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Metal <jats:italic>N<\/jats:italic>\u2010alkyldithiocarbamates were used as the precursors to the metal\u2013sulfide nanophases and, in particular, Ag<jats:sub>2<\/jats:sub>S nanostructures were investigated in more detail. These were observed as nano\u2010islands at the surface of TiO<jats:sub>2<\/jats:sub> (anatase) particles, which were used as substrates. To explain the formation of these nanocomposite particulates, a tentative mechanism has been proposed which involves the controlled release of sulfide ions from an intermediate coordination compound. Because the growth of the metal sulfide can be controlled at the surface of a photoactive substrate, we anticipate the potential of this synthetic method to chemical design reasonable amounts of semiconductor\u2010sensitized TiO<jats:sub>2<\/jats:sub>, such as Ag<jats:sub>2<\/jats:sub>S\/TiO<jats:sub>2<\/jats:sub> nanocomposites. (\u00a9 Wiley\u2010VCH Verlag GmbH &amp; Co. 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