A new series of five complexes of oxovanadium(IV) with the general formula [VO(mac)]SO4 (where mac = tetraazamacrocyclic ligands derived by condensation of 1,1’-oxalyldiimidazole with 1,2-diaminopropane and their reactions with β-diketones) have been prepared using oxometal ion as kinetic template. The prepared complexes have been characterized on the basis of electrical conductance, molecular weight, magnetic moment, elemental analyses, infrared, e.s.r. and electronic spectral data. The probable coordination number of central metal is five (distorted square-pyramid)