Programmed Molecular Engineering: Stepwise, Multicomponent Assembly of a Dimetallic Metallotriangulane

The design and construction of a novel terpyridine‐based, dimetallic, 2D [4]triangulane architecture are reported. Synthesis of the metallotriangulane is achieved by multicomponent stepwise assembly of six bidentate and three tetradentate monomers. Characterization was accomplished by NMR spectroscopy, mass spectrometry and TEM microscopy. It's all in the connectivity: Polytriangular objects, such as the [4]triangulane reported herein, provide insights into new materials construction. The synthesis of stable, 60°‐based, dimeric, >‐‐< complexes easily facilitate the construction of trimeric building blocks that, in turn, trimerize to give a new triangulane.