The direct assembly of single component 4',4''''-(1,4-phenylene)bis(2,2' : 6',2''-terpyridine) (PTPy) and Co(2+) and PTPy mixed arrays was examined on a Au(111) surface by a simple immersion method. A redox active 2D adlayer consisting of a bisterpyridine derivative and cobalt ions was found to form directly on Au(111) from solution, suggesting that new nanostructures and/or adlayers with electrochemical activity can be precisely designed and controlled by selection of the metal ion and ligand.