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The resulting hydrogen isocyanide complexes [Mo(CNH)<jats:sub>8<\/jats:sub>]<jats:sup>4+<\/jats:sup> [SbF<jats:sub>6<\/jats:sub>]<jats:sup>\u2212<\/jats:sup><jats:sub>4<\/jats:sub> and [W(CNH)<jats:sub>8<\/jats:sub>]<jats:sup>4+<\/jats:sup> [SbF<jats:sub>6<\/jats:sub>]<jats:sup>\u2212<\/jats:sup><jats:sub>4<\/jats:sub> are the first examples of eight\u2010coordinate homoleptic metal complexes containing hydrogen isocyanide (CNH) ligands. The complexes were crystallographically characterized, revealing hydrogen\u2010bonded networks with short N\u22c5\u22c5\u22c5H\u22c5\u22c5\u22c5F contacts. Low\u2010temperature NMR measurements in HF confirmed rapid proton exchange even at \u221240\u2009\u00b0C. Upon protonation, \u03bd(C\u2261N) increases of about 50\u2005cm<jats:sup>\u22121<\/jats:sup> which is in agreement with DFT calculations.<\/jats:p>","DOI":"10.1002\/anie.202002366","type":"journal-article","created":{"date-parts":[[2020,3,24]],"date-time":"2020-03-24T14:18:13Z","timestamp":1585059493000},"page":"10519-10522","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":12,"title":["Isolation and Structural Characterization of Eightfold Protonated Octacyanometalates [M(CNH)<sub>8<\/sub>]<sup>4+<\/sup> (M=Mo<sup>IV<\/sup>, W<sup>IV<\/sup>) from Superacids"],"prefix":"10.1002","volume":"59","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-0424-2261","authenticated-orcid":false,"given":"Malte","family":"Sellin","sequence":"first","affiliation":[{"name":"Freie Universit\u00e4t Berlin Institut f\u00fcr Chemie und Biochemie Anorganische Chemie  Fabeckstrasse 34\u201336 14195 Berlin Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9322-9212","authenticated-orcid":false,"given":"Val\u00e9rie","family":"Marvaud","sequence":"additional","affiliation":[{"name":"Sorbonne Universit\u00e9 IPCM-CNRS-UMR8232, cc 229  4 place Jussieu 75252 Paris Cedex 05 France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6756-2951","authenticated-orcid":false,"given":"Moritz","family":"Malischewski","sequence":"additional","affiliation":[{"name":"Freie Universit\u00e4t Berlin Institut f\u00fcr Chemie und Biochemie Anorganische Chemie  Fabeckstrasse 34\u201336 14195 Berlin Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2020,4,14]]},"reference":[{"key":"e_1_2_2_1_1","doi-asserted-by":"publisher","DOI":"10.1021\/cr00019a016"},{"key":"e_1_2_2_2_1","doi-asserted-by":"publisher","DOI":"10.1016\/S1387-7003(01)00267-2"},{"key":"e_1_2_2_3_1","doi-asserted-by":"publisher","DOI":"10.1002\/chem.201605293"},{"key":"e_1_2_2_4_1","doi-asserted-by":"publisher","DOI":"10.1039\/C7CC09401A"},{"key":"e_1_2_2_5_1","doi-asserted-by":"publisher","DOI":"10.1039\/c39880000730"},{"key":"e_1_2_2_6_1","doi-asserted-by":"publisher","DOI":"10.1107\/S0567740871005922"},{"key":"e_1_2_2_7_1","doi-asserted-by":"publisher","DOI":"10.1080\/00958977308072992"},{"key":"e_1_2_2_8_1","doi-asserted-by":"publisher","DOI":"10.1107\/S0567740875006309"},{"key":"e_1_2_2_9_1","doi-asserted-by":"publisher","DOI":"10.1039\/C39930001388"},{"key":"e_1_2_2_10_1","doi-asserted-by":"publisher","DOI":"10.1016\/S0010-8545(00)80247-7"},{"key":"e_1_2_2_11_1","doi-asserted-by":"publisher","DOI":"10.1039\/C6DT01301E"},{"key":"e_1_2_2_12_1","doi-asserted-by":"publisher","DOI":"10.1002\/zaac.201700220"},{"key":"e_1_2_2_13_1","doi-asserted-by":"publisher","DOI":"10.1002\/slct.201600399"},{"key":"e_1_2_2_14_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201608795"},{"key":"e_1_2_2_14_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.201608795"},{"key":"e_1_2_2_15_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201708552"},{"key":"e_1_2_2_15_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.201708552"},{"key":"e_1_2_2_16_1","first-page":"493","volume":"34","author":"Chilesotti A.","year":"1905","journal-title":"Gazz. 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