The design and synthesis of coordinative truncated tetrahedra is described. Coordination-driven self-assembly of a truncated tetrahedron was achieved using 90° organoplatinum acceptors and a hexapyridyl ligand with six-fold symmetry under mild conditions. This assembly can act as a host towards 1,3,5-triphenylbenzene. The truncated tetrahedral structures and the host-guest complex were identified using multinuclear (31P and 1H) NMR spectroscopy, electrospray ionization (ESI) mass spectrometry, X-ray crystallography, and pulsed field gradient spin-echo (PGSE) NMR, along with computational simulations.
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