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Here, we demonstrate a facile one\u2010pot synthesis of laminated 2D coordination polymer films comprising bis(terpyridine)iron and cobalt at a water\/dichloromethane interface. Cross\u2010sectional elemental mapping unveiled the stratum\u2010like structure of the film and revealed that the second layer grows to the dichloromethane side below the first layer. Cyclic voltammetry clarified that the bottom layer mediates charge transfer between the top layer and the substrate in a narrow potential region of mixed\u2010valence states. Furthermore, the bilayer film sandwiched by electrodes in a dry condition shows stable rectification character, and the barrier voltage corresponds to the redox potential difference between the two layers. This study introduces a new strategy for polymer design to explore the materials science of molecular 2D materials.<\/jats:p>","DOI":"10.1002\/chem.202201316","type":"journal-article","created":{"date-parts":[[2022,6,13]],"date-time":"2022-06-13T07:11:24Z","timestamp":1655104284000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Chemically Laminated 2D Bis(terpyridine)metal Polymer Films: Formation Mechanism at the Liquid\u2013Liquid Interface and Redox Rectification"],"prefix":"10.1002","volume":"28","author":[{"given":"Joe","family":"Komeda","sequence":"first","affiliation":[{"name":"Research Institute for Science and Technology Tokyo University of Science  2641 Yamazaki Noda Chiba 278-8510 Japan"},{"name":"Department of Chemistry School of Science The University of Tokyo  7-3-1, Hongo, Bunkyo-ku Tokyo 113-0033 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Kenji","family":"Takada","sequence":"additional","affiliation":[{"name":"Research Institute for Science and Technology Tokyo University of Science  2641 Yamazaki Noda Chiba 278-8510 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hiroaki","family":"Maeda","sequence":"additional","affiliation":[{"name":"Research Institute for Science and Technology Tokyo University of Science  2641 Yamazaki Noda Chiba 278-8510 Japan"},{"name":"Department of Chemistry School of Science The University of Tokyo  7-3-1, Hongo, Bunkyo-ku Tokyo 113-0033 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Naoya","family":"Fukui","sequence":"additional","affiliation":[{"name":"Research Institute for Science and Technology Tokyo University of Science  2641 Yamazaki Noda Chiba 278-8510 Japan"},{"name":"Department of Chemistry School of Science The University of Tokyo  7-3-1, Hongo, Bunkyo-ku Tokyo 113-0033 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Takuya","family":"Tsuji","sequence":"additional","affiliation":[{"name":"Department of Chemistry School of Science The University of Tokyo  7-3-1, Hongo, Bunkyo-ku Tokyo 113-0033 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6568-5640","authenticated-orcid":false,"given":"Hiroshi","family":"Nishihara","sequence":"additional","affiliation":[{"name":"Research Institute for Science and Technology Tokyo University of Science  2641 Yamazaki Noda Chiba 278-8510 Japan"},{"name":"Department of Chemistry School of Science The University of Tokyo  7-3-1, Hongo, Bunkyo-ku Tokyo 113-0033 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2022,7,4]]},"reference":[{"key":"e_1_2_8_1_1","doi-asserted-by":"publisher","DOI":"10.1039\/C7CS00811B"},{"key":"e_1_2_8_2_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.201103241"},{"key":"e_1_2_8_3_1","doi-asserted-by":"publisher","DOI":"10.1021\/ja312380b"},{"key":"e_1_2_8_4_1","doi-asserted-by":"publisher","DOI":"10.1039\/C7CC00810D"},{"key":"e_1_2_8_5_1","doi-asserted-by":"publisher","DOI":"10.1039\/D0CS01160F"},{"key":"e_1_2_8_6_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201100669"},{"key":"e_1_2_8_6_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.201100669"},{"key":"e_1_2_8_7_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemrev.8b00056"},{"key":"e_1_2_8_8_1","doi-asserted-by":"publisher","DOI":"10.1246\/bcsj.20200391"},{"key":"e_1_2_8_9_1","doi-asserted-by":"publisher","DOI":"10.1126\/science.aav4450"},{"key":"e_1_2_8_10_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41586-018-0631-z"},{"key":"e_1_2_8_11_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.201104497"},{"key":"e_1_2_8_12_1","doi-asserted-by":"publisher","DOI":"10.1021\/nl404795z"},{"key":"e_1_2_8_13_1","first-page":"3055","volume":"20","author":"Wu Z.","year":"2021","journal-title":"Nat. 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