Although reversible photo-dimerization or oxygenation of anthracene and its derivatives is a common reaction, light-initiated reversible conversion of endoperoxide organometallic frameworks has only rarely been addressed. Herein, a series of tetranuclear organometallic macrocycles, [Cp*Rh(μ-CO-κO)](BP4VA)(OTf) (4), [Cp*Rh(BiBzIm)](BP4VA)(OTf) (5), and [Cp*Rh(DHBQ)](BP4VA)(OTf) (6), were obtained in good yields from the reactions of the binuclear half-sandwich rhodium precursors [Cp*Rh(μ-CO-κO)Cl] (1), [Cp*Rh(BiBzIm)Cl] (2), and [Cp*Rh(DHBQ)Cl] (3) with the 9,10-bis((E)-2-(pyrid-4-yl)vinyl)anthracene (BP4VA) ligand. The photochemical reaction of these metallarectangles was investigated by NMR and UV/vis spectroscopy. We have demonstrated that complexes 4, 5, and 6 can be reversibly and nearly quantitatively converted to the macrocyclic endoperoxides 4-O2, 5-O2, and 6-O2. Meanwhile, the structure of the endoperoxide photoproducts was unambiguously confirmed by H/C NMR spectroscopy, IR spectroscopy, elemental analyses, and X-ray crystallography.
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