Abstract: Four macrocyclic d-f heterodinuclear complexes \[M1M2L\](NO3)(H2O)n(L, ligand) were synthesized and characterized. The complexes with different valences were then immobilized on mesoporous SBA-15 synthesized by microwave heating. The samples are characterized by IR, UV-vis, XRD, ICP-AES, TG/DTA and used as catalysts in the oxidation of cyclohexane with H2O2 as an oxidant. The influences of solvent, reaction temperature, and time on the conversion of cyclohexane were examined. The complexes encapsulated in SBA15 exhibit excellent catalytic activity and stability in cyclohexane oxidation with H2O2.