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Here, we combine solution- and solid-state proton (1H) NMR spectroscopy, NMR relaxometry, modulated-gradient spin\u2013echo (MGSE) NMR diffusometry, infrared spectroscopy, and molecular dynamics simulations to demonstrate that surface hydroxyls drive the structural and dynamic differentiation of water in imogolite nanotubes. In saturated suspensions, we observe the coexistence of distinct water 1H environments, each exhibiting significantly reduced mobility, which we attribute to strong interactions with the imogolite surfaces. As more mobile water is removed, long-range water diffusivity in the fibrous solid samples slows to 1.6 \u00d7 10\u201310 m2\u00b7s\u20131 while local fluctuations increase to 3.4 \u00d7 10\u20138 m2\u00b7s\u20131, indicating a significant increase in molecular restriction through surface interactions. Together, our experiments reveal three coexisting populations with varied structures and mobilities, all distinct from liquid bulk water. We resolve a persistent solid-like interfacial layer strongly bound to surface hydroxyls, characterized by an unusually short T2 (&amp;lt;1 ms), and a very close effective 1H\u20131H distance of \u223c1.55 \u00c5 between water and the inner-surface silanol group. An inner-core population occupying the inner cavity exhibits an intermediate dynamic regime with restricted axial diffusion, while outer-surface water associated with aluminum hydroxyls retains relatively higher mobility. These results experimentally substantiate a hierarchy of water populations in imogolite and show how surface chemistry dictates the structures and dynamics of confined water.<\/jats:p>","DOI":"10.1021\/jacs.5c22784","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T13:17:09Z","timestamp":1785849429000},"page":"32993-33003","source":"Crossref","is-referenced-by-count":0,"title":["Surface Hydroxyls of\nImogolite Nanotubes Drive Distinct\nStructures and Mobility Differentiation of Nanoconfined Water"],"prefix":"10.1021","volume":"148","author":[{"ORCID":"https:\/\/orcid.org\/0009-0006-0102-5375","authenticated-orcid":true,"given":"Xander B.","family":"Fleming","sequence":"first","affiliation":[{"name":"Earth and Environmental Sciences Area, Lawrence Berkeley National Laboratory , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0183-466X","authenticated-orcid":true,"given":"Sophia N.","family":"Fricke","sequence":"additional","affiliation":[{"name":"University of California , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Navya","family":"Singh","sequence":"additional","affiliation":[{"name":"Earth and Environmental Sciences Area, Lawrence Berkeley National Laboratory , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7208-6929","authenticated-orcid":true,"given":"Raynald","family":"Giovine","sequence":"additional","affiliation":[{"name":"University of California , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8716-9463","authenticated-orcid":true,"given":"Pierre","family":"Picot","sequence":"additional","affiliation":[{"name":"Universite\u0301 Paris-Saclay, CEA, CNRS, NIMBE\/LIONS , ,","place":["Gif-sur-Yvette, France, 91191"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hasan","family":"Celik","sequence":"additional","affiliation":[{"name":"University of California , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jeffrey A.","family":"Reimer","sequence":"additional","affiliation":[{"name":"University of California , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0853-0826","authenticated-orcid":true,"given":"Benjamin","family":"Gilbert","sequence":"additional","affiliation":[{"name":"Earth and Environmental Sciences Area, Lawrence Berkeley National Laboratory , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhao","family":"Hao","sequence":"additional","affiliation":[{"name":"Earth and Environmental Sciences Area, Lawrence Berkeley National Laboratory , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,7,29]]},"reference":[{"issue":"11","key":"2026081210082654800_cit1","doi-asserted-by":"publisher","first-page":"136","DOI":"10.1140\/epje\/s10189-021-00136-4","article-title":"Structure and Dynamics\nof Nanoconfined Water and Aqueous Solutions","volume":"44","author":"Corti","year":"2021","journal-title":"Eur. 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