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Layered two\u2010dimensional (2D) membranes offer energy\u2010efficient alternatives to conventional extraction and adsorption technologies, yet their selectivity is often constrained by fixed and poorly tunable transport pathways. Here we introduce a coordination\u2010occupation\u2010coupled strategy to program ion transport in layered 2D hybrid membranes combining a confined polyacrylate network between layered vermiculite. Irreversible crosslinking with Al\n                    <jats:sup>3+<\/jats:sup>\n                    ions within polyacrylate network forms unexchangeable coordination sites that stabilize the membrane structure and selectively occupy transport pathways for multivalent ions. This targeted pathway occupation suppresses the transport of Sr\n                    <jats:sup>2+<\/jats:sup>\n                    , La\n                    <jats:sup>3+<\/jats:sup>\n                    and Zr\n                    <jats:sup>4+<\/jats:sup>\n                    , while allowing Cs\n                    <jats:sup>+<\/jats:sup>\n                    to permeate efficiently through alternative routes. The resulting membranes achieve Cs\n                    <jats:sup>+<\/jats:sup>\n                    \/Sr\n                    <jats:sup>2+<\/jats:sup>\n                    separation factors approaching 10\n                    <jats:sup>3<\/jats:sup>\n                    and near\u2010complete separation of Cs\n                    <jats:sup>+<\/jats:sup>\n                    from trivalent and tetravalent ions. This work establishes coordination\u2010occupation coupling as a scalable and material\u2010efficient principle for high\u2010selectivity ion separations, with direct implications for sustainable radionuclide remediation and critical metal recovery.\n                  <\/jats:p>","DOI":"10.1002\/adma.73120","type":"journal-article","created":{"date-parts":[[2026,4,20]],"date-time":"2026-04-20T06:51:08Z","timestamp":1776667868000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":12,"title":["Programming Ion Transport in Layered 2D Hybrid Membranes via Coordination\u2010Occupation Coupling"],"prefix":"10.1002","volume":"38","author":[{"given":"Yumei","family":"Tan","sequence":"first","affiliation":[{"name":"School of Chemical Engineering Sichuan University  Chengdu Sichuan P. R. 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