Experimental. Recrystallization from benzene, toluene, chloroform, dichloromethane, diethyl ether, tetrahydrofuran, ethyl acetate, acetonitrile and methanol solutions under the air were failed. These solutions under hexane atmosphere also gave unsatisfactory results. Only the condition mentioned above has been quite effective to afford the single crystals suitable for X-ray analysis.; M.p. 458.7–459.2 K (not corrected); IR (film): 3524, 2945, 2890, 1790, 1715, 1274, 714 cm-1; 1H NMR (500 MHz, CDCl3): δ (p.p.m.) 8.13–8.10 (m, 2H), 8.03–7.99 (m, 2H), 7.60–7.53 (m, 2H), 7.48–7.42 (m, 4H), 5.56 (d, J = 6.0 Hz, 1H), 5.41 (t, J = 0.9 Hz, 1H), 5.09 (dd, J = 11.5, 4.6 Hz, 1H), 4.84 (s, 1H), 4.49 (d, J = 7.7 Hz, 1H), 4.13 (d, J = 7.7 Hz, 1H), 3.76–3.68 (m, 2H), 3.63 (ddd, J = 10.6, 7.2, 7.2 Hz, 1H), 3.08 (d, J = 14.9 Hz, 1H), 2.66 (s, 3H), 2.40 (dddd, J = 12.9, 4.3, 4.0, 4.0 Hz, 1H), 2.34 (d, J = 10.3 Hz, 1H), 2.29 (dd, J = 15.5, 6.3 Hz, 1H), 1.93 (dddd, J = 12.9, 4.3, 4.3, 4.0 Hz, 1H), 1.75 (d, J = 0.9 Hz, 3H), 1.73–1.60 (m, 3H), 1.59–1.45 (m, 2H), 1.22 (s, 3H), 1.20 (s, 3H), 1.11 (s, 3H); 13C NMR (125 MHz, CDCl3): δ (p.p.m.) 166.4 (C), 166.0 (C), 155.2 (C), 135.1 (CH), 133.4 (CH), 133.3 (CH), 130.5 (C), 130.2 (C), 130.0 (CH), 129.7 (CH), 129.0 (C), 128.7 (CH), 128.7 (CH), 97.9 (CH2), 87.1 (C), 76.9 (CH), 76.5 (CH), 75.1 (CH), 68.7 (CH), 58.3 (CH2), 54.7 (CH3), 45.9 (CH), 42.0 (C), 41.2 (C), 38.1 (CH2), 31.5 (CH2), 30.6 (CH2), 25.7 (CH3), 25.1 (CH2), 22.3 (CH3), 20.2 (CH3), 16.8 (CH3); HRMS (ESI): m/z calcd for C36H44O10Na+ [M+Na]+ 659.2832, found 659.2836.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.Problematic 13 reflections with |I(obs)-I(calc)|/σW(I) greater than 10 (–8 –2 1, –8 –2 2, –8 –1 2, –7 –4 3, –8 –3 6, 3 11 7, 3 10 8, 0 9 9, 2 10 9, 2 8 10, 4 9 10, 2 7 11, 3 8 11) have been omitted in the final refinement.