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One of the major challenges in this field lies in elucidating the intracellular generation of small molecules, such as carbon monoxide (CO), nitric oxide (NO), and others, which possess significant therapeutic potential. In this study, in situ surface\u2010enhanced Raman spectroscopy (SERS) is employed to visualize and monitor the carbon dioxide (CO\n                    <jats:sub>2<\/jats:sub>\n                    ) reduction process mediated by a rhenium coated gold nanoflower (Re@Au) catalyst within living cells. The findings provide direct spectroscopic evidence of CO\n                    <jats:sub>2<\/jats:sub>\n                    reduction under intracellular conditions, demonstrating that CO can be catalytically generated from CO\n                    <jats:sub>2<\/jats:sub>\n                    in the cellular environment. 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