Synthesis and characterization of host-guest nanocomposite materials MCM-41-based [Fe(phen)(3)](2+), [Fe(bpy)(3)](2+), [Ru(bpy)(3)](2+), and [Ru(bpy)(2)Cl-2](+) (where phen = 1,10-phenanthroline and bpy = 2,2'-bipyridine) and studied. Powder X-ray diffraction, FTIR spectrometry, and cyclic voltammetry are used to characterize the prepared nanocomposite materials. The cyclic voltammograms for the complexes dissolved in aqueous solution at glassy carbon electrode yield only a well-defined pair of peaks attributable to the well-known monoelectronic redox processes. The cyclic voltammograms for the MCM-41-based complexes-modified glassy carbon electrode yield three well-defined pairs of peaks attributable to the monoelectronic redox processes of complexes with various coordination numbers. preliminary experimental results of cyclic voltammetry and LR spectrometry demonstrate that the silanol groups within the MCM-41 possess the active sites for adsorption of pyridine ring in ligand, and can be used as a li,ligand to coordinate with the central ion, as well as enable original complexes to be partly dissociated.