In this study, two new salicylidene phosphonate ligands (HL 1 and HL 2 ) and their metal complexes (Cu 2+ , VO 2+ and La 3+ ) were synthesized and characterized by spectroscopic and analytical methods. The molecular structure of the ligand HL 1 was determined by single-crystal X-ray diffraction study. In the structure of the ligand, there is an intramolecular phenol-imine hydrogen bond. The synthesized compounds exhibit only one emission maximum upon excitation at 270-295 nm range. Complexation of the Schiff base ligands with metal ions did not cause a considerable quenching effect. Finally, the complexes prepared were used as catalysts in cyclohexane oxidation under microwave irradiation. The complexes showed high conversion rates (> 90%) for cyclohexane oxidation; however, poor selectivity was observed for all complexes. The La 3+ complexes showed better selectivity for cyclohexane → cyclohexanol transformation with about 45% selectivity.