In this paper we study the solution properties of several metallo-supramolecular assemblies containing polystyrene (PS) and poly(ethylene oxide) (PEO) blocks linked via Ru2+ ions: PS20–[Ru2+]–PEO70, PS20–[Ru2+]–PS20, and PEO225–[Ru2+]–PEO225. Sedimentation equilibrium measurements were performed to determine the molar mass distribution and state of association, and the sedimentation velocity measurements were used to obtain the molar mass distribution, sedimentation coefficient distribution, their average values, and average diffusion coefficient. The results obtained from the two types of experiments are compared and discussed.