Abstract. C21H2006, Mr=368"39, orthorhombic, P2~2121, a = 11.669 (2), b = 14.975 (2), c = 10-663 (2) A, V = 1863 (2)/k 3, Z= 4, Dx = 1.31 g cm -3, A(Mo Ka) = 0.71069 A, F = 0.90 cm-1, F(000) = 7768, T = 203 K, R = 0.064 for 1233 unique data with I> 20,(/). The molecular structure is very close to having idealized twofold geometry with the two substituents on the acetal carbon displaced 1.06 and 1.28 A with respect to the dioxolane ring and the two ethoxycarbonyl groups on the 4 and 5 positions in equatorial positions; the torsional angle about the backbone is 87.4 (6) ° .Introduction. We have synthesized a homochiral dioxolane derived from fluorenone dimethylacetal and diethyl tartrate as part of a program in chiral organometallic reagents. The structure of the dioxolane, reported here, contains several remarkable features important for the study and possible application of homochiral dioxolanes in stereoselective synthesis.