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However, for ions with identical charge and similar size (e.g., Li+, Na+, K+), it is usually difficult to create sufficiently large differences in transport behavior to achieve high selectivity. Here, we report a covalent organic framework (COF) membrane featuring spatially organized 18-crown-6 sites. These uncharged \u201c\u2013CH2\u2013O\u2013CH2\u2013\u201d groups leverage weak yet size-specific coordination with alkali metal ions. The size compatibility and stable binding of K+ with 18-crown-6 significantly lower its transport energy barrier and enhance its flux, yielding monovalent cation selectivity up to 14.5. Furthermore, we demonstrate that K+ ion can be rapidly delivered between the rotatable neighboring 18-crown-6 sites in the COF nanochannel, following a \u201crotate-and-deliver\u201d mechanism. This study sheds lights on the fundamentals of ion transport within subnanoconfined systems and would stimulate the design of high-performance membranes.<\/jats:p>","DOI":"10.1021\/acs.analchem.6c02518","type":"journal-article","created":{"date-parts":[[2026,7,16]],"date-time":"2026-07-16T03:54:08Z","timestamp":1784174048000},"page":"21660-21669","source":"Crossref","is-referenced-by-count":0,"title":["Spatial Synergy\nof Crown Ether Groups in Covalent\nOrganic Framework Nanochannels Enabling Efficient Monovalent Cation\nSeparation"],"prefix":"10.1021","volume":"98","author":[{"given":"Ri-Jian","family":"Mo","sequence":"first","affiliation":[{"name":"Nanjing University , , ,","place":["Nanjing, China, 210023"]},{"name":"Guangdong Ocean University , , ,","place":["Zhanjiang, China, 524088"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhong-Yan","family":"Xu","sequence":"additional","affiliation":[{"name":"Nanjing University , , ,","place":["Nanjing, China, 210023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shuang","family":"Chen","sequence":"additional","affiliation":[{"name":"Nanjing University , , ,","place":["Nanjing, China, 210023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Saima","family":"Rafique","sequence":"additional","affiliation":[{"name":"Nanjing University , , ,","place":["Nanjing, China, 210023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tian-Run","family":"Zhang","sequence":"additional","affiliation":[{"name":"Nanjing University , , ,","place":["Nanjing, China, 210023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9831-4048","authenticated-orcid":true,"given":"Xing-Hua","family":"Xia","sequence":"additional","affiliation":[{"name":"Nanjing University , , ,","place":["Nanjing, China, 210023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3827-3402","authenticated-orcid":true,"given":"Zhong-Qiu","family":"Li","sequence":"additional","affiliation":[{"name":"Nanjing University , , ,","place":["Nanjing, China, 210023"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,7,15]]},"reference":[{"issue":"1","key":"2026072808090389100_cit1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-023-44625-w","article-title":"Solar-driven membrane separation for direct lithium extraction from\nartificial salt-lake brine","volume":"15","author":"Zhang","year":"2024","journal-title":"Nat. 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