A self-assembled multilayer consisting of transition metal and biscarboxyl acid was fabricated by simply immersing an oxide-covered silicon substrate into zirconium (Zr) n-butoxide and terephthalic acid (TPA) solutions alternately. In this multilayer, two TPA monolayers were bridged with a Zr-IV monolayer. The chemistry connecting these monolayers is most likely coordinate bonds between Zr-IV ions and carboxyl groups.