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The anionic [(VO<jats:sub>2<\/jats:sub>)<jats:sub>4<\/jats:sub>(PO<jats:sub>4<\/jats:sub>)<jats:sub>2<\/jats:sub>]<jats:sub><jats:italic>n<\/jats:italic><\/jats:sub><jats:sup><jats:italic>2n\u2212<\/jats:italic><\/jats:sup> perforated layers are strongly hydrogen bonded to the interlayer 4,4\u2032\u2010bipyridinium cations and are assembled by an unprecedented secondary tetrametallic V<jats:sup>V<\/jats:sup> building unit constructed from a distorted cubane\u2010like {V<jats:sub>4<\/jats:sub>O<jats:sub>4<\/jats:sub>} cluster. The compound was further characterised by IR, Raman, <jats:sup>1<\/jats:sup>H, <jats:sup>1<\/jats:sup>H\u2010<jats:sup>13<\/jats:sup>C, <jats:sup>31<\/jats:sup>P and <jats:sup>51<\/jats:sup>V MAS NMR spectroscopy, and by thermal and elemental analysis. (\u00a9 Wiley\u2010VCH Verlag GmbH &amp; Co. 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