The title compound. 4-n-pentylphenyl-4-n-hexyloxythiobenzoate (6OS5), C24H32O2S crystallizes in the orthorhombic system, space group Pbca. with cell constants a = 5.668(2), b = 52.400(10), c = 15.587(4) Angstrom. Z = 8. The structure was solved by direct methods and refined to the final R = 0.0941 for 1717 observed reflections. The hexyloxythiobenzoate moiety is nearly planar. In the crystal. molecules form molecular layers parallel to the (001) plans and within the layer. they are linked in molecular chains parallel to [100] direction by C - H . . .O weak intermolecular hydrogen bond.