Department of Chemistry, University of Munich (LMU), Butenandtstr. 5-13, 81377, München, Germany.
Chemistry. 2018 Oct 22;24(59):15889-15896. doi: 10.1002/chem.201803125. Epub 2018 Sep 24.
The (imido)nitridophosphates SrH P N and SrP N were synthesized as colorless crystals by high-pressure/high-temperature reactions using the multianvil technique (5 GPa, ca. 1075 °C). Stoichiometric amounts of Sr(N ) P N , and amorphous HPN were used as starting materials. Whereas the crystal structure of SrH P N was solved and refined from single-crystal X-ray diffraction data and confirmed by Rietveld refinement, the structure of SrP N was determined from powder diffraction data. In order to confirm the structures, H and P solid-state NMR spectroscopy and FTIR spectroscopy were carried out. The chemical composition was confirmed with EDX measurements. Both compounds show unprecedented layered network structure types, built up from all-side vertex-sharing PN tetrahedra which are structurally related. The structural comparison of both compounds gives first insights into the hitherto unknown condensation mechanism of nitridophosphates under high pressure.
(亚氨基)氮化磷酸盐 SrH P N 和 SrP N 是通过使用多砧技术(5 GPa,约 1075°C)的高温高压反应合成的无色晶体。使用化学计量比的 Sr(N ) P N 和无定形 HPN 作为起始材料。虽然 SrH P N 的晶体结构是通过单晶 X 射线衍射数据解决和精修,并通过 Rietveld 精修证实的,但 SrP N 的结构是通过粉末衍射数据确定的。为了确认结构,进行了 H 和 P 固态 NMR 光谱和 FTIR 光谱的研究。化学组成通过 EDX 测量来确认。这两种化合物都显示出前所未有的层状网络结构类型,由全顶角共享的 PN 四面体构建而成,这些四面体在结构上是相关的。对这两种化合物的结构比较首次深入了解了迄今为止未知的高压下氮化磷酸盐的缩合机制。