New polystyrene supported mixed Schiff bases(PSCH 2 –LH 2 ) and their coordination compounds with nickel(II), dioxomolybdenum(VI), and dioxouranium(VI) have been synthesized. PSCH 2 –LH 2 have been synthesized by the reaction of chloromethylated polystyrene crosslinked with divinylbenzene(PSCH 2 –Cl) and the Schiff bases(LH 2 ) derived from 3-formylsalicylic acid, ethylenediamine or propylene diamine, and acetylacetone. The polystyrene-supported coordination compounds are of the types: PSCH 2 –LM(where M = Ni, MoO 2, UO 2 ). They have been synthesized by the reaction of PSCH 2 –LH 2 and the metal salt/metal coordination compounds in DMF. The coordination compounds have been characterized on the basis of elemental analyses, IR, reflectance, and magnetic susceptibility measurements. The shifts of the ν (C=N)(azomethine), ν (C–O)(phenolic) and ν (C–O)(enolic) stretches indicate the ONNO donor behavior of PSCH 2 –LH 2. The polystyrene-supported Ni(II) compound is square planar; MoO2 (VI) and UO2 (VI) compounds are octahedral and Zr(IV) compounds are pentagonal bipyramidal. The compounds, PSCH 2 –LM(where M = Ni, MoO 2, and UO 2 ) are diamagnetic
