Three new heteronuclear complexes [Ru(NO)(NO2)(4)(OH)M(Py)(3)] (M = Co2+,Ni2+,Zn2+) were synthesized and structurally characterized. In all compounds, the [Ru(NO)(NO2)(4)(OH)] fragment is coordinated to the M atom by a bridging OH and two bridging NO2 groups. The coordination environment of the metal also includes three pyridine nitrogen atoms. Thermal decomposition of cobalt and nickel complexes in an inert atmosphere yields bimetallic solid solutions.