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Here, we report the synthesis of two giant dendritic PPs fulfilling this criteria with 366 and 546 carbon atoms by applying a \u201clayer\u2010by\u2010layer\u201d extension strategy. Although our initial attempts on their cyclodehydrogenation toward the corresponding NGs in solution were unsuccessful, we achieved their deposition on metal substrates under ultrahigh vacuum through the electrospray technique. Scanning probe microscopy imaging provides valuable information on the possible thermally induced partial planarization of such giant dendritic PPs on a metal surface.<\/jats:p>","DOI":"10.1002\/asia.202200220","type":"journal-article","created":{"date-parts":[[2022,4,5]],"date-time":"2022-04-05T04:08:09Z","timestamp":1649131689000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["Synthesis of Giant Dendritic Polyphenylenes with 366\u2009and 546 Carbon Atoms and Their High\u2010vacuum Electrospray Deposition"],"prefix":"10.1002","volume":"17","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-1949-1124","authenticated-orcid":false,"given":"Ian Cheng\u2010Yi","family":"Hou","sequence":"first","affiliation":[{"name":"Synthetic Chemistry Max Planck Institute for Polymer Research  Ackermannweg 10 D-55128 Mainz Germany"},{"name":"Department of Chemistry Johannes Gutenberg University Mainz  Duesbergweg 10\u201314 D-55128 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