We also examined a different method to synthesize the linkage. An attempt was made to synthesize a linkage of Au13 clusters by reacting compound 1 with a diyne having ethynyl groups at both ends (Scheme S2B). Fig. shows the ESI mass spectrum of the product obtained by adding deb-H2 (Fig. ) to an acetonitrile solution of 1•(BF4 -)3 in the presence of a base (triethylamine). The peak with the strongest ion intensity was attributed to [Au13(dppe)5(deb-H)2] 3+ . This result indicates that the Cl ligands on the Au13 surface were substituted by the [deb-H] -anion generated through deprotonation of one of the hydrogens of deb-H2 by the base. By contrast, no distinct peaks were observed in the expected m/z range (1550, 1565, 1580) associated with dimer formation. If both terminal hydrogens of [deb-H2] are deprotonated by the base, [deb] 2-is expected to replace one Cl on each Au13 cluster, forming the desired dimer. However, if both Cl ligands on each Au13 cluster are replaced by [deb] 2-, this would lead to the formation of a polymer connecting multiple Au13 clusters (Scheme S2B). As the reaction proceeded to form structures linking many Au13 clusters, we conclude that selective formation of the desired dimer cannot be achieved using this method.