Complexes of Cu(II) nitrate and chloride salts with p-chloro-, p-bromo-and p-iodo-anils of 2-thiophene glyoxal, isolated as binary mixtures of isomers, were separated on thin-layers of silica gel. Separation of mixtures in bulk and of their known quantity was done by column chromatography for determination of isomeric composition of isolates. Resolved isomers were identified using correlation of their R F with spectral properties. The effect of chelate ring contraction on R F values has also been investigated.