J . Am. Chem. SOC. 1991, 113, 1791-1799
1791
0.040 and 0.052, respectively. The final difference Fourier map contained no features greater than f0.15 e A-3.
were separated by column chromatography on silica gel. The first fraction (elution with benzene-hexane (1:l)) contained the ozonide 8 (86% yield). From the second fraction (elution with benzene) was isolated the diketone 11 (2% yield). Crystal data for solvent-participated product 9: C22H2004r colorless needles, M , = 348.4, triclinic, a = 8.5201 (9) A, b 9.3045 (13) A, c = 12.0403 (12) A, a = 71.817 (9)O, P = 88.336 (8)03Y = 83.044 V = 900.1 A3>2 = 2, D, = 1.285 g ~ m - space ~ , group (No. 2) from successful structure solution and refinement, = 0.710693 A, A M 0 Ka) = 0.82 cm-’, F(000) = 368, data crystal -0.45 X 0.35 X 0.20 mm. Structure Solution and Refinement. The intensity data were collected on an Enraf-Nonius CAD-4 diffractometer with use of w-26 scannine. and graphite-monochromated Mo KCYX-radiation over the region 1.5