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Here we introduce a sequential topotactic transformation (STT) strategy, in which a simple steaming treatment induces a cascade of structurally correlated topotactic transformations, systematically uncovering a family of hidden metastable frameworks. Using this STT approach, the small-pore aluminophosphate molecular sieve (AlPO MS) DNL-17 undergoes sequential crystalline\u2013state transitions to yield three previously unknown MSs (DNL-18, DNL-19, and DNL-20). Structural characterization and DFT calculations reveal that these transformations preserve partial ABC-6 stacking motif through selective bond cleavage and framework-fragment sliding. This strategy not only accesses diverse metastable states but also enables pore-size modulation from small-pore to ultramicroporous regimes, leading to efficient propane\/propylene and water\/carbon dioxide separations. It broadens the structural diversity of MSs and provides a strategy for tailoring pore architectures toward application-specific performance.<\/jats:p>","DOI":"10.1021\/jacs.6c14957","type":"journal-article","created":{"date-parts":[[2026,9,2]],"date-time":"2026-09-02T01:03:12Z","timestamp":1788310992000},"page":"38511-38518","source":"Crossref","is-referenced-by-count":0,"title":["Sequential Topotactic\nTransformations Traverse Metastable\nPhases in Complex Aluminophosphate Frameworks with Tunable Pore Architectures"],"prefix":"10.1021","volume":"148","author":[{"given":"Jiahui","family":"Zhu","sequence":"first","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chenyang","family":"Nie","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuanhao","family":"Li","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiaona","family":"Liu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chao","family":"Ma","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Nana","family":"Yan","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5392-3915","authenticated-orcid":true,"given":"Peng","family":"Guo","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7999-2940","authenticated-orcid":true,"given":"Zhongmin","family":"Liu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, China, 116023"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,28]]},"reference":[{"issue":"4","key":"2026090910100494200_cit1","doi-asserted-by":"publisher","first-page":"1146","DOI":"10.1021\/ja00368a062","article-title":"Aluminophosphate\nmolecular sieves: a new class of microporous crystalline inorganic\nsolids","volume":"104","author":"Wilson","year":"1982","journal-title":"J. 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