We report on the impregnation of THF solutions of the low-valent heterometallic cluster NEt(4)[Co(3)Ru(CO)(12)] into two mesoporous silica matrices, amorphous xerogels and ordered MCM-41, and a study of its thermal decomposition into metallic nanoparticles by X-ray diffraction, transmission electron microscopy and in situ magnetic measurements under controlled atmospheres. The decomposition of the cluster was monitored as a function of temperature by examining the chemical composition of the particles, their size distributions and their structures as well as their magnetic properties. Treatment under inert atmosphere (i.
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