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The crystal structure of a third polymorph ( γ ) of C.I. Pigment Red 1, 1-[(4-nitrophenyl)azo]-2-naphthol has been determined by X-ray diffraction techniques. It crystallises in the monoclinic system with cell parameters  a  = 7.715 ± 0.025 Å,  b  = 25.998 ± 0.081 Å,  c  = 6.964 ± 0.025 Å,  β  = 107.58 ± 0.17°. The space group is  P 2 1 / c  and there are four molecules per unit cell. The structure was solved using direct methods and least-squares refinement has been completed on three-dimensional data, 689 reflections (Cu Kα  radiation). The hydrogen atoms have been found and included but not refined. The final residual is 8.4%. The molecule exists as the hydrazone tautomer and is approximately planar; the benzene and naphthalene groups are planar but are inclined at an angle of 10.8° with respect to each other. The molecules are linked by van der Waals forces. There would appear to be no relationship between this crystal structure and previously reported polymorphs.