Abstract: | The crystal structure of 3b‐acetoxy‐5a‐cholestan‐6‐one‐semicarbazone (C30H51O3N3) has been determined by X‐ray diffraction methods. It crystallizes in the orthorhombic space group P212121 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. |