A family of macrocyclic complexes [M 2 L n Cl 2 ] have been synthesized and characterized (M: Cu II or Zn II ; L n : macrocyclic ligand derived from 2-hydroxy-5-methyl-1,3-benzenedicarbaldehyde and different aliphatic diamines and o-phenylenediamine). The influence of the aromaticity of the ligand and the metal center on the spectroscopic properties of the complexes (absorption and emission) has been studied. Making use of the weak interactions between hydrated potassium ions and the layers of the K 0.4 Mn 0.8 PS 3 precursor, the obtained macrocyclic complexes have been intercalated in the interlamellar space by a microwave assisted cationic exchange reaction. The optical properties of the obtained hybrid materials are reported. The absorption edge, recorded by solid state reflectance spectroscopy for Cu II and the Zn II macrocycle-based composites, is 1.67-1.76 eV, both shifted to lower energy compared with that of the pristine MnPS 3 .