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Ts3 binds to the domain IV voltage sensor of voltage\u2010gated sodium channels (Na<jats:sub>v<\/jats:sub>) and slows down their fast inactivation. The covalent structure of the Ts3 toxin is uncertain, and the structure of the folded protein molecule is unknown. Herein, we report the total chemical synthesis of four candidate Ts3 toxin protein molecules and the results of structure\u2013activity studies that enabled us to establish the covalent structure of biologically active Ts3 toxin. We also report the synthesis of the mirror image form of the Ts3 protein molecule, and the use of racemic protein crystallography to determine the folded (tertiary) structure of biologically active Ts3 toxin by X\u2010ray diffraction.<\/jats:p>","DOI":"10.1002\/anie.201603420","type":"journal-article","created":{"date-parts":[[2016,5,31]],"date-time":"2016-05-31T20:14:52Z","timestamp":1464725692000},"page":"8639-8642","source":"Crossref","is-referenced-by-count":19,"title":["Elucidation of the Covalent and Tertiary Structures of Biologically Active Ts3 Toxin"],"prefix":"10.1002","volume":"55","author":[{"given":"Bobo","family":"Dang","sequence":"first","affiliation":[{"name":"Department of Chemistry University of Chicago  Chicago IL 60637 USA"},{"name":"Department of Biochemistry &amp; Molecular Biology University of Chicago  Chicago IL 60637 USA"},{"name":"Institute for Biophysical Dynamics University of Chicago  Chicago IL 60637 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Tomoya","family":"Kubota","sequence":"additional","affiliation":[{"name":"Department of Biochemistry &amp; Molecular Biology University of Chicago  Chicago IL 60637 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Kalyaneswar","family":"Mandal","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of Chicago  Chicago IL 60637 USA"},{"name":"Department of Biochemistry &amp; Molecular Biology University of Chicago  Chicago IL 60637 USA"},{"name":"Institute for Biophysical Dynamics University of Chicago  Chicago IL 60637 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Ana M.","family":"Correa","sequence":"additional","affiliation":[{"name":"Department of Biochemistry &amp; Molecular Biology University of Chicago  Chicago IL 60637 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Francisco","family":"Bezanilla","sequence":"additional","affiliation":[{"name":"Department of Biochemistry &amp; Molecular Biology University of Chicago  Chicago IL 60637 USA"},{"name":"Institute for Biophysical Dynamics University of Chicago  Chicago IL 60637 USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Stephen B. 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