Interestingly, all our efforts to synthesize homologues of 4, such as [Au24Pt(TBBT)12((S-(CH2)n-S))3] 0 (n = 2, 4 or 6), using alkyl dithiolate ligands of varying chain lengths resulted in a mixture of products, which precipitated as insoluble substances during the prolonged reaction or purification steps (Schemes S6-S8 and Figures ). Precipitation occurred regardless of whether the reactions were conducted at room temperature or elevated temperatures under conditions similar to those used to synthesize 4. These results suggest that there is an optimum dithiolate chain length for the high-yield synthesis of 4 or its homologues.