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To this end, a new, highly reactive phosphorus oxonitride imide precursor compound was prepared and treated at 12\u2005GPa and 750\u2009\u00b0C by using a multianvil assembly. H<jats:sub>3<\/jats:sub>P<jats:sub>8<\/jats:sub>O<jats:sub>8<\/jats:sub>N<jats:sub>9<\/jats:sub> was obtained as a colorless, microcrystalline solid. The crystal structure of H<jats:sub>3<\/jats:sub>P<jats:sub>8<\/jats:sub>O<jats:sub>8<\/jats:sub>N<jats:sub>9<\/jats:sub> was solved ab initio by powder X\u2010ray diffraction analysis, applying the charge\u2010flipping algorithm, and refined by the Rietveld method (<jats:italic>C<\/jats:italic>2\/<jats:italic>c<\/jats:italic> (no. 15), <jats:italic>a<\/jats:italic>=1352.11(7), <jats:italic>b<\/jats:italic>=479.83(3), <jats:italic>c<\/jats:italic>=1820.42(9)\u2005pm, <jats:italic>\u03b2<\/jats:italic>=96.955(4)\u00b0, <jats:italic>Z<\/jats:italic>=4). H<jats:sub>3<\/jats:sub>P<jats:sub>8<\/jats:sub>O<jats:sub>8<\/jats:sub>N<jats:sub>9<\/jats:sub> exhibits a highly condensed (<jats:italic>\u03ba<\/jats:italic>=0.47), 3D, but interrupted network that is composed of all\u2010side vertex\u2010sharing (Q<jats:sup>4<\/jats:sup>) and only threefold\u2010linking (Q<jats:sup>3<\/jats:sup>) P(O,N)<jats:sub>4<\/jats:sub> tetrahedra in a Q<jats:sup>4<\/jats:sup>\/Q<jats:sup>3<\/jats:sup> ratio of 3:1. The structure, which includes 4\u2010ring assemblies as the smallest ring size, can be subdivided into alternating open\u2010branched zweier double layers {oB,<jats:styled-content>${2{{2\\hfill \\atop \\infty \\hfill}}}$<jats:inline-graphic xmlns:xlink=\"http:\/\/www.w3.org\/1999\/xlink\" xlink:href=\"graphic\/tex2gif-ueqn-1.gif\" xlink:title=\"equation image\"\/><\/jats:styled-content>}[<jats:sup>2<\/jats:sup>P<jats:sub>3<\/jats:sub>(O,N)<jats:sub>7<\/jats:sub>] and layers containing pairwise\u2010linked Q<jats:sup>3<\/jats:sup> tetrahedra parallel (001). Information on the hydrogen atoms in H<jats:sub>3<\/jats:sub>P<jats:sub>8<\/jats:sub>O<jats:sub>8<\/jats:sub>N<jats:sub>9<\/jats:sub> was obtained by 1D <jats:sup>1<\/jats:sup>H\u2005MAS, 2D homo\u2010 and heteronuclear (together with <jats:sup>31<\/jats:sup>P) correlation NMR spectroscopy, and a <jats:sup>1<\/jats:sup>H spin\u2010diffusion experiment with a hard\u2010pulse sequence designed for selective excitation of a single peak. Two hydrogen sites with a multiplicity ratio of 2:1 were identified and thus the formula of H<jats:sub>3<\/jats:sub>P<jats:sub>8<\/jats:sub>O<jats:sub>8<\/jats:sub>N<jats:sub>9<\/jats:sub> was unambiguously determined. The protons were assigned to Wyckoff positions 8<jats:italic>f<\/jats:italic> and 4<jats:italic>e<\/jats:italic>, the latter located within the Q<jats:sup>3<\/jats:sup> tetrahedra layers.<\/jats:p>","DOI":"10.1002\/chem.201103010","type":"journal-article","created":{"date-parts":[[2012,2,28]],"date-time":"2012-02-28T09:39:46Z","timestamp":1330421986000},"page":"4358-4366","source":"Crossref","is-referenced-by-count":4,"title":["High\u2010Pressure Synthesis and Structural Investigation of H<sub>3<\/sub>P<sub>8<\/sub>O<sub>8<\/sub>N<sub>9<\/sub>: A New Phosphorus(V) Oxonitride Imide with an Interrupted Framework Structure"],"prefix":"10.1002","volume":"18","author":[{"given":"Stefan J.","family":"Sedlmaier","sequence":"first","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Vinicius R.","family":"Celinski","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"J\u00f6rn","family":"Schmedt\u2005auf\u2005der\u2005G\u00fcnne","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Wolfgang","family":"Schnick","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2012,2,28]]},"reference":[{"key":"e_1_2_6_1_2","first-page":"469","volume":"29","author":"Beall G. 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