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The new hexanuclear tricoordinate triply bridging thiolatocopper(I) clusters [NEt<jats:sub>4<\/jats:sub>]<jats:sub>4<\/jats:sub>[Cu<jats:sub>6<\/jats:sub>(SPh)<jats:sub>4<\/jats:sub>Cl<jats:sub>6<\/jats:sub>] (<jats:bold>1<\/jats:bold>) and[NEt<jats:sub>4<\/jats:sub>]<jats:sub>4<\/jats:sub>[Cu<jats:sub>6<\/jats:sub>(SPh)<jats:sub>4<\/jats:sub>Br<jats:sub>6<\/jats:sub>] (<jats:bold>2<\/jats:bold>) were synthesized from the soup of polymeric [Cu<jats:sup>I<\/jats:sup>SPh]<jats:italic><jats:sub>n<\/jats:sub><\/jats:italic> and quaternary ammonium halide. These complexes readily converted into [Et<jats:sub>4<\/jats:sub>N]<jats:sub>2<\/jats:sub>[Cu<jats:sub>5<\/jats:sub>(SPh)<jats:sub>7<\/jats:sub>] (<jats:bold>3<\/jats:bold>) and [Et<jats:sub>4<\/jats:sub>N]<jats:sub>2<\/jats:sub>[Cu<jats:sub>4<\/jats:sub>(SPh)<jats:sub>6<\/jats:sub>] (<jats:bold>4<\/jats:bold>) in the presence of excess amounts of thiol. All are structurally characterized by single\u2010crystal X\u2010ray crystallography and these smaller clusters may be inscribed into the structurally characterized larger cluster {Cu<jats:sub>8<\/jats:sub>S<jats:sub>10<\/jats:sub>} obtained from synthetic copper yeast metallothioneins. Like Cu\u2013MT proteins, all these clusters show photoluminescence around 560 nm on excitation at 350 nm, and these emission spectra are completely quenched by molecular oxygen. Variable copper stoichiometry and the interconversion of only monodentate thiolate ligands in these clusters convey the importance of flexibility, which is relevant to metallothioneins. (\u00a9 Wiley\u2010VCH Verlag GmbH &amp; Co. 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