The crystal of cholesteryl crotylcarbonate was investigated by X-ray diffraction method. Crystallographic data for the title compound: P21, a=13.510(2)Å, b=11.843(2)Å, c=19.882(2)Å, β=106.88(1)°, Z=4. Reflections were collected with an Enraf-Nonius CAD-4 diffractometer equipped with a graphite monochromator. The structure was solved by direct methods and refined by least-squares analyses. The final R value was 0.125 for 2607 reflections. The cholesterol fragment of the title compound were in good agreement with those for related cholesterol derivatives. The molecules were stacked in clearly separated layers. At the center of the layers, there were cholesteryl-cholesteryl interactions between the symmetry-related B molecules and the cholesteryl-C(17) side chain of A molecules. There were also interactions between the C(17) side chain of B molecules and the crotylcarbonate chain in the interface region between layers. The crystal structure of the title compound turned out to be isostructural with those of cholesteryl ethylcarbonate and cholesteryl propylcarbonate.