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It was synthesized as dark gray powder in a high\u2010pressure high\u2010temperature reaction at 800\u2009\u00b0C and 6\u2005GPa from Sn<jats:sub>3<\/jats:sub>N<jats:sub>4<\/jats:sub> and P<jats:sub>3<\/jats:sub>N<jats:sub>5<\/jats:sub>. The crystal structure was elucidated from single\u2010crystal diffraction data (space group <jats:italic>C<\/jats:italic>2\/<jats:italic>m<\/jats:italic> (no. 12), <jats:italic>a<\/jats:italic>=12.9664(4), <jats:italic>b<\/jats:italic>=10.7886(4), <jats:italic>c<\/jats:italic>=4.8238(2) \u00c5, <jats:italic>\u03b2<\/jats:italic>=109.624(1)\u00b0) and shows a 3D\u2010network of PN<jats:sub>4<\/jats:sub> tetrahedra, incorporating Sn in oxidation states +II and +IV. The Sn cations are located within eight\u2010membered rings of vertex\u2010sharing PN<jats:sub>4<\/jats:sub> tetrahedra, stacked along the [001] direction. A combination of solid\u2010state nuclear magnetic resonance spectroscopy, <jats:sup>119<\/jats:sup>Sn M\u00f6ssbauer spectroscopy and density functional theory calculations was used to confirm the mixed oxidation of Sn. Temperature\u2010dependent powder X\u2010ray diffraction measurements reveal a low thermal expansion of 3.6\u2005ppm\/K up to 750\u2009\u00b0C, beyond which Sn<jats:sub>3<\/jats:sub>P<jats:sub>8<\/jats:sub>N<jats:sub>16<\/jats:sub> starts to decompose.<\/jats:p>","DOI":"10.1002\/chem.202401428","type":"journal-article","created":{"date-parts":[[2024,5,8]],"date-time":"2024-05-08T10:59:06Z","timestamp":1715165946000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Mixed Tin Valence in the Tin(II\/IV)\u2010Nitridophosphate Sn<sub>3<\/sub>P<sub>8<\/sub>N<sub>16<\/sub>"],"prefix":"10.1002","volume":"30","author":[{"given":"Sebastian J.","family":"Ambach","sequence":"first","affiliation":[{"name":"Department of Chemistry University of Munich (LMU)  Butenandtstra\u00dfe 5\u201313 D-81377 Munich 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