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We report the synthesis and oxygen-atom transfer (OAT) photochemistry of [Cu(tpa)BrO 3 ]ClO 4 . In situ spectroscopy and in crystallo experiments indicate OAT proceeds from a Cu–O fragment generated by sequential Cu–O bond cleavage and OAT from BrO x to [Cu(tpa)] + . These results highlight synthetic opportunities in M–O photochemistry and demonstrate the utility of in crystallo experiments to evaluating photochemical reaction mechanisms.more » « less