Thin films of the metallopolymer [Os(bpy)(2) (pVp)(10)](2+), where bpy is 2,2'-dipyridyl and PVP is poly(4-vinylpyridine), luminesce at 750 +/- 12 nm upon excitation at 355nm. The luminescence decay responses can be described by a double exponential decay model in which the limiting lifetimes are 75 14 (population fraction of 0.9) and 35 +/- 8 its (population fraction of 0.1) for films in contact with aqueous 0.1 M H2SO4. Electrochemistry has been used to create well defined concentrations of the luminescence quencher, Os3+ within the films. Time resolved spectroscopy reveals that both dynamic and static processes contribute to luminescence quenching with a rate constant for electron transfer between the photoexcited Os-2* and the Os3+ centres of 1.3x10(7) M(-1)s(-1) being observed. Stable gold nanoparticles have been created within the metallopolymer by the chemical reduction of tetrachloroaurate. These nanocomposite materials exhibit enhanced emission intensity compared to the gold free films.