Light brown [VO(5-NO 2 salen)]·2H 2 O (1; H 2 (5-NO 2 salen)=N,N′-di-5-nitrosalicylidene-1,2-ethanediamine) and orange [VO(5-NO 2 sal-meso-stien)]·0.5H 2 O (2; H 2 (5-NO 2 sal-meso-stien)=N,N′-di-5-nitrosalicylidene-(R,S)(S,R)-1,2-diphenyl-1,2-ethanediamine) which have linear chain structures in the solid state turn dark brown and yellow-brown, respectively, when ground thoroughly in mortars. The IR spectra of 1 and 2 in Nujol mulls show strong V=O stretching bands at 875 and 905 cm −1 , respectively. On the other hand, the spectra of the finely ground complexes in Nujol mulls show very weak V=O stretching bands. X-ray powder diffraction patterns of the ground complexes scarcely show diffraction peaks. The spectroscopic and magnetic data suggest that the linear chain structures in the crystals of 1 and 2 are destroyed on grinding to yield the fragments of the polymeric chains.