BACKGROUND: TRANSITION METAL SCHIFF BASE COMPLEXES HAVE BEEN THE SUBJECT OF GROWING GREAT INTEREST DUE TO THEIR POTENTIAL APPLICATION IN DIFFERENT FIELDS OF BIOLOGICAL ACTIVITIES, MOLECULAR MAGNETIC MATERIALS AND METALLOSUPRAMOLECULAR CHEMISTRY [1].SCHIFF BASE LIGANDS HAVE GAINED MUCH IMPORTANCE IN MEDICINAL INORGANIC CHEMISTRY IN VIEW OF THEIR DIVERSE BIOLOGICAL, PHARMACO-LOGICAL, ANTITUMOR ACTIVITY AND THEIR EXCEPTIONAL CHELATING ABILITY [2]. MOLYBDENUM PLAY IMPORTANT ROLE IN BIOLOGICAL SYSTEMS. MOLYBDENUM COMPLEXE CHEMISTRY HAS GAINED MUCH ATTENTION SINCE MOLYBDENUM WAS FOUND IN THE ACTIVE SITES OF ENZYMES SUCH AS NITROGENASE, ALDEHYDE OXIDASE, XANTHINE OXIDASE, SULFITE OXIDASE, NITRATE REDUCTASE AND XANTHINE DEHYDROGENASE. MOREOVER, FOR POSSESSING ONE OR MORE MO=O UNIT IN THEIR ACTIVE SITES, THESE NATURAL OXOMOLYBDENUM ENZYMES ARE ALSO WIDELY USED AS CATALYSTS IN INDUSTRIAL PROCESSES SUCH AS OLEFIN METATHESIS, OLEFIN EPOXIDATION ETC. TO SIMULATE THE BIOLOGICAL ACTIVITIES, A NUMBER OF OXO-MOLYBDENUM COMPLEXES WITH STABLE AND VARIABLE OXIDATION STATES VARYING FROM FOUR TO EIGHT, HAVE BEEN INVESTIGATED. HOWEVER, IT IS STILL A CHALLENGE FOR PEOPLE TO UNDERSTAND WELL THAT THE IMPORTANT PROPERTIES OF THIS METAL AND ITS INTERACTION MECHANISM WITH LIVING ORGANISM. [3]METHODS: THE ASYMMETRIC TRIDENTATE SCHIFF BASE (H2L) WAS OBTAINED BY ADDITION OF A SOLUTION OF 2-AMINO-2- METHYLPROPAN-1-OL (0.01 MOL) IN ETHANOL TO A SOLUTION OF 2-HYDROXY-1-BEBZALDEHYDE (0.01 MOL) IN ETHANOL AND THE REACTION MIXTURE WAS STIRRED IN AIR AT REFLUX FOR 1 H. THE SOLUTION WAS KEPT ONE DAY GIVING A YELLOW PRECIPITATE. THE CRUDE PRODUCT WAS RECRYSTALLIZED FROM CHCL3. TO PREPARE NANO-SIZED [MOO2LCH3OH], A TETRAHYDROFURAN (THF) SOLUTION OF THE SCHIFF BASE LIGAND, H2L (5 MMOL) WAS POURED DROPWISE UNDER ULTRASONIC IRRADIATION INTO TO A [MOO2 (ACAC)2] (5MMOL) IN THF DURING 40 MIN. AFTER THE END OF THE TITRATION, THE SOLUTION WAS KEPT IN THE ULTRASONIC BATH FOR A PERIOD OF 120 MIN. THE OBTAINED PRECIPITATES WERE FILTERED AND THEN DRIED.RESULTS: NANOSTRUCTURES OF A NEW DIOXO MOLYBDENUM COMPLEX, [MOO2LCH3OH] HAVE BEEN SYNTHESIZED BY A SONOCHEMICAL PROCESS AND CHARACTERIZED BY SCANNING ELECTRON MICROSCOPY (SEM), X-RAY POWDER DIFFRACTION (XRD) AND FT-IR SPECTROSCOPY.CONCLUSION: SYNTHESIS OF A NEW NANO-SCALE DIOXIDOMOLYBDENUM (VI) COMPLEXES FROM 2-HYDROXY-1- BENZLALDEHYDE AND 2-AMINO-2-METHYL PROPANOL HAS BEEN PREPARED AND CHARACTERIZED.