A series of Ru-II heterodinuclear complexes of ABA-type with electron-deficient bis-terpyridines as building blocks was synthesized by (R-tpy)(RuCI3)-C-III complexation. These compounds were characterized by NMR spectroscopy, MALDI-TOF, ESI-TOF mass spectrometry, and elemental analysis. The results were compared with a coil-rod-coil Ru-II metallo-supra-molecular copolymer, which was synthesized by bis-complex formation between a hydrophilic omega-terpyridine poly(ethylene glycol) Ru-II mono-complex and a hydrophobic bis-terpyridine-functionalized rigid core. This amphiphilic Ru-II triblock copolymer showed self-assembly to clusters and micelles in aqueous solution, which was studied by transmission electron microscopy and dynamic light scattering. Applying velocity sedimentation experiments the number of amphiphilic Ru-II ABA triblock copolymer molecules within the micelles could be estimated. Finally, the photophysical properties of the Ru-II supramolecular assemblies were investigated by UV-vis spectroscopy. (C) 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 49: 1396-1408, 2011