The crystal structure of 3β-acetoxy-5α-cholestan-6-one-semicarbazone (C 30H 51O 3 N 3) has been determined by X-ray diffraction methods. It crystallizes in the orthorhombic space group P2 12 12 1 with cell parameters a = 11.641(1), b = 16.552(1) c = 31.181(4) Å and Z = 8. The structure has been refined to an R-value of 0.050 for 4407 observed reflections. Two molecules in the asymmetric unit have been observed. In both the crystallographically independent molecules, all the three six-membered rings (A, B and C) of steroid nucleus exist in chair conformation, while the five- membered ring D exists in 13β distorted-envelope in molecule-I and 13β, 14α half-chair conformation in molecule-II. Three intermolecular N-H...O hydrogen bonds have been observed.