# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 188/156 data_comp4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H58 O9' _chemical_formula_weight 851.00 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.979(5) _cell_length_b 12.7224(11) _cell_length_c 17.618(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.88(3) _cell_angle_gamma 90.00 _cell_volume 4645.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 283 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22.58 _cell_measurement_theta_max 28.42 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9634 _exptl_absorpt_correction_T_max 0.9712 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 283 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 300 _diffrn_standards_decay_% 2 _diffrn_reflns_number 8376 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.1160 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 24.97 _reflns_number_total 8140 _reflns_number_gt 3599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'WinGX publication routines (Farrugia, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _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^)+(0.0300P)^2^+0.5000P] 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 8140 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2107 _refine_ls_R_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.1640 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.320 _refine_ls_restrained_S_all 1.320 _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 O1 O 0.10939(13) -0.1342(2) -0.00085(16) 0.0414(8) Uani 1 1 d . . . O2 O 0.20880(14) 0.0260(2) 0.24378(16) 0.0457(8) Uani 1 1 d . . . O3 O 0.32342(15) -0.0107(2) -0.04331(17) 0.0515(9) Uani 1 1 d . . . O4 O 0.37111(14) -0.2320(2) 0.18747(17) 0.0484(9) Uani 1 1 d . . . O5 O 0.4451(3) -0.4020(4) 0.1472(3) 0.157(3) Uani 1 1 d . . . O6 O 0.3526(3) -0.5477(4) 0.1151(3) 0.142(2) Uani 1 1 d . . . O7 O 0.19181(17) -0.5589(3) 0.0425(2) 0.0702(11) Uani 1 1 d . . . O8 O 0.07827(15) -0.4628(3) -0.06133(19) 0.0590(10) Uani 1 1 d . . . O9 O 0.05048(15) -0.2733(2) -0.12738(18) 0.0535(9) Uani 1 1 d . . . C1 C 0.1346(2) -0.0330(3) 0.0115(3) 0.0398(12) Uani 1 1 d . . . C2 C 0.1721(2) 0.0067(3) -0.0403(3) 0.0393(11) Uani 1 1 d . . . C3 C 0.1941(2) 0.1093(4) -0.0299(3) 0.0519(14) Uani 1 1 d . . . H3 H 0.2186 0.1385 -0.0643 0.062 Uiso 1 1 calc R . . C4 C 0.1799(3) 0.1680(4) 0.0306(3) 0.0611(15) Uani 1 1 d . . . H4 H 0.1927 0.2380 0.0354 0.073 Uiso 1 1 calc R . . C5 C 0.1467(2) 0.1239(4) 0.0844(3) 0.0540(14) Uani 1 1 d . . . H5 H 0.1394 0.1636 0.1265 0.065 Uiso 1 1 calc R . . C6 C 0.1241(2) 0.0213(4) 0.0769(3) 0.0416(12) Uani 1 1 d . . . C7 C 0.0954(2) -0.0310(4) 0.1412(3) 0.0523(13) Uani 1 1 d . . . H7A H 0.0862 0.0218 0.1777 0.063 Uiso 1 1 calc R . . H7B H 0.0552 -0.0651 0.1203 0.063 Uiso 1 1 calc R . . C8 C 0.1415(2) -0.1114(4) 0.1819(3) 0.0439(12) Uani 1 1 d . . . C9 C 0.1981(2) -0.0800(4) 0.2281(2) 0.0402(12) Uani 1 1 d . . . C10 C 0.2462(2) -0.1522(4) 0.2566(2) 0.0433(12) Uani 1 1 d . . . C11 C 0.2333(2) -0.2578(4) 0.2434(3) 0.0522(14) Uani 1 1 d . . . H11 H 0.2641 -0.3074 0.2626 0.063 Uiso 1 1 calc R . . C12 C 0.1757(3) -0.2907(4) 0.2024(3) 0.0596(15) Uani 1 1 d . . . H12 H 0.1671 -0.3621 0.1961 0.072 Uiso 1 1 calc R . . C13 C 0.1311(2) -0.2179(4) 0.1708(3) 0.0541(14) Uani 1 1 d . . . H13 H 0.0930 -0.2408 0.1413 0.065 Uiso 1 1 calc R . . C14 C 0.1867(3) 0.0589(4) 0.3130(3) 0.0714(17) Uani 1 1 d . . . H14A H 0.1400 0.0563 0.3057 0.086 Uiso 1 1 calc R . . H14B H 0.2030 0.0110 0.3542 0.086 Uiso 1 1 calc R . . C15 C 0.2078(5) 0.1634(6) 0.3338(4) 0.174(5) Uani 1 1 d . . . H15A H 0.1802 0.1885 0.3693 0.209 Uiso 1 1 calc R . . H15B H 0.2507 0.1566 0.3633 0.209 Uiso 1 1 calc R . . C16 C 0.2114(4) 0.2456(5) 0.2810(4) 0.112(3) Uani 1 1 d . . . H16A H 0.2281 0.3075 0.3081 0.169 Uiso 1 1 calc R . . H16B H 0.1690 0.2599 0.2537 0.169 Uiso 1 1 calc R . . H16C H 0.2393 0.2252 0.2453 0.169 Uiso 1 1 calc R . . C17 C 0.3114(2) -0.1135(4) 0.2966(2) 0.0481(13) Uani 1 1 d . . . H17A H 0.3050 -0.0627 0.3358 0.058 Uiso 1 1 calc R . . H17B H 0.3357 -0.1721 0.3215 0.058 Uiso 1 1 calc R . . C18 C 0.3490(2) -0.0630(4) 0.2395(3) 0.0438(12) Uani 1 1 d . . . C19 C 0.3552(2) 0.0450(4) 0.2364(3) 0.0553(14) Uani 1 1 d . . . H19 H 0.3399 0.0865 0.2731 0.066 Uiso 1 1 calc R . . C20 C 0.3839(2) 0.0921(4) 0.1795(3) 0.0593(15) Uani 1 1 d . . . H20 H 0.3909 0.1643 0.1805 0.071 Uiso 1 1 calc R . . C21 C 0.4020(2) 0.0319(4) 0.1213(3) 0.0543(14) Uani 1 1 d . . . H21 H 0.4183 0.0644 0.0810 0.065 Uiso 1 1 calc R . . C22 C 0.3962(2) -0.0772(4) 0.1224(3) 0.0447(13) Uani 1 1 d . . . C23 C 0.3724(2) -0.1230(4) 0.1831(3) 0.0414(12) Uani 1 1 d . . . C24 C 0.4091(2) -0.1429(4) 0.0542(3) 0.0502(13) Uani 1 1 d . . . H24A H 0.4362 -0.2023 0.0724 0.060 Uiso 1 1 calc R . . H24B H 0.4319 -0.1007 0.0212 0.060 Uiso 1 1 calc R . . C25 C 0.3459(2) -0.1826(4) 0.0084(2) 0.0417(12) Uani 1 1 d . . . C26 C 0.3265(2) -0.2847(4) 0.0151(3) 0.0479(13) Uani 1 1 d . . . H26 H 0.3543 -0.3320 0.0437 0.057 Uiso 1 1 calc R . . C27 C 0.2661(2) -0.3189(4) -0.0201(3) 0.0478(13) Uani 1 1 d . . . H27 H 0.2542 -0.3890 -0.0173 0.057 Uiso 1 1 calc R . . C28 C 0.2239(2) -0.2464(4) -0.0595(2) 0.0436(12) Uani 1 1 d . . . H28 H 0.1827 -0.2680 -0.0812 0.052 Uiso 1 1 calc R . . C29 C 0.2417(2) -0.1430(4) -0.0673(2) 0.0372(11) Uani 1 1 d . . . C30 C 0.1924(2) -0.0624(3) -0.1023(2) 0.0453(13) Uani 1 1 d . . . H30A H 0.2109 -0.0192 -0.1388 0.054 Uiso 1 1 calc R . . H30B H 0.1549 -0.0980 -0.1298 0.054 Uiso 1 1 calc R . . C31 C 0.3036(2) -0.1132(4) -0.0354(2) 0.0411(12) Uani 1 1 d . . . C32 C 0.3542(3) 0.0068(4) -0.1085(3) 0.0684(16) Uani 1 1 d . . . H32A H 0.3236 -0.0029 -0.1551 0.082 Uiso 1 1 calc R . . H32B H 0.3892 -0.0431 -0.1088 0.082 Uiso 1 1 calc R . . C33 C 0.3804(3) 0.1176(5) -0.1052(3) 0.097(2) Uani 1 1 d . . . H33A H 0.3456 0.1657 -0.0996 0.116 Uiso 1 1 calc R . . H33B H 0.4127 0.1244 -0.0597 0.116 Uiso 1 1 calc R . . C34 C 0.4091(4) 0.1497(5) -0.1714(4) 0.132(3) Uani 1 1 d . . . H34A H 0.4235 0.2213 -0.1650 0.198 Uiso 1 1 calc R . . H34B H 0.3777 0.1441 -0.2170 0.198 Uiso 1 1 calc R . . H34C H 0.4452 0.1051 -0.1761 0.198 Uiso 1 1 calc R . . C35 C 0.4242(3) -0.2766(4) 0.2375(3) 0.0790(19) Uani 1 1 d . . . H35A H 0.4147 -0.2768 0.2897 0.095 Uiso 1 1 calc R . . H35B H 0.4623 -0.2336 0.2366 0.095 Uiso 1 1 calc R . . C36 C 0.4373(3) -0.3827(5) 0.2153(3) 0.090(2) Uani 1 1 d . . . H36A H 0.4759 -0.4061 0.2486 0.108 Uiso 1 1 calc R . . H36B H 0.4021 -0.4265 0.2265 0.108 Uiso 1 1 calc R . . C37 C 0.4592(4) -0.5000(5) 0.1209(3) 0.081(2) Uani 1 1 d . . . C38 C 0.5202(4) -0.5216(6) 0.1067(4) 0.109(3) Uani 1 1 d . . . H38 H 0.5532 -0.4732 0.1201 0.131 Uiso 1 1 calc R . . C39 C 0.5323(4) -0.6136(7) 0.0732(4) 0.094(2) Uani 1 1 d . . . H39 H 0.5739 -0.6280 0.0643 0.112 Uiso 1 1 calc R . . C40 C 0.4855(4) -0.6845(6) 0.0526(4) 0.099(2) Uani 1 1 d . . . H40 H 0.4946 -0.7473 0.0295 0.119 Uiso 1 1 calc R . . C41 C 0.4247(4) -0.6638(5) 0.0657(4) 0.108(3) Uani 1 1 d . . . H41 H 0.3922 -0.7129 0.0515 0.130 Uiso 1 1 calc R . . C42 C 0.4105(4) -0.5715(5) 0.0996(4) 0.087(2) Uani 1 1 d . . . C43 C 0.3029(3) -0.5869(5) 0.0817(5) 0.136(4) Uani 1 1 d . . . H43A H 0.3044 -0.6621 0.0906 0.163 Uiso 1 1 calc R . . H43B H 0.3009 -0.5755 0.0270 0.163 Uiso 1 1 calc R . . C44 C 0.2411(3) -0.5424(5) 0.1070(3) 0.091(2) Uani 1 1 d . . . H44A H 0.2311 -0.5793 0.1518 0.109 Uiso 1 1 calc R . . H44B H 0.2459 -0.4681 0.1189 0.109 Uiso 1 1 calc R . . C45 C 0.1294(2) -0.5353(4) 0.0559(3) 0.0697(16) Uani 1 1 d . . . H45A H 0.1270 -0.4623 0.0709 0.084 Uiso 1 1 calc R . . H45B H 0.1184 -0.5789 0.0971 0.084 Uiso 1 1 calc R . . C46 C 0.0832(2) -0.5555(4) -0.0167(3) 0.0614(15) Uani 1 1 d . . . H46A H 0.0987 -0.6130 -0.0450 0.074 Uiso 1 1 calc R . . H46B H 0.0412 -0.5746 -0.0044 0.074 Uiso 1 1 calc R . . C47 C 0.0353(2) -0.4614(4) -0.1285(3) 0.0456(13) Uani 1 1 d . . . C48 C 0.0052(2) -0.5496(4) -0.1640(3) 0.0539(14) Uani 1 1 d . . . H48 H 0.0131 -0.6156 -0.1417 0.065 Uiso 1 1 calc R . . C49 C -0.0364(2) -0.5396(5) -0.2319(3) 0.0596(15) Uani 1 1 d . . . H49 H -0.0561 -0.5990 -0.2557 0.072 Uiso 1 1 calc R . . C50 C -0.0490(2) -0.4434(5) -0.2646(3) 0.0642(16) Uani 1 1 d . . . H50 H -0.0771 -0.4375 -0.3108 0.077 Uiso 1 1 calc R . . C51 C -0.0201(2) -0.3542(4) -0.2293(3) 0.0617(15) Uani 1 1 d . . . H51 H -0.0287 -0.2884 -0.2516 0.074 Uiso 1 1 calc R . . C52 C 0.0213(2) -0.3638(4) -0.1612(3) 0.0456(13) Uani 1 1 d . . . C53 C 0.0234(2) -0.2408(4) -0.0621(3) 0.0558(14) Uani 1 1 d . . . H53A H 0.0372 -0.2882 -0.0196 0.067 Uiso 1 1 calc R . . H53B H -0.0233 -0.2435 -0.0738 0.067 Uiso 1 1 calc R . . C54 C 0.0444(2) -0.1314(4) -0.0400(3) 0.0567(15) Uani 1 1 d . . . H54A H 0.0419 -0.0879 -0.0856 0.068 Uiso 1 1 calc R . . H54B H 0.0163 -0.1016 -0.0068 0.068 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 0.0392(19) 0.0314(18) 0.050(2) -0.0023(16) -0.0055(15) -0.0006(15) O2 0.049(2) 0.047(2) 0.043(2) -0.0079(17) 0.0132(15) 0.0019(17) O3 0.061(2) 0.045(2) 0.049(2) 0.0027(17) 0.0096(17) -0.0048(18) O4 0.053(2) 0.044(2) 0.046(2) -0.0008(17) -0.0019(16) 0.0051(18) O5 0.214(6) 0.126(4) 0.104(4) -0.038(4) -0.059(4) 0.118(4) O6 0.104(4) 0.140(5) 0.195(6) -0.024(4) 0.062(4) 0.017(4) O7 0.052(2) 0.052(2) 0.101(3) -0.009(2) -0.003(2) 0.0054(19) O8 0.059(2) 0.050(2) 0.062(2) -0.001(2) -0.0096(19) -0.0063(19) O9 0.052(2) 0.048(2) 0.059(2) -0.0110(18) 0.0025(18) -0.0127(18) C1 0.033(3) 0.032(3) 0.049(3) -0.002(3) -0.009(2) 0.011(2) C2 0.037(3) 0.036(3) 0.040(3) 0.007(2) -0.007(2) 0.007(2) C3 0.057(4) 0.038(3) 0.058(4) 0.015(3) -0.001(3) -0.001(3) C4 0.072(4) 0.032(3) 0.074(4) -0.004(3) -0.005(3) -0.003(3) C5 0.052(3) 0.041(3) 0.064(4) -0.016(3) -0.005(3) 0.000(3) C6 0.034(3) 0.041(3) 0.047(3) -0.007(3) -0.002(2) 0.009(2) C7 0.041(3) 0.063(4) 0.053(3) -0.009(3) 0.006(2) 0.001(3) C8 0.041(3) 0.044(3) 0.047(3) -0.004(3) 0.009(2) 0.002(3) C9 0.050(3) 0.039(3) 0.034(3) -0.004(2) 0.013(2) -0.004(3) C10 0.048(3) 0.052(3) 0.031(3) -0.002(2) 0.007(2) -0.002(3) C11 0.067(4) 0.045(3) 0.044(3) 0.005(3) 0.008(3) 0.008(3) C12 0.077(4) 0.048(3) 0.053(3) 0.001(3) 0.008(3) -0.013(3) C13 0.056(4) 0.051(4) 0.054(3) 0.000(3) 0.008(3) -0.007(3) C14 0.086(4) 0.070(4) 0.066(4) -0.025(3) 0.039(3) -0.006(3) C15 0.359(14) 0.072(5) 0.129(7) -0.045(5) 0.159(9) -0.051(7) C16 0.181(8) 0.064(5) 0.093(5) -0.025(4) 0.024(5) -0.008(5) C17 0.051(3) 0.052(3) 0.040(3) -0.004(3) 0.000(2) 0.004(3) C18 0.041(3) 0.054(3) 0.034(3) -0.008(3) -0.002(2) -0.005(3) C19 0.059(4) 0.051(4) 0.055(4) -0.012(3) 0.007(3) 0.001(3) C20 0.069(4) 0.049(3) 0.057(4) -0.007(3) 0.000(3) -0.010(3) C21 0.056(3) 0.055(4) 0.050(3) 0.004(3) 0.000(3) -0.009(3) C22 0.036(3) 0.050(3) 0.046(3) -0.004(3) -0.003(2) 0.004(2) C23 0.037(3) 0.046(3) 0.038(3) 0.000(3) -0.005(2) -0.004(3) C24 0.049(3) 0.055(3) 0.046(3) 0.000(3) 0.006(2) 0.010(3) C25 0.046(3) 0.048(3) 0.032(3) -0.003(2) 0.006(2) 0.005(3) C26 0.055(3) 0.047(3) 0.042(3) -0.001(3) 0.008(3) 0.012(3) C27 0.061(4) 0.033(3) 0.049(3) -0.006(3) 0.009(3) 0.001(3) C28 0.050(3) 0.042(3) 0.037(3) -0.009(2) 0.003(2) -0.001(3) C29 0.044(3) 0.040(3) 0.026(3) -0.004(2) 0.003(2) 0.004(2) C30 0.052(3) 0.044(3) 0.036(3) 0.002(2) -0.004(2) -0.001(3) C31 0.055(3) 0.036(3) 0.034(3) -0.001(2) 0.014(2) -0.002(3) C32 0.078(4) 0.063(4) 0.064(4) 0.009(3) 0.010(3) -0.017(3) C33 0.117(6) 0.109(6) 0.067(4) 0.019(4) 0.020(4) -0.050(5) C34 0.162(8) 0.114(6) 0.124(7) 0.017(5) 0.035(6) -0.054(6) C35 0.094(5) 0.063(4) 0.066(4) -0.003(3) -0.030(3) 0.029(4) C36 0.111(5) 0.115(6) 0.041(4) 0.004(4) 0.001(4) 0.077(4) C37 0.113(6) 0.051(4) 0.072(4) -0.005(3) -0.011(4) 0.030(5) C38 0.089(6) 0.100(6) 0.116(6) -0.011(5) -0.055(5) 0.032(5) C39 0.095(6) 0.111(6) 0.071(5) 0.009(5) 0.003(4) 0.043(5) C40 0.122(7) 0.080(5) 0.099(6) -0.025(4) 0.026(5) 0.021(5) C41 0.106(6) 0.071(5) 0.161(7) -0.030(5) 0.062(5) -0.008(5) C42 0.097(6) 0.067(5) 0.105(6) 0.011(4) 0.045(5) 0.027(5) C43 0.034(4) 0.099(6) 0.246(10) -0.074(6) -0.066(5) 0.035(4) C44 0.080(5) 0.077(5) 0.103(5) 0.005(4) -0.027(4) -0.010(4) C45 0.061(4) 0.081(4) 0.067(4) 0.007(3) 0.010(3) 0.014(3) C46 0.053(3) 0.060(4) 0.070(4) 0.003(3) 0.006(3) 0.000(3) C47 0.033(3) 0.052(3) 0.049(3) -0.009(3) -0.001(2) -0.009(3) C48 0.054(3) 0.044(3) 0.064(4) -0.008(3) 0.011(3) -0.011(3) C49 0.054(4) 0.064(4) 0.059(4) -0.023(3) 0.004(3) -0.017(3) C50 0.053(4) 0.084(4) 0.050(3) -0.015(3) -0.009(3) -0.012(3) C51 0.064(4) 0.060(4) 0.055(4) -0.001(3) -0.008(3) -0.009(3) C52 0.038(3) 0.047(3) 0.051(3) -0.010(3) 0.007(2) -0.012(3) C53 0.042(3) 0.049(3) 0.077(4) -0.013(3) 0.012(3) -0.008(3) C54 0.043(3) 0.047(3) 0.073(4) -0.009(3) -0.016(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.395(5) . ? O1 C54 1.430(5) . ? O2 C9 1.389(5) . ? O2 C14 1.431(5) . ? O3 C31 1.383(5) . ? O3 C32 1.420(5) . ? O4 C23 1.390(5) . ? O4 C35 1.428(5) . ? O5 C36 1.258(6) . ? O5 C37 1.378(7) . ? O6 C43 1.221(6) . ? O6 C42 1.321(7) . ? O7 C45 1.398(5) . ? O7 C44 1.429(6) . ? O8 C47 1.373(5) . ? O8 C46 1.413(5) . ? O9 C52 1.394(5) . ? O9 C53 1.420(5) . ? C1 C2 1.389(6) . ? C1 C6 1.390(6) . ? C2 C3 1.386(6) . ? C2 C30 1.514(6) . ? C3 C4 1.373(6) . ? C4 C5 1.378(6) . ? C5 C6 1.388(6) . ? C6 C7 1.516(6) . ? C7 C8 1.509(6) . ? C8 C13 1.382(6) . ? C8 C9 1.391(6) . ? C9 C10 1.399(6) . ? C10 C11 1.383(6) . ? C10 C17 1.520(6) . ? C11 C12 1.373(6) . ? C12 C13 1.373(6) . ? C14 C15 1.431(7) . ? C15 C16 1.409(8) . ? C17 C18 1.514(6) . ? C18 C19 1.381(6) . ? C18 C23 1.400(6) . ? C19 C20 1.383(6) . ? C20 C21 1.380(6) . ? C21 C22 1.394(6) . ? C22 C23 1.378(6) . ? C22 C24 1.522(6) . ? C24 C25 1.528(6) . ? C25 C26 1.371(6) . ? C25 C31 1.396(6) . ? C26 C27 1.392(6) . ? C27 C28 1.388(6) . ? C28 C29 1.380(6) . ? C29 C31 1.385(6) . ? C29 C30 1.519(6) . ? C32 C33 1.511(7) . ? C33 C34 1.452(7) . ? C35 C36 1.444(7) . ? C37 C38 1.368(8) . ? C37 C42 1.377(8) . ? C38 C39 1.352(8) . ? C39 C40 1.342(8) . ? C40 C41 1.356(8) . ? C41 C42 1.370(8) . ? C43 C44 1.543(8) . ? C45 C46 1.502(6) . ? C47 C52 1.381(6) . ? C47 C48 1.388(6) . ? C48 C49 1.374(6) . ? C49 C50 1.361(6) . ? C50 C51 1.389(6) . ? C51 C52 1.374(6) . ? C53 C54 1.493(6) . ? 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 C1 O1 C54 111.3(3) . . ? C9 O2 C14 112.9(4) . . ? C31 O3 C32 114.2(4) . . ? C23 O4 C35 114.3(4) . . ? C36 O5 C37 124.2(6) . . ? C43 O6 C42 123.4(7) . . ? C45 O7 C44 114.6(4) . . ? C47 O8 C46 118.2(4) . . ? C52 O9 C53 112.5(4) . . ? C2 C1 C6 122.8(4) . . ? C2 C1 O1 118.2(4) . . ? C6 C1 O1 118.9(4) . . ? C3 C2 C1 117.8(5) . . ? C3 C2 C30 121.1(5) . . ? C1 C2 C30 120.9(4) . . ? C4 C3 C2 120.5(5) . . ? C3 C4 C5 120.3(5) . . ? C4 C5 C6 121.3(5) . . ? C5 C6 C1 116.8(5) . . ? C5 C6 C7 120.7(5) . . ? C1 C6 C7 122.2(4) . . ? C8 C7 C6 110.7(4) . . ? C13 C8 C9 117.7(4) . . ? C13 C8 C7 121.5(4) . . ? C9 C8 C7 120.7(4) . . ? O2 C9 C8 119.5(4) . . ? O2 C9 C10 118.8(4) . . ? C8 C9 C10 121.7(4) . . ? C11 C10 C9 117.8(4) . . ? C11 C10 C17 122.1(4) . . ? C9 C10 C17 120.0(4) . . ? C12 C11 C10 121.2(5) . . ? C13 C12 C11 119.8(5) . . ? C12 C13 C8 121.5(5) . . ? C15 C14 O2 111.3(5) . . ? C16 C15 C14 124.4(7) . . ? C18 C17 C10 110.7(4) . . ? C19 C18 C23 117.9(5) . . ? C19 C18 C17 120.7(5) . . ? C23 C18 C17 121.1(4) . . ? C18 C19 C20 121.0(5) . . ? C21 C20 C19 119.9(5) . . ? C20 C21 C22 120.5(5) . . ? C23 C22 C21 118.4(5) . . ? C23 C22 C24 120.7(4) . . ? C21 C22 C24 120.6(5) . . ? C22 C23 O4 118.5(4) . . ? C22 C23 C18 122.0(5) . . ? O4 C23 C18 119.6(4) . . ? C22 C24 C25 110.6(4) . . ? C26 C25 C31 118.3(4) . . ? C26 C25 C24 120.8(4) . . ? C31 C25 C24 120.6(4) . . ? C25 C26 C27 121.3(5) . . ? C28 C27 C26 118.8(4) . . ? C29 C28 C27 121.4(4) . . ? C28 C29 C31 118.2(4) . . ? C28 C29 C30 120.4(4) . . ? C31 C29 C30 121.1(4) . . ? C2 C30 C29 110.4(3) . . ? O3 C31 C29 119.7(4) . . ? O3 C31 C25 118.5(4) . . ? C29 C31 C25 121.8(4) . . ? O3 C32 C33 108.9(5) . . ? C34 C33 C32 115.2(6) . . ? O4 C35 C36 111.6(4) . . ? O5 C36 C35 119.9(6) . . ? C38 C37 C42 119.5(6) . . ? C38 C37 O5 119.9(8) . . ? C42 C37 O5 120.1(7) . . ? C39 C38 C37 119.8(7) . . ? C40 C39 C38 121.4(7) . . ? C39 C40 C41 119.4(7) . . ? C40 C41 C42 120.9(7) . . ? O6 C42 C41 123.7(8) . . ? O6 C42 C37 117.3(7) . . ? C41 C42 C37 118.9(7) . . ? O6 C43 C44 113.9(6) . . ? O7 C44 C43 104.8(5) . . ? O7 C45 C46 108.6(4) . . ? O8 C46 C45 108.2(4) . . ? O8 C47 C52 116.1(4) . . ? O8 C47 C48 124.7(5) . . ? C52 C47 C48 119.2(4) . . ? C49 C48 C47 120.0(5) . . ? C50 C49 C48 120.6(5) . . ? C49 C50 C51 120.1(5) . . ? C52 C51 C50 119.5(5) . . ? C51 C52 C47 120.6(4) . . ? C51 C52 O9 118.5(5) . . ? C47 C52 O9 120.9(4) . . ? O9 C53 C54 110.1(4) . . ? O1 C54 C53 108.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C54 O1 C1 C2 -96.8(4) . . . . ? C54 O1 C1 C6 86.7(5) . . . . ? C6 C1 C2 C3 -7.0(6) . . . . ? O1 C1 C2 C3 176.6(4) . . . . ? C6 C1 C2 C30 168.6(4) . . . . ? O1 C1 C2 C30 -7.8(6) . . . . ? C1 C2 C3 C4 1.3(6) . . . . ? C30 C2 C3 C4 -174.3(4) . . . . ? C2 C3 C4 C5 3.6(7) . . . . ? C3 C4 C5 C6 -3.2(8) . . . . ? C4 C5 C6 C1 -2.2(7) . . . . ? C4 C5 C6 C7 172.0(4) . . . . ? C2 C1 C6 C5 7.4(6) . . . . ? O1 C1 C6 C5 -176.2(4) . . . . ? C2 C1 C6 C7 -166.7(4) . . . . ? O1 C1 C6 C7 9.7(6) . . . . ? C5 C6 C7 C8 -106.4(5) . . . . ? C1 C6 C7 C8 67.5(5) . . . . ? C6 C7 C8 C13 -105.5(5) . . . . ? C6 C7 C8 C9 70.4(5) . . . . ? C14 O2 C9 C8 92.3(5) . . . . ? C14 O2 C9 C10 -90.6(5) . . . . ? C13 C8 C9 O2 -176.8(4) . . . . ? C7 C8 C9 O2 7.2(7) . . . . ? C13 C8 C9 C10 6.2(7) . . . . ? C7 C8 C9 C10 -169.8(4) . . . . ? O2 C9 C10 C11 177.0(4) . . . . ? C8 C9 C10 C11 -5.9(7) . . . . ? O2 C9 C10 C17 -6.3(6) . . . . ? C8 C9 C10 C17 170.7(4) . . . . ? C9 C10 C11 C12 1.3(7) . . . . ? C17 C10 C11 C12 -175.3(4) . . . . ? C10 C11 C12 C13 2.9(8) . . . . ? C11 C12 C13 C8 -2.7(8) . . . . ? C9 C8 C13 C12 -1.8(8) . . . . ? C7 C8 C13 C12 174.2(4) . . . . ? C9 O2 C14 C15 170.5(6) . . . . ? O2 C14 C15 C16 37.8(12) . . . . ? C11 C10 C17 C18 106.2(5) . . . . ? C9 C10 C17 C18 -70.3(6) . . . . ? C10 C17 C18 C19 104.9(5) . . . . ? C10 C17 C18 C23 -68.1(6) . . . . ? C23 C18 C19 C20 -0.2(7) . . . . ? C17 C18 C19 C20 -173.4(4) . . . . ? C18 C19 C20 C21 5.2(8) . . . . ? C19 C20 C21 C22 -4.8(8) . . . . ? C20 C21 C22 C23 -0.6(7) . . . . ? C20 C21 C22 C24 173.3(4) . . . . ? C21 C22 C23 O4 -175.1(4) . . . . ? C24 C22 C23 O4 11.0(6) . . . . ? C21 C22 C23 C18 5.7(7) . . . . ? C24 C22 C23 C18 -168.1(4) . . . . ? C35 O4 C23 C22 97.9(5) . . . . ? C35 O4 C23 C18 -82.9(5) . . . . ? C19 C18 C23 C22 -5.4(7) . . . . ? C17 C18 C23 C22 167.9(4) . . . . ? C19 C18 C23 O4 175.5(4) . . . . ? C17 C18 C23 O4 -11.3(6) . . . . ? C23 C22 C24 C25 68.3(5) . . . . ? C21 C22 C24 C25 -105.4(5) . . . . ? C22 C24 C25 C26 -103.0(5) . . . . ? C22 C24 C25 C31 70.8(5) . . . . ? C31 C25 C26 C27 -0.6(7) . . . . ? C24 C25 C26 C27 173.3(4) . . . . ? C25 C26 C27 C28 -3.1(7) . . . . ? C26 C27 C28 C29 3.0(7) . . . . ? C27 C28 C29 C31 0.8(7) . . . . ? C27 C28 C29 C30 -172.7(4) . . . . ? C3 C2 C30 C29 105.3(5) . . . . ? C1 C2 C30 C29 -70.2(5) . . . . ? C28 C29 C30 C2 103.9(5) . . . . ? C31 C29 C30 C2 -69.5(5) . . . . ? C32 O3 C31 C29 -92.0(5) . . . . ? C32 O3 C31 C25 91.5(5) . . . . ? C28 C29 C31 O3 178.9(4) . . . . ? C30 C29 C31 O3 -7.6(6) . . . . ? C28 C29 C31 C25 -4.7(7) . . . . ? C30 C29 C31 C25 168.8(4) . . . . ? C26 C25 C31 O3 -179.0(4) . . . . ? C24 C25 C31 O3 7.1(6) . . . . ? C26 C25 C31 C29 4.6(7) . . . . ? C24 C25 C31 C29 -169.4(4) . . . . ? C31 O3 C32 C33 -173.3(4) . . . . ? O3 C32 C33 C34 -175.5(5) . . . . ? C23 O4 C35 C36 -153.9(5) . . . . ? C37 O5 C36 C35 178.5(7) . . . . ? O4 C35 C36 O5 52.5(9) . . . . ? C36 O5 C37 C38 -105.8(9) . . . . ? C36 O5 C37 C42 82.5(9) . . . . ? C42 C37 C38 C39 -1.2(10) . . . . ? O5 C37 C38 C39 -172.9(6) . . . . ? C37 C38 C39 C40 0.7(11) . . . . ? C38 C39 C40 C41 -0.1(11) . . . . ? C39 C40 C41 C42 0.1(12) . . . . ? C43 O6 C42 C41 -23.2(12) . . . . ? C43 O6 C42 C37 158.6(8) . . . . ? C40 C41 C42 O6 -178.7(7) . . . . ? C40 C41 C42 C37 -0.6(11) . . . . ? C38 C37 C42 O6 179.3(6) . . . . ? O5 C37 C42 O6 -8.9(10) . . . . ? C38 C37 C42 C41 1.1(10) . . . . ? O5 C37 C42 C41 172.9(6) . . . . ? C42 O6 C43 C44 -176.9(6) . . . . ? C45 O7 C44 C43 172.9(5) . . . . ? O6 C43 C44 O7 154.7(7) . . . . ? C44 O7 C45 C46 179.6(4) . . . . ? C47 O8 C46 C45 -176.1(4) . . . . ? O7 C45 C46 O8 -88.4(5) . . . . ? C46 O8 C47 C52 165.9(4) . . . . ? C46 O8 C47 C48 -13.2(7) . . . . ? O8 C47 C48 C49 -179.0(4) . . . . ? C52 C47 C48 C49 2.0(7) . . . . ? C47 C48 C49 C50 -0.7(8) . . . . ? C48 C49 C50 C51 -0.3(8) . . . . ? C49 C50 C51 C52 0.0(8) . . . . ? C50 C51 C52 C47 1.3(8) . . . . ? C50 C51 C52 O9 179.1(4) . . . . ? O8 C47 C52 C51 178.6(4) . . . . ? C48 C47 C52 C51 -2.3(7) . . . . ? O8 C47 C52 O9 0.9(7) . . . . ? C48 C47 C52 O9 -180.0(4) . . . . ? C53 O9 C52 C51 105.8(5) . . . . ? C53 O9 C52 C47 -76.4(5) . . . . ? C52 O9 C53 C54 -166.1(4) . . . . ? C1 O1 C54 C53 171.5(4) . . . . ? O9 C53 C54 O1 -77.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.750 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.059 data_comp5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H74 O9' _chemical_formula_weight 963.21 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.110(4) _cell_length_b 18.355(3) _cell_length_c 11.861(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.92(4) _cell_angle_gamma 90.00 _cell_volume 2827(3) _cell_formula_units_Z 2 _cell_measurement_temperature 288(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 8.32 _cell_measurement_theta_max 12.72 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.187 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 288(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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega/2theta scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 300 _diffrn_standards_decay_% 1.032 _diffrn_reflns_number 4568 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1759 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 23.98 _reflns_number_total 4568 _reflns_number_gt 993 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction CAD4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEPII _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 5(5) _refine_ls_number_reflns 4568 _refine_ls_number_parameters 425 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.2116 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1554 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.874 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.2842(9) 0.0823(6) 0.4989(9) 0.088(4) Uani 1 d . . . O2 O 0.1847(5) -0.0379(8) 0.2173(6) 0.086(2) Uani 1 d . . . O3 O 0.0331(5) -0.0398(7) 0.5106(5) 0.067(2) Uiso 1 d . . . O4 O 0.2814(6) -0.1647(5) 0.4913(8) 0.060(3) Uani 1 d . . . O5 O 0.4510(9) -0.2691(5) 0.7030(10) 0.083(3) Uani 1 d . . . O6 O 0.4515(9) -0.1949(6) 0.9003(8) 0.089(4) Uani 1 d D . . O7 O 0.4790(6) -0.0353(8) 0.9757(5) 0.088(3) Uani 1 d . . . O8 O 0.4384(8) 0.1192(6) 0.8928(8) 0.078(3) Uani 1 d . . . O9 O 0.4393(8) 0.1964(6) 0.7011(9) 0.078(3) Uiso 1 d D . . C1 C 0.1761(14) 0.1013(9) 0.4320(15) 0.092(6) Uani 1 d . . . C2 C 0.0985(12) 0.1085(8) 0.4922(14) 0.066(4) Uiso 1 d . . . C3 C 0.0204(13) 0.1364(7) 0.4003(16) 0.080(5) Uani 1 d . . . H3 H -0.0410 0.1503 0.4251 0.096 Uiso 1 calc R . . C4 C 0.0212(16) 0.1456(10) 0.2856(17) 0.102(6) Uani 1 d . . . H4 H -0.0381 0.1589 0.2378 0.122 Uiso 1 calc R . . C5 C 0.1115(14) 0.1346(10) 0.2446(14) 0.089(6) Uani 1 d . . . H5 H 0.1162 0.1408 0.1676 0.107 Uiso 1 calc R . . C6 C 0.1941(12) 0.1146(9) 0.3178(15) 0.074(5) Uiso 1 d . . . C7 C 0.2846(12) 0.1064(8) 0.2554(14) 0.081(5) Uiso 1 d . . . H7A H 0.2625 0.1148 0.1750 0.097 Uiso 1 calc R . . H7B H 0.3349 0.1435 0.2819 0.097 Uiso 1 calc R . . C8 C 0.3341(10) 0.0347(7) 0.2694(10) 0.044(3) Uiso 1 d . . . C9 C 0.4378(11) 0.0438(8) 0.3018(11) 0.072(4) Uiso 1 d . . . H9 H 0.4702 0.0889 0.3076 0.086 Uiso 1 calc R . . C10 C 0.4884(8) -0.0209(7) 0.3245(8) 0.055(3) Uiso 1 d . . . H10 H 0.5580 -0.0157 0.3519 0.066 Uiso 1 calc R . . C11 C 0.4555(11) -0.0923(8) 0.3142(11) 0.069(4) Uiso 1 d . . . H11 H 0.4993 -0.1319 0.3304 0.082 Uiso 1 calc R . . C12 C 0.3478(15) -0.0996(10) 0.2764(16) 0.111(6) Uiso 1 d . . . C13 C 0.2926(8) -0.0392(10) 0.2540(8) 0.059(3) Uiso 1 d . . . C14 C 0.1573(8) -0.0485(13) 0.0992(10) 0.095(5) Uani 1 d . . . H14A H 0.1849 -0.0941 0.0751 0.114 Uiso 1 calc R . . H14B H 0.1823 -0.0089 0.0564 0.114 Uiso 1 calc R . . C15 C 0.0391(11) -0.0501(10) 0.0834(9) 0.116(7) Uani 1 d D . . H15A H 0.0141 -0.0999 0.0774 0.139 Uiso 1 calc R . . H15B H 0.0132 -0.0268 0.1472 0.139 Uiso 1 calc R . . C16 C 0.0077(11) -0.0122(9) -0.0167(11) 0.144(8) Uani 1 d D . . H16A H -0.0662 -0.0102 -0.0300 0.217 Uiso 1 calc R . . H16B H 0.0326 -0.0366 -0.0791 0.217 Uiso 1 calc R . . H16C H 0.0349 0.0364 -0.0102 0.217 Uiso 1 calc R . . C17 C 0.2853(11) -0.1692(8) 0.2613(13) 0.073(5) Uiso 1 d . . . H17A H 0.2699 -0.1761 0.1796 0.087 Uiso 1 calc R . . H17B H 0.3329 -0.2078 0.2887 0.087 Uiso 1 calc R . . C18 C 0.1916(11) -0.1861(8) 0.3052(12) 0.060(4) Uiso 1 d . . . C19 C 0.0937(12) -0.2137(8) 0.2471(13) 0.072(5) Uiso 1 d . . . H19 H 0.0862 -0.2233 0.1694 0.086 Uiso 1 calc R . . C20 C 0.0143(12) -0.2251(8) 0.3058(13) 0.066(4) Uiso 1 d . . . H20 H -0.0453 -0.2445 0.2651 0.079 Uiso 1 calc R . . C21 C 0.0114(12) -0.2115(7) 0.4177(12) 0.065(4) Uiso 1 d . . . H21 H -0.0476 -0.2164 0.4526 0.078 Uiso 1 calc R . . C22 C 0.1072(11) -0.1891(8) 0.4751(12) 0.059(4) Uiso 1 d . . . C23 C 0.1959(8) -0.1789(6) 0.4280(9) 0.029(3) Uiso 1 d . . . C24 C 0.1007(15) -0.1784(10) 0.6021(16) 0.118(7) Uiso 1 d . . . H24A H 0.0288 -0.1819 0.6129 0.142 Uiso 1 calc R . . H24B H 0.1367 -0.2186 0.6433 0.142 Uiso 1 calc R . . C25 C 0.1421(11) -0.1100(8) 0.6546(12) 0.053(4) Uiso 1 d . . . C26 C 0.2124(11) -0.1075(8) 0.7508(12) 0.057(4) Uiso 1 d D . . H26 H 0.2392 -0.1506 0.7840 0.068 Uiso 1 calc R . . C27 C 0.2435(8) -0.0424(11) 0.7986(8) 0.077(4) Uani 1 d D . . H27 H 0.2941 -0.0406 0.8618 0.092 Uiso 1 calc R . . C28 C 0.1978(15) 0.0222(11) 0.7510(16) 0.110(6) Uani 1 d . . . H28 H 0.2146 0.0660 0.7886 0.132 Uiso 1 calc R . . C29 C 0.1289(12) 0.0237(9) 0.6507(14) 0.073(5) Uiso 1 d . . . C30 C 0.1002(8) -0.0416(12) 0.6125(9) 0.074(3) Uiso 1 d . . . C31 C -0.0689(8) -0.0440(14) 0.5213(9) 0.098(4) Uani 1 d . . . H31A H -0.0924 0.0000 0.5550 0.118 Uiso 1 calc R . . H31B H -0.0829 -0.0856 0.5672 0.118 Uiso 1 calc R . . C32 C -0.1213(10) -0.0532(12) 0.3930(12) 0.124(6) Uiso 1 d D . . H32A H -0.0775 -0.0331 0.3412 0.149 Uiso 1 calc R . . H32B H -0.1334 -0.1043 0.3749 0.149 Uiso 1 calc R . . C33 C -0.2090(10) -0.0175(9) 0.3847(12) 0.143(7) Uani 1 d D . . H33A H -0.2425 -0.0193 0.3075 0.214 Uiso 1 calc R . . H33B H -0.1960 0.0323 0.4068 0.214 Uiso 1 calc R . . H33C H -0.2527 -0.0394 0.4339 0.214 Uiso 1 calc R . . C34 C 0.0988(12) 0.0951(6) 0.6083(11) 0.057(4) Uani 1 d . . . H34A H 0.0300 0.1046 0.6261 0.069 Uiso 1 calc R . . H34B H 0.1444 0.1303 0.6503 0.069 Uiso 1 calc R . . C35 C 0.3335(12) -0.2257(8) 0.5398(13) 0.073(5) Uiso 1 d . . . H35A H 0.3632 -0.2520 0.4813 0.087 Uiso 1 calc R . . H35B H 0.2849 -0.2577 0.5696 0.087 Uiso 1 calc R . . C36 C 0.4199(12) -0.2051(9) 0.6368(14) 0.078(5) Uiso 1 d . . . H36 H 0.3980 -0.1661 0.6844 0.094 Uiso 1 calc R . . C37 C 0.5156(11) -0.1877(9) 0.5974(12) 0.083(5) Uiso 1 d . . . H37A H 0.5053 -0.1462 0.5465 0.099 Uiso 1 calc R . . H37B H 0.5366 -0.2287 0.5543 0.099 Uiso 1 calc R . . C38 C 0.6002(11) -0.1704(10) 0.6922(12) 0.094(5) Uani 1 d . . . H38A H 0.6056 -0.2095 0.7477 0.113 Uiso 1 calc R . . H38B H 0.5831 -0.1261 0.7299 0.113 Uiso 1 calc R . . C39 C 0.7042(12) -0.1606(9) 0.6487(11) 0.091(5) Uani 1 d . . . H39A H 0.7167 -0.2022 0.6020 0.109 Uiso 1 calc R . . H39B H 0.7015 -0.1174 0.6013 0.109 Uiso 1 calc R . . C40 C 0.7887(13) -0.1536(11) 0.7407(18) 0.119(7) Uani 1 d . . . H40A H 0.8517 -0.1462 0.7097 0.179 Uiso 1 calc R . . H40B H 0.7938 -0.1973 0.7857 0.179 Uiso 1 calc R . . H40C H 0.7764 -0.1128 0.7876 0.179 Uiso 1 calc R . . C41 C 0.3891(11) -0.2824(8) 0.7805(13) 0.066(4) Uiso 1 d . . . C42 C 0.3353(12) -0.3442(9) 0.7415(14) 0.099(6) Uiso 1 d . . . H42 H 0.3436 -0.3633 0.6707 0.119 Uiso 1 calc R . . C43 C 0.2709(10) -0.3772(8) 0.8047(11) 0.063(4) Uiso 1 d . . . H43 H 0.2326 -0.4175 0.7764 0.075 Uiso 1 calc R . . C44 C 0.2626(12) -0.3509(9) 0.9107(13) 0.080(5) Uiso 1 d . . . H44 H 0.2224 -0.3743 0.9584 0.097 Uiso 1 calc R . . C45 C 0.3184(13) -0.2855(8) 0.9458(15) 0.068(5) Uiso 1 d . . . H45 H 0.3088 -0.2654 1.0155 0.081 Uiso 1 calc R . . C46 C 0.3834(12) -0.2511(9) 0.8852(15) 0.078(5) Uiso 1 d D . . C47 C 0.4726(10) -0.1553(7) 1.0068(12) 0.071(4) Uiso 1 d . . . H47A H 0.4075 -0.1383 1.0272 0.086 Uiso 1 calc R . . H47B H 0.5014 -0.1892 1.0653 0.086 Uiso 1 calc R . . C48 C 0.5406(10) -0.0940(7) 1.0091(12) 0.077(5) Uani 1 d . . . H48A H 0.5768 -0.0866 1.0852 0.093 Uiso 1 calc R . . H48B H 0.5908 -0.1015 0.9573 0.093 Uiso 1 calc R . . C49 C 0.5120(11) 0.0369(8) 1.0164(13) 0.072(5) Uiso 1 d . . . H49A H 0.5378 0.0325 1.0968 0.087 Uiso 1 calc R . . H49B H 0.5699 0.0506 0.9782 0.087 Uiso 1 calc R . . C50 C 0.4417(9) 0.0953(6) 1.0044(11) 0.058(4) Uiso 1 d . . . H50A H 0.3741 0.0793 1.0186 0.070 Uiso 1 calc R . . H50B H 0.4648 0.1341 1.0574 0.070 Uiso 1 calc R . . C51 C 0.3833(15) 0.1825(11) 0.8690(18) 0.097(6) Uiso 1 d . . . C52 C 0.3289(16) 0.1991(10) 0.9557(19) 0.106(7) Uani 1 d . . . H52 H 0.3394 0.1716 1.0221 0.127 Uiso 1 calc R . . C53 C 0.2580(11) 0.2562(9) 0.9477(9) 0.076(5) Uani 1 d D . . H53 H 0.2167 0.2643 1.0043 0.091 Uiso 1 calc R . . C54 C 0.2515(11) 0.3008(9) 0.8515(10) 0.098(6) Uani 1 d D . . H54 H 0.2123 0.3432 0.8455 0.118 Uiso 1 calc R . . C55 C 0.3048(11) 0.2794(8) 0.7672(12) 0.070(4) Uiso 1 d . . . H55 H 0.2919 0.3056 0.6997 0.084 Uiso 1 calc R . . C56 C 0.3723(12) 0.2264(8) 0.7684(13) 0.075(5) Uiso 1 d D . . C57 C 0.4162(11) 0.1342(8) 0.6390(12) 0.057(4) Uiso 1 d . . . H57 H 0.3846 0.1028 0.6913 0.068 Uiso 1 calc R . . C58 C 0.5008(13) 0.0882(9) 0.6058(14) 0.099(6) Uiso 1 d . . . H58A H 0.4659 0.0482 0.5633 0.119 Uiso 1 calc R . . H58B H 0.5306 0.1173 0.5504 0.119 Uiso 1 calc R . . C59 C 0.5880(17) 0.0550(12) 0.6741(19) 0.178(11) Uiso 1 d . . . H59A H 0.5666 0.0398 0.7456 0.214 Uiso 1 calc R . . H59B H 0.6060 0.0113 0.6353 0.214 Uiso 1 calc R . . C60 C 0.6723(15) 0.0952(11) 0.6976(17) 0.125(7) Uiso 1 d . . . H60A H 0.6535 0.1366 0.7412 0.150 Uiso 1 calc R . . H60B H 0.6873 0.1144 0.6255 0.150 Uiso 1 calc R . . C61 C 0.7674(17) 0.0685(15) 0.756(2) 0.207(14) Uani 1 d . . . H61A H 0.8199 0.1049 0.7545 0.311 Uiso 1 calc R . . H61B H 0.7869 0.0251 0.7186 0.311 Uiso 1 calc R . . H61C H 0.7595 0.0574 0.8331 0.311 Uiso 1 calc R . . C62 C 0.3357(13) 0.1444(9) 0.5468(14) 0.085(5) Uani 1 d . . . H7A H 0.2848 0.1764 0.5726 0.103 Uiso 1 calc R . . H7B H 0.3644 0.1697 0.4867 0.103 Uiso 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 0.107(10) 0.097(9) 0.060(7) -0.010(7) 0.015(7) -0.026(8) O2 0.068(5) 0.116(7) 0.072(5) 0.024(9) 0.004(4) 0.001(9) O4 0.045(5) 0.066(7) 0.062(6) -0.026(5) -0.024(5) -0.008(5) O5 0.106(8) 0.068(7) 0.072(6) 0.005(5) -0.006(6) 0.035(6) O6 0.122(10) 0.101(9) 0.049(6) -0.011(6) 0.031(6) 0.019(8) O7 0.105(7) 0.093(7) 0.062(5) 0.009(8) -0.010(5) 0.052(9) O8 0.085(7) 0.110(9) 0.032(5) -0.003(6) -0.021(5) -0.042(7) C1 0.110(14) 0.076(11) 0.096(12) 0.016(10) 0.041(11) -0.018(10) C3 0.095(12) 0.028(8) 0.122(14) -0.004(9) 0.034(11) 0.010(8) C4 0.116(16) 0.080(12) 0.103(15) 0.003(12) -0.013(13) -0.003(12) C5 0.101(13) 0.107(13) 0.049(9) 0.027(9) -0.026(9) -0.009(12) C14 0.053(8) 0.125(14) 0.102(11) -0.011(14) -0.013(8) 0.015(12) C15 0.150(15) 0.126(16) 0.062(9) -0.079(11) -0.018(9) 0.075(14) C16 0.131(13) 0.14(2) 0.152(15) 0.054(15) -0.002(12) 0.015(13) C27 0.068(9) 0.119(12) 0.038(7) -0.021(12) -0.013(6) -0.022(13) C28 0.118(15) 0.108(15) 0.108(14) -0.016(13) 0.027(12) -0.009(13) C31 0.084(10) 0.106(11) 0.100(10) 0.013(15) -0.003(8) 0.008(14) C33 0.119(13) 0.113(19) 0.196(16) 0.060(14) 0.022(12) 0.008(13) C34 0.096(10) 0.025(7) 0.058(8) -0.020(6) 0.035(7) 0.015(7) C38 0.074(11) 0.134(15) 0.074(10) -0.018(11) 0.009(9) 0.015(12) C39 0.097(13) 0.124(14) 0.057(9) -0.010(10) 0.032(9) -0.018(11) C40 0.070(12) 0.125(17) 0.153(19) 0.051(15) -0.021(12) -0.022(12) C48 0.065(10) 0.082(12) 0.071(10) 0.008(9) -0.039(8) -0.013(9) C52 0.099(14) 0.101(14) 0.129(16) -0.031(12) 0.052(12) -0.014(11) C53 0.089(11) 0.130(15) 0.019(7) -0.023(9) 0.040(7) -0.043(11) C54 0.083(11) 0.175(18) 0.042(9) -0.052(11) 0.023(8) -0.033(11) C61 0.114(19) 0.33(4) 0.19(3) -0.07(3) 0.056(18) 0.06(2) C62 0.096(12) 0.097(12) 0.059(9) 0.031(9) -0.003(8) -0.044(10) _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 C62 1.403(18) . ? O1 C1 1.564(19) . ? O2 C14 1.411(11) . ? O2 C13 1.422(10) . ? O3 C31 1.362(10) . ? O3 C30 1.394(10) . ? O4 C23 1.286(13) . ? O4 C35 1.393(17) . ? O5 C41 1.329(15) . ? O5 C36 1.440(17) . ? O6 C46 1.361(14) . ? O6 C47 1.451(15) . ? O7 C48 1.372(15) . ? O7 C49 1.455(18) . ? O8 C51 1.377(19) . ? O8 C50 1.390(14) . ? O9 C57 1.370(16) . ? O9 C56 1.380(13) . ? C1 C2 1.328(19) . ? C1 C6 1.43(2) . ? C2 C34 1.399(18) . ? C2 C3 1.48(2) . ? C3 C4 1.37(2) . ? C3 H3 0.9300 . ? C4 C5 1.36(2) . ? C4 H4 0.9300 . ? C5 C6 1.34(2) . ? C5 H5 0.9300 . ? C6 C7 1.49(2) . ? C7 C8 1.467(18) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.371(17) . ? C8 C13 1.46(2) . ? C9 C10 1.368(16) . ? C9 H9 0.9300 . ? C10 C11 1.381(16) . ? C10 H10 0.9300 . ? C11 C12 1.43(2) . ? C11 H11 0.9300 . ? C12 C13 1.33(2) . ? C12 C17 1.51(2) . ? C14 C15 1.536(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.388(14) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.433(18) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.456(17) . ? C18 C19 1.461(19) . ? C19 C20 1.347(19) . ? C19 H19 0.9300 . ? C20 C21 1.356(18) . ? C20 H20 0.9300 . ? C21 C22 1.405(19) . ? C21 H21 0.9300 . ? C22 C23 1.370(16) . ? C22 C24 1.53(2) . ? C24 C25 1.47(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.365(19) . ? C25 C30 1.43(2) . ? C26 C27 1.360(15) . ? C26 H26 0.9300 . ? C27 C28 1.41(2) . ? C27 H27 0.9300 . ? C28 C29 1.39(2) . ? C28 H28 0.9300 . ? C29 C30 1.32(2) . ? C29 C34 1.439(19) . ? C31 C32 1.590(15) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.316(14) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.55(2) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.433(19) . ? C36 H36 0.9800 . ? C37 C38 1.500(18) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.533(17) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.45(2) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C46 1.38(2) . ? C41 C42 1.38(2) . ? C42 C43 1.347(18) . ? C42 H42 0.9300 . ? C43 C44 1.366(18) . ? C43 H43 0.9300 . ? C44 C45 1.44(2) . ? C44 H44 0.9300 . ? C45 C46 1.34(2) . ? C45 H45 0.9300 . ? C47 C48 1.433(16) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.409(16) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.36(2) . ? C51 C56 1.43(2) . ? C52 C53 1.40(2) . ? C52 H52 0.9300 . ? C53 C54 1.398(14) . ? C53 H53 0.9300 . ? C54 C55 1.354(16) . ? C54 H54 0.9300 . ? C55 C56 1.314(18) . ? C55 H55 0.9300 . ? C57 C62 1.42(2) . ? C57 C58 1.488(19) . ? C57 H57 0.9800 . ? C58 C59 1.44(2) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.33(2) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.43(3) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H7A 0.9700 . ? C62 H7B 0.9700 . ? 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 C62 O1 C1 112.1(12) . . ? C14 O2 C13 114.1(8) . . ? C31 O3 C30 115.3(8) . . ? C23 O4 C35 114.7(11) . . ? C41 O5 C36 111.9(12) . . ? C46 O6 C47 122.5(12) . . ? C48 O7 C49 118.9(9) . . ? C51 O8 C50 114.1(13) . . ? C57 O9 C56 122.2(12) . . ? C2 C1 C6 137.1(18) . . ? C2 C1 O1 117.2(15) . . ? C6 C1 O1 105.3(13) . . ? C1 C2 C34 127.9(16) . . ? C1 C2 C3 98.2(15) . . ? C34 C2 C3 133.9(15) . . ? C4 C3 C2 132.4(17) . . ? C4 C3 H3 113.8 . . ? C2 C3 H3 113.8 . . ? C5 C4 C3 117.6(18) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? C6 C5 C4 118.3(17) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C5 C6 C1 116.0(16) . . ? C5 C6 C7 109.4(16) . . ? C1 C6 C7 134.5(16) . . ? C8 C7 C6 113.9(13) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C13 119.0(12) . . ? C9 C8 C7 109.2(12) . . ? C13 C8 C7 131.8(12) . . ? C10 C9 C8 112.7(12) . . ? C10 C9 H9 123.7 . . ? C8 C9 H9 123.7 . . ? C9 C10 C11 132.0(11) . . ? C9 C10 H10 114.0 . . ? C11 C10 H10 114.0 . . ? C10 C11 C12 113.6(15) . . ? C10 C11 H11 123.2 . . ? C12 C11 H11 123.2 . . ? C13 C12 C11 118.2(17) . . ? C13 C12 C17 114.1(16) . . ? C11 C12 C17 127.7(17) . . ? C12 C13 O2 124.5(16) . . ? C12 C13 C8 124.4(12) . . ? O2 C13 C8 111.1(14) . . ? O2 C14 C15 103.8(9) . . ? O2 C14 H14A 111.0 . . ? C15 C14 H14A 111.0 . . ? O2 C14 H14B 111.0 . . ? C15 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? C16 C15 C14 105.7(15) . . ? C16 C15 H15A 110.6 . . ? C14 C15 H15A 110.6 . . ? C16 C15 H15B 110.6 . . ? C14 C15 H15B 110.6 . . ? H15A C15 H15B 108.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C12 128.1(14) . . ? C18 C17 H17A 105.3 . . ? C12 C17 H17A 105.3 . . ? C18 C17 H17B 105.3 . . ? C12 C17 H17B 105.3 . . ? H17A C17 H17B 106.0 . . ? C17 C18 C23 115.3(13) . . ? C17 C18 C19 130.2(14) . . ? C23 C18 C19 114.4(12) . . ? C20 C19 C18 120.1(14) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 127.2(16) . . ? C19 C20 H20 116.4 . . ? C21 C20 H20 116.4 . . ? C20 C21 C22 112.6(14) . . ? C20 C21 H21 123.7 . . ? C22 C21 H21 123.7 . . ? C23 C22 C21 126.5(13) . . ? C23 C22 C24 123.3(14) . . ? C21 C22 C24 110.2(13) . . ? O4 C23 C22 120.6(11) . . ? O4 C23 C18 120.8(11) . . ? C22 C23 C18 118.5(11) . . ? C25 C24 C22 117.3(14) . . ? C25 C24 H24A 108.0 . . ? C22 C24 H24A 108.0 . . ? C25 C24 H24B 108.0 . . ? C22 C24 H24B 108.0 . . ? H24A C24 H24B 107.2 . . ? C26 C25 C30 116.4(13) . . ? C26 C25 C24 123.4(15) . . ? C30 C25 C24 119.9(14) . . ? C27 C26 C25 120.5(13) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 119.0(11) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C29 C28 C27 123.3(17) . . ? C29 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? C30 C29 C28 113.4(17) . . ? C30 C29 C34 131.0(15) . . ? C28 C29 C34 115.6(16) . . ? C29 C30 O3 113.2(17) . . ? C29 C30 C25 126.8(11) . . ? O3 C30 C25 119.3(16) . . ? O3 C31 C32 102.5(9) . . ? O3 C31 H31A 111.3 . . ? C32 C31 H31A 111.3 . . ? O3 C31 H31B 111.3 . . ? C32 C31 H31B 111.3 . . ? H31A C31 H31B 109.2 . . ? C33 C32 C31 106.1(15) . . ? C33 C32 H32A 110.5 . . ? C31 C32 H32A 110.5 . . ? C33 C32 H32B 110.5 . . ? C31 C32 H32B 110.5 . . ? H32A C32 H32B 108.7 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C2 C34 C29 117.9(12) . . ? C2 C34 H34A 107.8 . . ? C29 C34 H34A 107.8 . . ? C2 C34 H34B 107.8 . . ? C29 C34 H34B 107.8 . . ? H34A C34 H34B 107.2 . . ? O4 C35 C36 112.3(12) . . ? O4 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? O4 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C37 C36 O5 99.5(13) . . ? C37 C36 C35 113.4(13) . . ? O5 C36 C35 109.3(13) . . ? C37 C36 H36 111.4 . . ? O5 C36 H36 111.4 . . ? C35 C36 H36 111.4 . . ? C36 C37 C38 113.2(13) . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? H37A C37 H37B 107.8 . . ? C37 C38 C39 111.9(12) . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38B 109.2 . . ? C39 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C40 C39 C38 112.4(12) . . ? C40 C39 H39A 109.1 . . ? C38 C39 H39A 109.1 . . ? C40 C39 H39B 109.1 . . ? C38 C39 H39B 109.1 . . ? H39A C39 H39B 107.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O5 C41 C46 131.4(15) . . ? O5 C41 C42 104.6(14) . . ? C46 C41 C42 123.6(15) . . ? C43 C42 C41 120.9(15) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 119.3(15) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C43 C44 C45 117.4(15) . . ? C43 C44 H44 121.3 . . ? C45 C44 H44 121.3 . . ? C46 C45 C44 124.9(16) . . ? C46 C45 H45 117.6 . . ? C44 C45 H45 117.6 . . ? C45 C46 O6 137.6(16) . . ? C45 C46 C41 113.8(16) . . ? O6 C46 C41 108.4(14) . . ? C48 C47 O6 117.0(12) . . ? C48 C47 H47A 108.1 . . ? O6 C47 H47A 108.1 . . ? C48 C47 H47B 108.1 . . ? O6 C47 H47B 108.1 . . ? H47A C47 H47B 107.3 . . ? O7 C48 C47 105.7(11) . . ? O7 C48 H48A 110.6 . . ? C47 C48 H48A 110.6 . . ? O7 C48 H48B 110.6 . . ? C47 C48 H48B 110.6 . . ? H48A C48 H48B 108.7 . . ? C50 C49 O7 120.0(12) . . ? C50 C49 H49A 107.3 . . ? O7 C49 H49A 107.3 . . ? C50 C49 H49B 107.3 . . ? O7 C49 H49B 107.3 . . ? H49A C49 H49B 106.9 . . ? O8 C50 C49 105.7(12) . . ? O8 C50 H50A 110.6 . . ? C49 C50 H50A 110.6 . . ? O8 C50 H50B 110.6 . . ? C49 C50 H50B 110.6 . . ? H50A C50 H50B 108.7 . . ? C52 C51 O8 110.4(18) . . ? C52 C51 C56 120.0(18) . . ? O8 C51 C56 129.4(17) . . ? C51 C52 C53 122(2) . . ? C51 C52 H52 119.0 . . ? C53 C52 H52 119.0 . . ? C52 C53 C54 117.4(13) . . ? C52 C53 H53 121.3 . . ? C54 C53 H53 121.3 . . ? C55 C54 C53 117.0(14) . . ? C55 C54 H54 121.5 . . ? C53 C54 H54 121.5 . . ? C56 C55 C54 128.5(15) . . ? C56 C55 H55 115.8 . . ? C54 C55 H55 115.8 . . ? C55 C56 O9 140.4(16) . . ? C55 C56 C51 114.6(15) . . ? O9 C56 C51 105.0(14) . . ? O9 C57 C62 112.9(13) . . ? O9 C57 C58 119.8(13) . . ? C62 C57 C58 111.8(14) . . ? O9 C57 H57 103.3 . . ? C62 C57 H57 103.3 . . ? C58 C57 H57 103.3 . . ? C59 C58 C57 130.8(17) . . ? C59 C58 H58A 104.6 . . ? C57 C58 H58A 104.6 . . ? C59 C58 H58B 104.6 . . ? C57 C58 H58B 104.6 . . ? H58A C58 H58B 105.7 . . ? C60 C59 C58 117.1(19) . . ? C60 C59 H59A 108.0 . . ? C58 C59 H59A 108.0 . . ? C60 C59 H59B 108.0 . . ? C58 C59 H59B 108.0 . . ? H59A C59 H59B 107.3 . . ? C59 C60 C61 124(2) . . ? C59 C60 H60A 106.4 . . ? C61 C60 H60A 106.4 . . ? C59 C60 H60B 106.4 . . ? C61 C60 H60B 106.4 . . ? H60A C60 H60B 106.4 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O1 C62 C57 118.0(14) . . ? O1 C62 H7A 107.8 . . ? C57 C62 H7A 107.8 . . ? O1 C62 H7B 107.8 . . ? C57 C62 H7B 107.8 . . ? H7A C62 H7B 107.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C62 O1 C1 C2 -82.4(17) . . . . ? C62 O1 C1 C6 90.9(15) . . . . ? C6 C1 C2 C34 -176.6(18) . . . . ? O1 C1 C2 C34 -6(2) . . . . ? C6 C1 C2 C3 1(3) . . . . ? O1 C1 C2 C3 171.9(12) . . . . ? C1 C2 C3 C4 6(2) . . . . ? C34 C2 C3 C4 -176.3(17) . . . . ? C2 C3 C4 C5 -7(3) . . . . ? C3 C4 C5 C6 1(3) . . . . ? C4 C5 C6 C1 5(3) . . . . ? C4 C5 C6 C7 -179.4(16) . . . . ? C2 C1 C6 C5 -7(3) . . . . ? O1 C1 C6 C5 -177.8(14) . . . . ? C2 C1 C6 C7 178.8(18) . . . . ? O1 C1 C6 C7 7(3) . . . . ? C5 C6 C7 C8 -124.6(16) . . . . ? C1 C6 C7 C8 50(3) . . . . ? C6 C7 C8 C9 -128.9(14) . . . . ? C6 C7 C8 C13 52(2) . . . . ? C13 C8 C9 C10 -5.0(16) . . . . ? C7 C8 C9 C10 175.6(11) . . . . ? C8 C9 C10 C11 4.5(17) . . . . ? C9 C10 C11 C12 -2(2) . . . . ? C10 C11 C12 C13 1(2) . . . . ? C10 C11 C12 C17 -176.9(15) . . . . ? C11 C12 C13 O2 -179.1(11) . . . . ? C17 C12 C13 O2 -1(2) . . . . ? C11 C12 C13 C8 -2(2) . . . . ? C17 C12 C13 C8 175.9(13) . . . . ? C14 O2 C13 C12 -83(2) . . . . ? C14 O2 C13 C8 99.8(17) . . . . ? C9 C8 C13 C12 4.6(16) . . . . ? C7 C8 C13 C12 -176.1(19) . . . . ? C9 C8 C13 O2 -178.3(10) . . . . ? C7 C8 C13 O2 1.0(18) . . . . ? C13 O2 C14 C15 176.2(16) . . . . ? O2 C14 C15 C16 140.4(16) . . . . ? C13 C12 C17 C18 -49(2) . . . . ? C11 C12 C17 C18 128.7(19) . . . . ? C12 C17 C18 C23 -55(2) . . . . ? C12 C17 C18 C19 128.6(19) . . . . ? C17 C18 C19 C20 -179.2(16) . . . . ? C23 C18 C19 C20 5(2) . . . . ? C18 C19 C20 C21 2(2) . . . . ? C19 C20 C21 C22 -6(2) . . . . ? C20 C21 C22 C23 2(2) . . . . ? C20 C21 C22 C24 -177.0(13) . . . . ? C35 O4 C23 C22 83.0(15) . . . . ? C35 O4 C23 C18 -95.5(14) . . . . ? C21 C22 C23 O4 -173.6(13) . . . . ? C24 C22 C23 O4 5(2) . . . . ? C21 C22 C23 C18 5(2) . . . . ? C24 C22 C23 C18 -176.2(14) . . . . ? C17 C18 C23 O4 -6.1(19) . . . . ? C19 C18 C23 O4 170.6(12) . . . . ? C17 C18 C23 C22 175.4(13) . . . . ? C19 C18 C23 C22 -7.9(18) . . . . ? C23 C22 C24 C25 50(2) . . . . ? C21 C22 C24 C25 -131.2(16) . . . . ? C22 C24 C25 C26 -127.4(17) . . . . ? C22 C24 C25 C30 60(2) . . . . ? C30 C25 C26 C27 -3(2) . . . . ? C24 C25 C26 C27 -176.4(14) . . . . ? C25 C26 C27 C28 3.5(18) . . . . ? C26 C27 C28 C29 -6(2) . . . . ? C27 C28 C29 C30 8(3) . . . . ? C27 C28 C29 C34 -173.5(14) . . . . ? C28 C29 C30 O3 -178.6(12) . . . . ? C34 C29 C30 O3 4(2) . . . . ? C28 C29 C30 C25 -9(2) . . . . ? C34 C29 C30 C25 173.5(16) . . . . ? C31 O3 C30 C29 -96.2(19) . . . . ? C31 O3 C30 C25 93.1(18) . . . . ? C26 C25 C30 C29 6.5(18) . . . . ? C24 C25 C30 C29 179.8(16) . . . . ? C26 C25 C30 O3 175.9(11) . . . . ? C24 C25 C30 O3 -10.8(18) . . . . ? C30 O3 C31 C32 -171.4(16) . . . . ? O3 C31 C32 C33 -144.5(16) . . . . ? C1 C2 C34 C29 -57(2) . . . . ? C3 C2 C34 C29 126.2(18) . . . . ? C30 C29 C34 C2 -48(2) . . . . ? C28 C29 C34 C2 134.3(16) . . . . ? C23 O4 C35 C36 -165.8(11) . . . . ? C41 O5 C36 C37 158.1(13) . . . . ? C41 O5 C36 C35 -82.9(15) . . . . ? O4 C35 C36 C37 -85.9(17) . . . . ? O4 C35 C36 O5 164.2(12) . . . . ? O5 C36 C37 C38 -62.0(17) . . . . ? C35 C36 C37 C38 -178.0(14) . . . . ? C36 C37 C38 C39 173.5(15) . . . . ? C37 C38 C39 C40 -172.2(15) . . . . ? C36 O5 C41 C46 -78(2) . . . . ? C36 O5 C41 C42 109.5(13) . . . . ? O5 C41 C42 C43 174.3(13) . . . . ? C46 C41 C42 C43 1(2) . . . . ? C41 C42 C43 C44 -3(2) . . . . ? C42 C43 C44 C45 4(2) . . . . ? C43 C44 C45 C46 -5(2) . . . . ? C44 C45 C46 O6 -172.3(18) . . . . ? C44 C45 C46 C41 3(2) . . . . ? C47 O6 C46 C45 2(3) . . . . ? C47 O6 C46 C41 -173.4(13) . . . . ? O5 C41 C46 C45 -172.2(15) . . . . ? C42 C41 C46 C45 -1(2) . . . . ? O5 C41 C46 O6 5(2) . . . . ? C42 C41 C46 O6 175.3(14) . . . . ? C46 O6 C47 C48 -175.8(14) . . . . ? C49 O7 C48 C47 152.2(12) . . . . ? O6 C47 C48 O7 89.1(14) . . . . ? C48 O7 C49 C50 -166.3(15) . . . . ? C51 O8 C50 C49 -172.1(13) . . . . ? O7 C49 C50 O8 -80.8(15) . . . . ? C50 O8 C51 C52 -11(2) . . . . ? C50 O8 C51 C56 172.9(16) . . . . ? O8 C51 C52 C53 -172.9(15) . . . . ? C56 C51 C52 C53 3(3) . . . . ? C51 C52 C53 C54 -6(3) . . . . ? C52 C53 C54 C55 8(2) . . . . ? C53 C54 C55 C56 -9(2) . . . . ? C54 C55 C56 O9 -175.4(17) . . . . ? C54 C55 C56 C51 6(2) . . . . ? C57 O9 C56 C55 -101(2) . . . . ? C57 O9 C56 C51 78.0(17) . . . . ? C52 C51 C56 C55 -3(3) . . . . ? O8 C51 C56 C55 172.7(16) . . . . ? C52 C51 C56 O9 178.2(17) . . . . ? O8 C51 C56 O9 -7(2) . . . . ? C56 O9 C57 C62 69.0(18) . . . . ? C56 O9 C57 C58 -155.9(14) . . . . ? O9 C57 C58 C59 55(3) . . . . ? C62 C57 C58 C59 -169.2(19) . . . . ? C57 C58 C59 C60 -87(3) . . . . ? C58 C59 C60 C61 -175(2) . . . . ? C1 O1 C62 C57 159.4(14) . . . . ? O9 C57 C62 O1 -161.1(13) . . . . ? C58 C57 C62 O1 60.3(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.209 _refine_diff_density_min -0.174 _refine_diff_density_rms 0.039