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Here we demonstrate that variation of the \u201cangle\u201d of the backbone of <jats:italic>C<\/jats:italic><jats:sub>3<\/jats:sub>\u2010symmetric tris\u2010bis(urea) ligands, from triphenylamine to triphenylphosphine oxide, results in the change of the final construct from an A<jats:sub>4<\/jats:sub>L<jats:sub>4<\/jats:sub> tetrahedron to a higher\u2010nuclearity, A<jats:sub>6<\/jats:sub>L<jats:sub>6<\/jats:sub> trigonal antiprism (A=anion, herein PO<jats:sub>4<\/jats:sub><jats:sup>3\u2212<\/jats:sup>; L=ligand). Most interestingly, this assembly features a huge hollow internal space that is divided into three compartments: one central cavity and two large outer pockets. This multi\u2010cavity character enables the binding of different guests, namely monosaccharides or polyethylene glycol molecules (PEG600, PEG1000 and PEG2000), respectively. The results prove that anion coordination by multiple hydrogen bonds may provide both sufficient strength and flexibility, thus making possible the formation of complicated structures with adaptive guest binding ability.<\/jats:p>","DOI":"10.1002\/anie.202301300","type":"journal-article","created":{"date-parts":[[2023,3,9]],"date-time":"2023-03-09T15:31:07Z","timestamp":1678375867000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":11,"title":["Assembly of an A<sub>6<\/sub>L<sub>6<\/sub> Anion Trigonal Antiprism and Binding of Glucopyranosides and Polyethylene Glycols (PEGs)"],"prefix":"10.1002","volume":"62","author":[{"given":"Boyang","family":"Li","sequence":"first","affiliation":[{"name":"Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of the Ministry of Education College of Chemistry and Materials Science Northwest University  Xi'an 710069 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China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Lizheng","family":"Xu","sequence":"additional","affiliation":[{"name":"Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of the Ministry of Education College of Chemistry and Materials Science Northwest University  Xi'an 710069 China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Xiao\u2010Juan","family":"Yang","sequence":"additional","affiliation":[{"name":"Key Laboratory of Medicinal Molecule Science and Pharmaceutics Engineering Ministry of Industry and Information Technology School of Chemistry and Chemical Engineering Beijing Institute of Technology  Beijing 100081 China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0724-4150","authenticated-orcid":false,"given":"Biao","family":"Wu","sequence":"additional","affiliation":[{"name":"Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of the Ministry of 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