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However, questions persist regarding the involvement of CO in ketene formation, and the impact of this elusive oxygenate intermediate on reactivity patterns. Using operando photoelectron photoion coincidence spectroscopy (PEPICO), we investigate the role of CO in methyl chloride conversion to hydrocarbons (MCTH), a prospective process for methane valorization with a reaction network akin to methanol to hydrocarbons (MTH) but without oxygenate intermediates. Our findings reveal the transformative role of CO in MCTH at the low pressures, inducing ketene formation in MCTH and boosting olefin production, confirming the Koch carbonylation step in the initial stages of C1 coupling. We uncover pressure\u2010dependent product distributions driven by CO\u2010induced ketene formation, and its subsequent desorption from the zeolite surface, which is enhanced at low pressure. Inspired by the above results, extension of the co\u2010feeding approach to CH<jats:sub>3<\/jats:sub>OH as another simple oxygenate showcases the additional potential for improved catalyst stability in MCTH at ambient pressure.<\/jats:p>","DOI":"10.1002\/anie.202401060","type":"journal-article","created":{"date-parts":[[2024,3,7]],"date-time":"2024-03-07T16:39:31Z","timestamp":1709829571000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["CO Cofeeding Affects Product Distribution in CH<sub>3<\/sub>Cl Coupling over ZSM\u20105 Zeolite: Pressure Twists the Plot"],"prefix":"10.1002","volume":"63","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-5106-2656","authenticated-orcid":false,"given":"Zihao","family":"Zhang","sequence":"first","affiliation":[{"name":"Paul Scherrer Institute  5232 Villigen Switzerland"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3657-9638","authenticated-orcid":false,"given":"Matteo","family":"Vanni","sequence":"additional","affiliation":[{"name":"Institute for Chemical and Bioengineering Department of Chemistry and Applied Biosciences ETH Zurich  Vladimir-Prelog-Weg 1 8093 Zurich Switzerland"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8515-3302","authenticated-orcid":false,"given":"Xiangkun","family":"Wu","sequence":"additional","affiliation":[{"name":"Paul Scherrer Institute  5232 Villigen Switzerland"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1251-4549","authenticated-orcid":false,"given":"Patrick","family":"Hemberger","sequence":"additional","affiliation":[{"name":"Paul Scherrer Institute  5232 Villigen Switzerland"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2742-1051","authenticated-orcid":false,"given":"Andras","family":"Bodi","sequence":"additional","affiliation":[{"name":"Paul Scherrer Institute  5232 Villigen Switzerland"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3933-2913","authenticated-orcid":false,"given":"Sharon","family":"Mitchell","sequence":"additional","affiliation":[{"name":"Institute for Chemical and Bioengineering Department of Chemistry and Applied Biosciences ETH Zurich  Vladimir-Prelog-Weg 1 8093 Zurich Switzerland"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5805-7355","authenticated-orcid":false,"given":"Javier","family":"P\u00e9rez\u2010Ram\u00edrez","sequence":"additional","affiliation":[{"name":"Institute for Chemical and Bioengineering Department of Chemistry and Applied Biosciences ETH Zurich  Vladimir-Prelog-Weg 1 8093 Zurich Switzerland"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2024,3,22]]},"reference":[{"key":"e_1_2_3_1_1","unstructured":"\u00a0"},{"key":"e_1_2_3_2_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.202107553"},{"key":"e_1_2_3_3_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202303124"},{"key":"e_1_2_3_4_2","doi-asserted-by":"crossref","unstructured":"S. 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