The metal complexes of isonitroso-5-methyl-2-hexanone (HIMH) and 5-methyl-2,3-hexanedione dioxime (H 2 MHDDO) with Fe(II), Cu(II) and Hg(II) have been synthesized. Their structures have been investigated by using elemental analyses, electrical conductance, magnetic susceptibility measurements, ESR, UV-Visible, reflectance, IR and NMR spectral measurements. Thermal studies have also been carried out. Results are reported here.