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This report demonstrates how charged side\u2010chain chemistry affects the hierarchical co\u2010assembly of a family of charge\u2010complementary \u03b2\u2010sheet\u2010forming peptide pairs known as CATCH(X+\/Y\u2212) at physiologic pH and ionic strength in water. In a concentration\u2010dependent manner, the CATCH(6K+) (Ac\u2010KQKFKFKFKQK\u2010Am) and CATCH(6D\u2212) (Ac\u2010DQDFDFDFDQD\u2010Am) pair formed either \u03b2\u2010sheet\u2010rich microspheres or \u03b2\u2010sheet\u2010rich gels with a micron\u2010scale plate\u2010like morphology, which were not observed with other CATCH(X+\/Y\u2212) pairs. This hierarchical order was disrupted by replacing D with E, which increased fibril twisting. Replacing K with R, or mutating the N\u2010 and C\u2010terminal amino acids in CATCH(6K+) and CATCH(6D\u2212) to Qs, increased observed co\u2010assembly kinetics, which also disrupted hierarchical order. Due to the ambient assembly conditions, active CATCH(6K+)\u2010green fluorescent protein fusions could be incorporated into the \u03b2\u2010sheet plates and microspheres formed by the CATCH(6K+\/6D\u2212) pair, demonstrating the potential to endow functionality.<\/jats:p>","DOI":"10.1002\/anie.202314531","type":"journal-article","created":{"date-parts":[[2023,11,6]],"date-time":"2023-11-06T20:19:11Z","timestamp":1699301951000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":11,"title":["Side\u2010Chain Chemistry Governs Hierarchical Order of Charge\u2010Complementary \u03b2\u2010sheet Peptide Coassemblies"],"prefix":"10.1002","volume":"62","author":[{"given":"Renjie","family":"Liu","sequence":"first","affiliation":[{"name":"J. 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