Six nanoscale molecular squares are reported. They areprepared in essentially quantitative yields viaspontaneous self-assembly of preprogrammed 90
angular
units withdiverse bimetallic linear linkers. Characterizationwas accomplished with multinuclear NMR and, in two cases, via ESI-FTICRmass spectral data. The size of thesenovel metallomacrocycles range from 3.6 nm (diagonal) and 2.6 nm (side)for the smallest to 4.7 nm (diagonal) and3.4 nm (side) for the largest as estimated by extensible systematicforce field calculations. The molecular squaresincorporating alkynyl
units as corners are able to complex fourAg
+ ions via the
-tweezer effect.