Polychelates of VO(II), Mn(II), Zn(II), Cr(III), and Fe(III) with the bis-oxime of 5, 5′-methylene-bis-salicylaldehyde have been prepared and are characterized on the basis of their elemental analyses, IR, diffuse reflectance spectra, magnetic moments, and thermogravimetric analyses. Except for VO(II), the other metal ions form octahedral polychelates. VO(II) forms a square-pyramidal coordination polymer. The Zn(II) poly-chelate has the highest thermal stability.