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Herein, we covalently graft a nitric oxide (NO)\u2010releasing <jats:italic>N<\/jats:italic>\u2010nitrosamine moiety onto the carbon monoxide (CO)\u2010releasing 3\u2010hydroxyflavone (3\u2010HF) antenna, resulting in the first NO\/CO\u2010releasing donor. Under visible light irradiation, photo\u2010mediated co\u2010release of NO and CO reveals a superior antimicrobial effect toward Gram\u2010positive bacteria with a combination index of 0.053. The synergy of NO and CO hyperpolarizes and permeabilizes bacterial membranes, which, however, shows negligible hemolysis and no evident toxicity toward normal mammalian cells. 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