(11) 0.0251(10) -0.0071(8) -0.0005(9) -0.0359(10) C29 0.0258(12) 0.0204(12) 0.0257(12) -0.0058(10) -0.0042(10) -0.0106(10) C30 0.0285(13) 0.0306(14) 0.0328(14) -0.0118(11) -0.0029(11) -0.0142(11) C31 0.0342(15) 0.0382(15) 0.0327(14) -0.0165(12) -0.0003(11) -0.0114(12) C32 0.0395(15) 0.0352(15) 0.0329(14) -0.0169(12) -0.0073(12) -0.0135(12) C33 0.0291(13) 0.0275(13) 0.0329(14) -0.0090(11) -0.0095(11) -0.0104(10) C34 0.0257(12) 0.0191(12) 0.0251(12) -0.0045(10) -0.0034(10) -0.0073(10) N35 0.0279(11) 0.0294(12) 0.0305(11) -0.0088(9) -0.0072(9) -0.0073(9) O36 0.0270(9) 0.0374(10) 0.0366(10) -0.0073(8) -0.0038(8) -0.0179(8) O37 0.0488(12) 0.0404(12) 0.0638(14) -0.0320(11) 0.0113(10) -0.0146(9) C38 0.0329(14) 0.0238(12) 0.0283(13) -0.0098(10) -0.0068(11) -0.0060(10) C39 0.0277(12) 0.0226(12) 0.0140(11) -0.0051(9) -0.0038(9) -0.0088(10) C40 0.0334(13) 0.0211(12) 0.0164(11) -0.0063(9) -0.0069(10) -0.0101(10) C41 0.0349(14) 0.0253(13) 0.0214(12) -0.0081(10) -0.0050(10) -0.0128(10) N42 0.0348(12) 0.0251(11) 0.0210(10) -0.0069(9) -0.0060(9) -0.0156(9) C43 0.0255(12) 0.0212(12) 0.0244(12) -0.0099(10) -0.0034(10) -0.0065(10) O44 0.0562(12) 0.0287(10) 0.0305(10) -0.0079(8) -0.0125(9) -0.0204(8) C45 0.0206(12) 0.0256(12) 0.0239(12) -0.0084(10) -0.0015(9) -0.0058(10) C46 0.0308(13) 0.0236(12) 0.0249(13) -0.0094(10) -0.0026(10) -0.0058(10) C47 0.0372(15) 0.0361(15) 0.0298(14) -0.0184(12) -0.0054(11) 0.0005(12) C48 0.0331(14) 0.0295(14) 0.0225(13) -0.0044(11) 0.0003(10) 0.0000(11) C49 0.0274(13) 0.0241(13) 0.0311(14) -0.0048(11) -0.0039(11) -0.0062(10) C50 0.0276(13) 0.0245(13) 0.0313(13) -0.0085(11) -0.0065(10) -0.0085(10) N51 0.0591(17) 0.0251(12) 0.0430(14) 0.0022(11) -0.0272(13) -0.0194(12) O52 0.0864(18) 0.0492(14) 0.0656(15) -0.0364(12) -0.0300(14) 0.0034(12) O53 0.0823(17) 0.0572(14) 0.0665(15) 0.0038(12) -0.0380(13) -0.0456(13) N54 0.0213(10) 0.0210(10) 0.0220(10) -0.0097(8) -0.0019(8) -0.0072(8) C55 0.0225(12) 0.0230(12) 0.0235(12) -0.0084(10) -0.0046(9) -0.0066(9) C56 0.0238(12) 0.0226(12) 0.0249(12) -0.0097(10) -0.0024(10) -0.0067(10) C57 0.0213(12) 0.0311(13) 0.0247(12) -0.0123(10) -0.0020(10) -0.0073(10) C58 0.0271(13) 0.0431(15) 0.0300(14) -0.0203(12) -0.0013(10) -0.0103(11) C59 0.0256(12) 0.0219(12) 0.0271(12) -0.0127(10) -0.0019(10) -0.0090(10) C60 0.0247(13) 0.0277(13) 0.0369(14) -0.0173(11) -0.0042(11) -0.0065(10) C61 0.0294(14) 0.0298(14) 0.0543(17) -0.0247(13) -0.0109(12) -0.0032(11) C62 0.0383(17) 0.0380(17) 0.092(2) -0.0403(17) -0.0208(16) 0.0041(13) C63 0.0214(12) 0.0232(12) 0.0278(13) -0.0102(10) -0.0019(10) -0.0091(9) C64 0.0269(13) 0.0359(14) 0.0275(13) -0.0127(11) -0.0014(10) -0.0112(11) C65 0.0277(13) 0.0309(14) 0.0311(14) -0.0092(11) 0.0005(11) -0.0101(11) C66 0.0379(16) 0.0454(17) 0.0320(15) -0.0099(13) 0.0037(12) -0.0109(13) C67 0.0217(12) 0.0245(12) 0.0226(12) -0.0097(10) -0.0049(9) -0.0042(9) C68 0.0240(12) 0.0271(13) 0.0258(12) -0.0129(10) -0.0023(10) -0.0075(10) C69 0.0255(13) 0.0321(14) 0.0336(14) -0.0112(11) -0.0015(11) -0.0069(11) C70 0.0239(13) 0.0412(16) 0.0471(17) -0.0183(13) -0.0003(12) -0.0082(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.273(3) . ? C2 O3 1.255(3) . ? C2 C4 1.506(4) . ? C4 H4C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? O5A O5B 0.792(10) 1 ? O5A O5B 0.792(10) . ? O5B O5B 0.00(4) 1 ? O5B O5A 0.792(10) 1 ? C6 C7 1.513(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.397(3) . ? C7 C40 1.400(3) . ? C8 C23 1.406(3) . ? C8 C9 1.510(3) . ? C9 N10 1.467(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? N10 C11 1.333(3) . ? N10 H10 0.92(3) . ? C11 O12 1.229(3) . ? C11 C13 1.499(3) . ? C13 C14 1.386(3) . ? C13 C18 1.392(3) . ? C14 C15 1.381(4) . ? C14 H14 0.9300 . ? C15 C16 1.374(4) . ? C15 H15 0.9300 . ? C16 C17 1.381(4) . ? C16 H16 0.9300 . ? C17 C18 1.384(3) . ? C17 H17 0.9300 . ? C18 N19 1.472(3) . ? N19 O21 1.222(3) . ? N19 O20 1.225(3) . ? C22 C23 1.520(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.394(3) . ? C24 C39 1.413(3) . ? C24 C25 1.513(3) . ? C25 N26 1.467(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? N26 C27 1.336(3) . ? N26 H26 0.87(3) . ? C27 O28 1.230(3) . ? C27 C29 1.498(3) . ? C29 C30 1.383(3) . ? C29 C34 1.394(3) . ? C30 C31 1.390(4) . ? C30 H30 0.9300 . ? C31 C32 1.383(4) . ? C31 H31 0.9300 . ? C32 C33 1.386(4) . ? C32 H32 0.9300 . ? C33 C34 1.377(3) . ? C33 H33 0.9300 . ? C34 N35 1.463(3) . ? N35 O36 1.224(2) . ? N35 O37 1.224(3) . ? C38 C39 1.509(3) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.395(3) . ? C40 C41 1.518(3) . ? C41 N42 1.462(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? N42 C43 1.337(3) . ? N42 H42 0.80(3) . ? C43 O44 1.225(3) . ? C43 C45 1.501(3) . ? C45 C46 1.387(3) . ? C45 C50 1.397(3) . ? C46 C47 1.384(3) . ? C46 H46 0.9300 . ? C47 C48 1.376(4) . ? C47 H47 0.9300 . ? C48 C49 1.380(4) . ? C48 H48 0.9300 . ? C49 C50 1.378(3) . ? C49 H49 0.9300 . ? C50 N51 1.492(3) . ? N51 O53 1.208(3) . ? N51 O52 1.221(3) . ? N54 C55 1.515(3) . ? N54 C67 1.517(3) . ? N54 C59 1.521(3) . ? N54 C63 1.522(3) . ? C55 C56 1.520(3) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.520(3) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.512(3) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C60 1.512(3) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.523(3) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.512(4) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 C64 1.508(3) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.524(3) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C66 1.510(4) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 C68 1.516(3) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.521(3) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.515(3) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C2 O1 124.9(2) . . ? O3 C2 C4 118.0(2) . . ? O1 C2 C4 117.1(2) . . ? C2 C4 H4C 109.5 . . ? C2 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C40 119.5(2) . . ? C8 C7 C6 120.9(2) . . ? C40 C7 C6 119.5(2) . . ? C7 C8 C23 120.2(2) . . ? C7 C8 C9 119.5(2) . . ? C23 C8 C9 120.1(2) . . ? N10 C9 C8 108.90(18) . . ? N10 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? N10 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C11 N10 C9 121.6(2) . . ? C11 N10 H10 119.0(17) . . ? C9 N10 H10 119.3(17) . . ? O12 C11 N10 123.2(2) . . ? O12 C11 C13 120.4(2) . . ? N10 C11 C13 116.3(2) . . ? C14 C13 C18 116.6(2) . . ? C14 C13 C11 117.9(2) . . ? C18 C13 C11 125.5(2) . . ? C15 C14 C13 121.4(2) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 120.6(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 120.0(2) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 118.5(2) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C17 C18 C13 123.0(2) . . ? C17 C18 N19 117.1(2) . . ? C13 C18 N19 119.9(2) . . ? O21 N19 O20 123.7(2) . . ? O21 N19 C18 118.0(2) . . ? O20 N19 C18 118.29(19) . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C8 120.0(2) . . ? C24 C23 C22 120.6(2) . . ? C8 C23 C22 119.4(2) . . ? C23 C24 C39 120.1(2) . . ? C23 C24 C25 119.9(2) . . ? C39 C24 C25 119.9(2) . . ? N26 C25 C24 111.50(18) . . ? N26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? N26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C27 N26 C25 121.2(2) . . ? C27 N26 H26 120.2(18) . . ? C25 N26 H26 118.1(18) . . ? O28 C27 N26 123.6(2) . . ? O28 C27 C29 118.6(2) . . ? N26 C27 C29 117.6(2) . . ? C30 C29 C34 116.6(2) . . ? C30 C29 C27 120.8(2) . . ? C34 C29 C27 121.6(2) . . ? C29 C30 C31 121.5(2) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C32 C31 C30 120.0(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.1(2) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 118.4(2) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C33 C34 C29 123.4(2) . . ? C33 C34 N35 116.7(2) . . ? C29 C34 N35 119.9(2) . . ? O36 N35 O37 123.5(2) . . ? O36 N35 C34 118.2(2) . . ? O37 N35 C34 118.28(19) . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C24 119.3(2) . . ? C40 C39 C38 121.4(2) . . ? C24 C39 C38 119.3(2) . . ? C39 C40 C7 120.9(2) . . ? C39 C40 C41 120.7(2) . . ? C7 C40 C41 118.4(2) . . ? N42 C41 C40 110.86(18) . . ? N42 C41 H41A 109.5 . . ? C40 C41 H41A 109.5 . . ? N42 C41 H41B 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C43 N42 C41 120.2(2) . . ? C43 N42 H42 121(2) . . ? C41 N42 H42 119(2) . . ? O44 C43 N42 121.8(2) . . ? O44 C43 C45 119.9(2) . . ? N42 C43 C45 118.3(2) . . ? C46 C45 C50 116.0(2) . . ? C46 C45 C43 123.7(2) . . ? C50 C45 C43 120.2(2) . . ? C47 C46 C45 121.2(2) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C48 C47 C46 120.7(2) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C49 120.2(2) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C50 C49 C48 117.9(2) . . ? C50 C49 H49 121.0 . . ? C48 C49 H49 121.0 . . ? C49 C50 C45 123.9(2) . . ? C49 C50 N51 114.3(2) . . ? C45 C50 N51 121.7(2) . . ? O53 N51 O52 124.8(3) . . ? O53 N51 C50 117.7(3) . . ? O52 N51 C50 117.4(2) . . ? C55 N54 C67 110.46(16) . . ? C55 N54 C59 108.80(16) . . ? C67 N54 C59 109.35(16) . . ? C55 N54 C63 108.83(16) . . ? C67 N54 C63 108.65(16) . . ? C59 N54 C63 110.74(16) . . ? N54 C55 C56 116.01(18) . . ? N54 C55 H55A 108.3 . . ? C56 C55 H55A 108.3 . . ? N54 C55 H55B 108.3 . . ? C56 C55 H55B 108.3 . . ? H55A C55 H55B 107.4 . . ? C57 C56 C55 110.52(19) . . ? C57 C56 H56A 109.5 . . ? C55 C56 H56A 109.5 . . ? C57 C56 H56B 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 108.1 . . ? C58 C57 C56 111.8(2) . . ? C58 C57 H57A 109.3 . . ? C56 C57 H57A 109.3 . . ? C58 C57 H57B 109.3 . . ? C56 C57 H57B 109.3 . . ? H57A C57 H57B 107.9 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 N54 114.91(18) . . ? C60 C59 H59A 108.5 . . ? N54 C59 H59A 108.5 . . ? C60 C59 H59B 108.5 . . ? N54 C59 H59B 108.5 . . ? H59A C59 H59B 107.5 . . ? C59 C60 C61 111.19(19) . . ? C59 C60 H60A 109.4 . . ? C61 C60 H60A 109.4 . . ? C59 C60 H60B 109.4 . . ? C61 C60 H60B 109.4 . . ? H60A C60 H60B 108.0 . . ? C62 C61 C60 111.1(2) . . ? C62 C61 H61A 109.4 . . ? C60 C61 H61A 109.4 . . ? C62 C61 H61B 109.4 . . ? C60 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 N54 115.88(18) . . ? C64 C63 H63A 108.3 . . ? N54 C63 H63A 108.3 . . ? C64 C63 H63B 108.3 . . ? N54 C63 H63B 108.3 . . ? H63A C63 H63B 107.4 . . ? C63 C64 C65 110.31(19) . . ? C63 C64 H64A 109.6 . . ? C65 C64 H64A 109.6 . . ? C63 C64 H64B 109.6 . . ? C65 C64 H64B 109.6 . . ? H64A C64 H64B 108.1 . . ? C66 C65 C64 112.3(2) . . ? C66 C65 H65A 109.1 . . ? C64 C65 H65A 109.1 . . ? C66 C65 H65B 109.1 . . ? C64 C65 H65B 109.1 . . ? H65A C65 H65B 107.9 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C68 C67 N54 115.71(18) . . ? C68 C67 H67A 108.4 . . ? N54 C67 H67A 108.4 . . ? C68 C67 H67B 108.4 . . ? N54 C67 H67B 108.4 . . ? H67A C67 H67B 107.4 . . ? C67 C68 C69 109.06(19) . . ? C67 C68 H68A 109.9 . . ? C69 C68 H68A 109.9 . . ? C67 C68 H68B 109.9 . . ? C69 C68 H68B 109.9 . . ? H68A C68 H68B 108.3 . . ? C70 C69 C68 112.4(2) . . ? C70 C69 H69A 109.1 . . ? C68 C69 H69A 109.1 . . ? C70 C69 H69B 109.1 . . ? C68 C69 H69B 109.1 . . ? H69A C69 H69B 107.8 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N10 H10 O5A 0.92(3) 1.97(3) 2.877(3) 166(2) 1 N10 H10 O5B 0.92(3) 2.24(3) 3.149(10) 170(2) 1 N26 H26 O3 0.87(3) 2.08(3) 2.886(3) 154(2) 2_766 N42 H42 O1 0.80(3) 2.08(3) 2.853(3) 163(3) 2_766 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.682 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.055