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Herein, we report the gas sorption properties of a nonporous coordination network, {[Co(bib)\n                    <jats:sub>2<\/jats:sub>\n                    Cl\n                    <jats:sub>2<\/jats:sub>\n                    ]\u2009\u22c5\u20092MeOH}\n                    <jats:sub>\n                      <jats:italic>n<\/jats:italic>\n                    <\/jats:sub>\n                    (\n                    <jats:bold>sql\u2010bib\u2010Co\u2010Cl\u2010\u03b1<\/jats:bold>\n                    ), featuring square lattice (\n                    <jats:bold>sql<\/jats:bold>\n                    ) topology and the bent linker 1,3\u2010bis(1\n                    <jats:italic>H<\/jats:italic>\n                    \u2010imidazol\u20101\u2010yl)benzene (bib). The as\u2010synthesized\n                    <jats:bold>sql\u2010bib\u2010Co\u2010Cl\u2010\u03b1<\/jats:bold>\n                    has 11.3\u2009% (313\u2005\u00c5\n                    <jats:sup>3<\/jats:sup>\n                    ) of its unit cell volume in closed pores occupied by methanol (MeOH). Upon desolvation and air exposure,\n                    <jats:bold>sql\u2010bib\u2010Co\u2010Cl\u2010\u03b1<\/jats:bold>\n                    underwent a single\u2010crystal to single\u2010crystal (SC\u2010SC) phase transformation to\n                    <jats:bold>sql\u2010bib\u2010Co\u2010Cl\u2010\u03b2\u2032<\/jats:bold>\n                    , wherein MeOH was replaced by water. Activation (vacuum or N\n                    <jats:sub>2<\/jats:sub>\n                    flow) resulted in dehydration and retention of the closed pores, affording\n                    <jats:bold>sql\u2010bib\u2010Co\u2010Cl\u2010\u03b2<\/jats:bold>\n                    with 7.7\u2009% (194\u2005\u00c5\n                    <jats:sup>3<\/jats:sup>\n                    ) guest\u2010accessible space.\n                    <jats:bold>sql\u2010bib\u2010Co\u2010Cl\u2010\u03b2<\/jats:bold>\n                    was found to preferentially adsorb C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    (at 265\u2005K) over CO\n                    <jats:sub>2<\/jats:sub>\n                    (at 195\u2005K) through gate\u2010opening mechanisms, at gate\u2010opening pressures of 59.8 and 27.7\u2005kPa, respectively, while other C2 gases were excluded. PXRD was used to monitor transformations between the three phases of\n                    <jats:bold>sql\u2010bib\u2010Co\u2010Cl<\/jats:bold>\n                    , while in situ DSC, in situ SCXRD under CO\n                    <jats:sub>2<\/jats:sub>\n                    pressure, and computational studies provided insight into the guest transport mechanism, which we attribute to the angular, flexible nature of the bib ligand. Further, the preferential adsorption of C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    over CO\n                    <jats:sub>2<\/jats:sub>\n                    and other C2 gases suggests that transiently porous sorbents might have utility in separations.\n                  <\/jats:p>","DOI":"10.1002\/anie.202423521","type":"journal-article","created":{"date-parts":[[2025,1,21]],"date-time":"2025-01-21T03:51:21Z","timestamp":1737431481000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["A Needle in a Haystack: Transient Porosity in a Closed Pore Square Lattice Coordination Network"],"prefix":"10.1002","volume":"64","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-6934-3261","authenticated-orcid":false,"given":"Kyriaki","family":"Koupepidou","sequence":"first","affiliation":[{"name":"Bernal Institute, Department of Chemical 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