We synthesized for the first time a series of emissive ring-shaped Re(I) complexes (Re-rings) with various numbers of Re(I) units and various lengths of bridge ligands. The photophysical properties of the Re-rings could be varied widely through changes in the size of the central cavity. A smaller central cavity of the Re-rings induced intramolecular π-π interactions between the ligands and consequently caused a stronger emission and a longer lifetime of the excited state. The Re-rings can function as efficient and durable photosensitizers. The combination of a trinuclear Re-ring photosensitizer with fac-[Re(bpy)(CO)3(MeCN)](+) (bpy = 2,2'-bipyridine) as a catalyst photocatalyzed CO2 reduction with the highest quantum yield of 82%.

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Various cationic rhenium(I) and ruthenium(II) mono-and multinuclear complexes were successfully separated by sizeexclusion chromatography (SEC), using a 50:50 (v/v) mixture of methanol and acetonitrile with CH3CO2NH4 as an eluent. The logarithms of the molecular weights were accurately linear in the distribution coefficients: for linear-shaped rhenium(I) multinuclear complexes, log MW = -2.86KSEC + 5.24 (r = -0.990 and n = 15); for ring-shaped rhenium(I) multinuclear complexes, log MW = -2.94KSEC + 5.40 (r = -0.999; n = 5); for bimetallic complexes including ruthenium(II), log MW = -0.40KSEC + 3.37 (r = -0.959; n = 6). This separation method is applicable to the preparativescale separation of cationic multinuclear complexes from a mixture.

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