Crystal data: C2,H,,0i,~(C9Hld02)0.5~(H20)3, M, =728.82, space group C222,. a = 24.0021(17), b=14.8120(13), c=21.7916(18)A; V=7747A3. Z = 8, p..,. =1.277 gcm-', R = 0.0828 for 1540 unique observed reflections with Fo t 4.0u(F0). Full description of the structure will be published elsewhere (manuscript in preparation). The small deviation in the optical rotation from the literature value is due to the presence of traces of TMaCD ([a];' =140) in (R)-1, which could not be easily removed. Column type: Rt-DDEX, (30 m, 0.32 i.d.), Restek Corporation; 70C isothermal run, He carrier gas; Retention times: fR(S) = 19.33 s, tR(R) = 19.74 s, resolution 0.6; we thank A. Ortiz, Dr. V. Roussis, and Dr. V. Mazomenos for the GC analysis. a) A. Botsi. Ph.D. Thesis, University of Athens, 1994; b) A. Botsi, K. Yannakopoulou, B. Perly, E. Hadjoudis, J. Org. Chem. 1995, 60, 4017-4023. This quantitative 13C NMR experiment (inverse gated decoupling, INVGATE) was carried out with a delay time of 10 s ( T I measurements of (k1-1 in aqueous solution suggested a maximum relaxation time of 1.45 s for the protonated carbon atoms) on a Bruker AC 250 MHz NMR spectrometer at 298 K.
