Self-Assembly of a Redox Active, Metallosupramolecular [Pd3 L6 ]6+ Complex Using a Rotationally Flexible Ferrocene Ligand.

A new ferrocene-containing [Pd3 (L4EFc )6 ]6+ (X- )6 (C ⋅ BF4 and C ⋅ SbF6 where X=BF4 - or SbF6 - ) self-assembled double-walled triangle has been synthesized from the known, rotationally flexible, 1,1'-bis(4-pyridylethynyl)ferrocene ligand (L4EFc ), and characterized by 1 H, 13 C and diffusion ordered (DOSY) NMR spectroscopies, high-resolution electrospray ionization mass spectrometry (HR-ESI-MS), X-ray crystallography and cyclic voltammetry (CV). The molecular structures confirmed that double-walled triangle cage systems (C ⋅ BF4 and C ⋅ SbF6 ) were generated. C ⋅ BF4 was shown to interact with the anionic guest, p-toluenesulfonate. CV experiments revealed that the triangles were redox active, however addition of the guest did not influence the redox potentials.