Three dimensional crystal structure analysis has been carried out on β-D, 1 → 4 xylobiose hexaacetate (1)[Formula: see text]The crystal data are: orthorhombic, P212121, a = 10.938(2), b = 8.377(4), c = 29.976(7) Å. It was found that the bond lengths and angles of the Cl chairs are similar to other carbohydrate structures, the conformational angles (Φ,Ψ) = (20.4°, −15.2°) and the orientations of the acetate groups are in good agreement with those predicted by stereochemical calculations using Flory functions. The structural resemblance between this molecule and the polymer, xylan diacetate, is discussed.