A thin film was formed by spreading a chloroform dispersion of ahydrophobic clay−organic complexat an air−water interface. The clay−organic complexes wereprepared by reacting synthetic saponite with3-(aminopropyl)dimethylethoxysilane and thereafter with alkanoylchlorides. From the analysis of surfacepressure−area curves, it was concluded that the film were composed of1−3 layers of clay crystallites. Thefilm was repeatedly transferred onto a glassy carbon electrode to buildup 30 layers by the Langmuir−Blodgett method. An electrode modified with the clay multilayer wasfound to be electroactive when itwas soaked in an aqueous solution of[Ru(bpy)3]Cl2 (1 ×10-5 M) and Na2SO4 (0.05M).