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Photosolvation of hexachloroplatinate(IV) in acetonitrile with the formation of the PtIVCl5(CH3CN)− complex was studied in the time range from hundreds of femtoseconds to seconds. The primary Pt(III) intermediate was recorded and interpreted as the primary Adamson radical pair [PtIIICl52‐(C4v)⋯Cl], which then accepts an electron from a solvent molecule. Two successive Pt(III) intermediates recorded...