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Previous experimental, theoretical, and simulation studies of methane in liquid water have reached widely conflicting conclusions regarding the structure of hydrophobic hydration\u2010shells. Herein we address this question by performing Raman hydration\u2010shell vibrational spectroscopic measurements of methane in liquid water from \u221210\u2009\u00b0C to 300\u2009\u00b0C (at 30\u2005MPa, along a path that parallels the liquid\u2010vapor coexistence curve). We show that, near ambient temperatures, methane's hydration\u2010shell is slightly more tetrahedral than pure water. Moreover, the hydration\u2010shell undergoes a crossover to a more disordered structure above ca. 85\u2009\u00b0C. Comparisons with the crossover temperature of aqueous methanol (and other alcohols) reveal the stabilizing influence of an alcohol OH head\u2010group on hydrophobic hydration\u2010shell fragility.<\/jats:p>","DOI":"10.1002\/anie.201809372","type":"journal-article","created":{"date-parts":[[2018,10,28]],"date-time":"2018-10-28T15:22:42Z","timestamp":1540740162000},"page":"15133-15137","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":54,"title":["Methane Hydration\u2010Shell Structure and Fragility"],"prefix":"10.1002","volume":"57","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-0021-3984","authenticated-orcid":false,"given":"Xiangen","family":"Wu","sequence":"first","affiliation":[{"name":"College of Marine Science and Technology China University of Geosciences  Wuhan 430074 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wanjun","family":"Lu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Geological Processes and Mineral Resources China University of Geosciences  Wuhan 430074 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Louis M.","family":"Streacker","sequence":"additional","affiliation":[{"name":"Purdue University Department of Chemistry  West Lafayette IN 47907 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9869-1900","authenticated-orcid":false,"given":"Henry S.","family":"Ashbaugh","sequence":"additional","affiliation":[{"name":"Department of Chemical and Biomolecular Engineering Tulane University  New Orleans Louisiana 70118 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4683-5401","authenticated-orcid":false,"given":"Dor","family":"Ben\u2010Amotz","sequence":"additional","affiliation":[{"name":"Purdue University Department of Chemistry  West Lafayette IN 47907 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2018,10,18]]},"reference":[{"key":"e_1_2_2_1_1","unstructured":"\u00a0"},{"key":"e_1_2_2_2_2","volume-title":"H2O: A Biography of Water","author":"Ball P.","year":"1999"},{"key":"e_1_2_2_3_2","volume-title":"Molecular Theory of Water and Aqueous Solutions. 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