To assess the effect of thiolate on the synthesis and properties of homologues of 4, a new series of NCs, [Au24Pt(SR)12(PDT)3] 0 , was produced from Au24Pt(SR)18 (SR = C6 or PET) (Schemes S11 and S12). Successful synthesis of [Au24Pt(SR)12(PDT)3] 0 NCs was confirmed with the UV-vis spectra of these products, which were similar to that of 4 (Figures and). In particular, [Au24Pt(C6)12(PDT)3] 0 was sufficiently stable to allow isolation and analysis of its composition by ESI-MS (Figure ), although [Au24Pt(PET)12(PDT)3] 0 completely decomposed/polymerized during washing an excess of PDTH2 (Figure ). Therefore, the structural characteristics of the SR moiety affects both the synthesis and stability of these novel [Au24Pt(SR)12(PDT)3] 0 NCs.