Building blocks of coordination polymers have attracted much attention because of promising applications in porous materials, molecular engineering and devices. We report here an interfacial self-assembly of bimetallic coordination polymer of Cd-Fe(pytetPY)(2) (pyterpy: 4'-(4-pyridyl)-2,2':6',2 ''-terpyridine). The surface pressure-area and area-time isotherms indicated that stable monolayers of Fe(pyterpy)(2)(BF4)(2) could be formed on the 0.1 mol/l CdCl2 subphase surface after an interfacial coordination reaction over 12 h. By using the Langmuir-Blodgett (LB) method, monolayers of the Cd-Fe(pyterpy)(2) coordination polymer were transferred on the substrate surfaces, and characterized by using the UV-vis absorption and X-ray photoelectron spectroscopy, as well as transition electron microscopy. The spectral data revealed that the LB film was composed of C, Cl, Cd, N and Fe elements, which was in agreement with the composition of the coordination polymer. Reversible redox wave centered at about 500 mV (vs Ag/AgCl) was recorded for the electrode modified with the LB film of the coordination polymer. The present method could be developed to prepare two- and three-dimensional nanoporous building blocks containing two metal ions. (C) 2007 Elsevier B.V. All rights reserved.