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Herein, the introduction of nitrogen into the para position of benzene in graphyne (2N\u2010GY) is proposed as a carrier for anchoring metal single\u2010atoms onto pyrazine nitrogen. These atoms are then coordinated to the center of the rhombic cavity, ensuring precisely controlled coordination numbers. Inspired by natural enzymes, a series of transition metal single\u2010atom nanozymes (SANs) are constructed utilizing 2N\u2010GY. Both theory\u00a0calculations and experiments demonstrated that the incorporation of metal single\u2010atoms of Fe, Mn, and Mo effectively augmented the enzyme\u2010like activity, with Mo\/GY exhibiting the highest peroxidase \u2010like activity. Based on the differing activities of M\/GY (M = Fe, Mn, Mo) and the varying abilities of sulfhydryl groups in biothiols to occupy metal active sites, sensing arrays for the high\u2010throughput identification of six biothiols are constructed. After combining the fingerprint feature responses of biothiols and SANs with machine learning algorithms, the efficient distinction of the six biothiols is achieved. This study introduces a novel pathway for designing and synthesizing SANs that mimic natural enzymes.<\/jats:p>","DOI":"10.1002\/smll.202409113","type":"journal-article","created":{"date-parts":[[2024,12,24]],"date-time":"2024-12-24T12:52:40Z","timestamp":1735044760000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":9,"title":["Boosting Enzyme\u2010Like Activity Through Controlled Coordination of Metal Single\u2010Atoms in Rhombic Cavity of Graphyne"],"prefix":"10.1002","volume":"21","author":[{"given":"Ruixue","family":"Fu","sequence":"first","affiliation":[{"name":"Department of Chemistry &amp; Institute for Sustainable Energy College of Sciences Shanghai University  Shanghai 200444 P. R. 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