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Powder X\u2010ray diffraction (PXRD) of the resultant material Zn,Al\u2010ALF795 showed that the ALF795 guest molecules assembled into a monolayer to give a basal spacing of 16.0 \u00c5. FTIR and <jats:sup>13<\/jats:sup>C{<jats:sup>1<\/jats:sup>H} CP MAS NMR spectroscopy confirmed that the molecular structure of the tricarbonyl complex was retained upon intercalation. Scanning electron microscopy (SEM), energy\u2010dispersive X\u2010ray spectroscopy (EDS) and elemental analyses confirmed the phase\u2010purity of Zn,Al\u2010ALF795. The myoglobin assay was used to demonstrate that intercalated ALF795 retains the photoactive behavior of the free CORM, with a substantial fraction (42\u2009%) of the high CO payload (2.46 mmol g<jats:sup>\u20131<\/jats:sup>) being released after exposure to UV light for 3 h under simulated physiological conditions. In addition, gas chromatography was used to track sequential light\u2010 and H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub>\u2010triggered decarbonylation of free and intercalated ALF795. In biological buffer solution (HEPES), less than 2\u2009% Mo leaching from Zn,Al\u2010ALF795 took place after 5 h, showing the strong capacity of the LDH host to retain the unaltered complex and decarbonylation fragments.<\/jats:p>","DOI":"10.1002\/ejic.202000202","type":"journal-article","created":{"date-parts":[[2020,6,22]],"date-time":"2020-06-22T21:45:51Z","timestamp":1592862351000},"page":"2726-2736","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":9,"title":["One\u2010Pot Intercalation Strategy for the Encapsulation of a CO\u2010Releasing Organometallic Molecule in a Layered Double Hydroxide"],"prefix":"10.1002","volume":"2020","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-3876-9195","authenticated-orcid":false,"given":"Isabel B.","family":"Calhau","sequence":"first","affiliation":[{"name":"CICECO \u2010 Aveiro Institute of Materials Department of Chemistry University of Aveiro  Campus Universit\u00e1rio de Santiago 3810\u2010193 Aveiro Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9598-1275","authenticated-orcid":false,"given":"Ana C.","family":"Gomes","sequence":"additional","affiliation":[{"name":"CICECO \u2010 Aveiro Institute of Materials Department of Chemistry University of Aveiro  Campus Universit\u00e1rio de Santiago 3810\u2010193 Aveiro Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6961-4911","authenticated-orcid":false,"given":"Sofia M.","family":"Bruno","sequence":"additional","affiliation":[{"name":"CICECO \u2010 Aveiro Institute of Materials Department of Chemistry University of Aveiro  Campus Universit\u00e1rio de Santiago 3810\u2010193 Aveiro Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3077-3859","authenticated-orcid":false,"given":"Ana C.","family":"Coelho","sequence":"additional","affiliation":[{"name":"Instituto de Tecnologia Qu\u00edmica e Biol\u00f3gica Ant\u00f3nio Xavier Universidade Nova de Lisboa  Av. da Rep\u00fablica, EAN 2780\u2010157 Oeiras Portugal"}]},{"given":"Clara I. 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