In this paper the synthesis of six polyamidoximes from their corresponding diamines with 4,4'-methylenebis (phenylglyoxylohydroximoyl chloride) and 4,4'-methylenebis(chlorophenylgly-oxime) is presented. The average molecular weights of these organic polymers were determined. In addition, the complexes of 4,4'-methylenebis(phenylglyoxylohydroximoyl chloride) with Ni(II), Co(II) and Cu(II) salts were prepared. The structures of these compounds were identified by IR or H-1 NMR spectral data, elemental analyses, magnetic measurements and thermal analysis.