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Here, we employ weakly bound CO2\u2013H2O clusters as experimentally tractable model systems to investigate how microsolvation influences ionization-driven molecular growth and bond formation. Using synchrotron-based vacuum ultraviolet photoionization mass spectrometry over the 10\u201314 eV photon-energy range, we investigate mixed CO2\u2013H2O clusters and observe new oxygen-bearing products formed through molecular growth and bond reorganization. We detect m\/z 78, assigned to [H2CO4]+, consistent with peroxide bond formation within mixed CO2\u2013H2O clusters. We further identify an indirect route to H2O2 through cluster rearrangement and evaporation, evidenced by m\/z 112 and assigned to [(H2O2)2(CO2)]+. Product branching depends strongly on cluster composition, with water-rich environments favoring peroxide-forming chemistry. Additional products, including formic acid and carbonic acid, reveal extensive ionization-induced molecular growth within hydrogen-bonded clusters. Density functional theory at the double-hybrid level reveals roaming-like intermediates, charge localization, and low-barrier rearrangements unique to the mixed cluster environment. Together, the experimental and theoretical results identify nanoscale CO\u2013H2O aggregates as chemically active reactors.<\/jats:p>","DOI":"10.1021\/jacs.6c07627","type":"journal-article","created":{"date-parts":[[2026,8,13]],"date-time":"2026-08-13T21:02:25Z","timestamp":1786654945000},"page":"35681-35693","source":"Crossref","is-referenced-by-count":0,"title":["Ionization-Driven Oxygen\u2013Oxygen\nBond Formation\nin Mixed CO2\u2013H2O Clusters: The Role of\nSolvation and Cluster Composition"],"prefix":"10.1021","volume":"148","author":[{"given":"Nureshan","family":"Dias","sequence":"first","affiliation":[{"name":"Lawrence Berkeley National Laboratory , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zeyi","family":"Zhang","sequence":"additional","affiliation":[{"name":"Lawrence Berkeley National Laboratory , , , ,","place":["Berkeley, California, United States, 94720"]},{"name":"University of California , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2474-2346","authenticated-orcid":true,"given":"Alexander K.","family":"Lemmens","sequence":"additional","affiliation":[{"name":"Lawrence Berkeley National Laboratory , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Anna","family":"Wannenmacher","sequence":"additional","affiliation":[{"name":"Lawrence Berkeley National Laboratory , , , ,","place":["Berkeley, California, United States, 94720"]},{"name":"University of California , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0162-0477","authenticated-orcid":true,"given":"Jin","family":"Qian","sequence":"additional","affiliation":[{"name":"Lawrence Berkeley National Laboratory , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4309-6669","authenticated-orcid":true,"given":"Martin","family":"Head\u2212Gordon","sequence":"additional","affiliation":[{"name":"Lawrence Berkeley National Laboratory , , , ,","place":["Berkeley, California, United States, 94720"]},{"name":"University of California , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1216-673X","authenticated-orcid":true,"given":"Musahid","family":"Ahmed","sequence":"additional","affiliation":[{"name":"Lawrence Berkeley National Laboratory , , , ,","place":["Berkeley, California, United States, 94720"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,13]]},"reference":[{"issue":"8","key":"2026090104493922800_cit1","doi-asserted-by":"publisher","first-page":"2293","DOI":"10.1039\/C7CS00443E","article-title":"Extraterrestrial prebiotic molecules: photochemistry\nvs. radiation chemistry of interstellar ices","volume":"48","author":"Arumainayagam","year":"2019","journal-title":"Chem. 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Chem."},{"issue":"1","key":"2026090104493922800_cit47","doi-asserted-by":"publisher","DOI":"10.1088\/0004-637X\/727\/1\/27","article-title":"Laboratory\nStudies on the Formation of Formic Acid (HCOOH) in Interstellar and\nCometary Ices","volume":"727","author":"Bennett","year":"2011","journal-title":"Astrophys. J."},{"issue":"9","key":"2026090104493922800_cit48","doi-asserted-by":"publisher","first-page":"1974","DOI":"10.1021\/acsearthspacechem.9b00168","article-title":"Formation\nof Formic Acid, Formaldehyde,\nand Carbon Dioxide by Electron-Induced Chemistry in Ices of Water\nand Carbon Monoxide","volume":"3","author":"Schmidt","year":"2019","journal-title":"AcsACS Earth Space Chem."},{"issue":"12","key":"2026090104493922800_cit49","doi-asserted-by":"publisher","first-page":"1410","DOI":"10.1515\/zna-1979-1205","article-title":"Rate Coefficients and Product Ion Distributions for\nReactions of CO2.CO2+ Ions with Neutral\nMolecules at 300-K","volume":"34","author":"Rakshit","year":"1979","journal-title":"Z. Nat. 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Lett."},{"issue":"18","key":"2026090104493922800_cit52","doi-asserted-by":"publisher","DOI":"10.1002\/cphc.202500282","article-title":"UV-Vis Spectra of Carbonic\nAcid: Rationalizing Experimental Redshifts between Monomer and Bulk\nbased on (H2CO3)n Calculations","volume":"26","author":"Dinu","year":"2025","journal-title":"ChemPhysChem"},{"issue":"22","key":"2026090104493922800_cit53","doi-asserted-by":"publisher","first-page":"4743","DOI":"10.1021\/acs.jpca.9b03823","article-title":"Activation\nof CO2 in Photoirradiated CO2-H2O\nClusters: Direct Ab Initio Molecular Dynamics (MD) Study","volume":"123","author":"Tachikawa","year":"2019","journal-title":"J. Phys. Chem. A"},{"key":"2026090104493922800_cit54","first-page":"793","article-title":"Carbonic\nacid production in H2O:CO2 ices. UV photolysis\nvs. proton bombardment","volume":"357","author":"Gerakines","year":"2000","journal-title":"Astron. Astrophys."}],"container-title":["Journal of the American\nChemical Society"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/pubs.acs.org\/doi\/pdf\/10.1021\/jacs.6c07627","content-type":"application\/pdf","content-version":"vor","intended-application":"unspecified"},{"URL":"https:\/\/pubs.acs.org\/jacsat\/article-pdf\/148\/33\/35681\/66538039\/jacs.6c07627.pdf","content-type":"application\/pdf","content-version":"vor","intended-application":"syndication"},{"URL":"https:\/\/pubs.acs.org\/jacsat\/article-pdf\/148\/33\/35681\/66538039\/jacs.6c07627.pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2026,9,1]],"date-time":"2026-09-01T08:49:57Z","timestamp":1788252597000},"score":1,"resource":{"primary":{"URL":"https:\/\/pubs.acs.org\/jacsat\/article\/148\/33\/35681\/5254960\/Ionization-Driven-Oxygen-Oxygen-Bond-Formation-in"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2026,8,13]]},"references-count":54,"journal-issue":{"issue":"33","published-online":{"date-parts":[[2026,8,13]]},"published-print":{"date-parts":[[2026,8,26]]}},"URL":"https:\/\/doi.org\/10.1021\/jacs.6c07627","relation":{},"ISSN":["0002-7863","1520-5126"],"issn-type":[{"value":"0002-7863","type":"print"},{"value":"1520-5126","type":"electronic"}],"subject":[],"published":{"date-parts":[[2026,8,13]]}}}