Department Chemie, Ludwig-Maximilians-Universität, Butenandtstrasse 5-13 (D), 81377 München, Germany.
Chemistry. 2011 Sep 26;17(40):11258-65. doi: 10.1002/chem.201101545. Epub 2011 Aug 23.
The oxonitridophosphate SrP(3)N(5)O has been synthesized by heating a multicomponent reactant mixture that consisted of phosphoryl triamide OP(NH(2))(3), thiophosphoryl triamide SP(NH(2))(3), SrS, and NH(4)Cl enclosed in evacuated and sealed silica-glass ampoules up to 750 °C. The compound was obtained as nanocrystalline powder with needle-shaped crystallites. The crystal structure was solved ab initio on the basis of electron diffraction data by means of automated electron diffraction tomography (ADT) and verified by Rietveld refinement with X-ray powder diffraction data. SrP(3)N(5)O crystallizes in the orthorhombic space group Pnma (no. 62) with unit-cell data of a=18.331(2), b=8.086(1), c=13.851(1) Å and Z=16. The compound is a highly condensed layer phosphate with a degree of condensation κ=½. The corrugated layers (∞)(2){(P(3)N(5)O)(2-)} consist of linked, triangular columns built up from P(O,N)(4) tetrahedra with 3-rings and triply binding nitrogen atoms. The Sr(2+) ions are located between the layers and exhibit six-, eight-, and ninefold coordination. FTIR and solid-state NMR spectra of SrP(3)N(5)O are discussed as well.
氧氮磷硫化锶 SrP(3)N(5)O 通过加热多组分反应物混合物合成，反应物混合物由三磷酰胺 OP(NH(2))(3)、硫代磷酰胺 SP(NH(2))(3)、SrS 和 NH(4)Cl 组成，封存在抽空密封的硅玻璃安瓿中，加热至 750°C。得到的化合物为纳米晶粉末，具有针状晶体。晶体结构通过基于电子衍射数据的自动电子衍射层析 (ADT) 从头计算得到解决，并通过 X 射线粉末衍射数据的 Rietveld 精修得到验证。SrP(3)N(5)O 属于正交晶系 Pnma(no.62)空间群，具有晶胞参数 a=18.331(2)、b=8.086(1)、c=13.851(1)Å 和 Z=16。该化合物是一种高度缩合的层状磷酸盐，缩合度 κ=½。波纹状的层（∞）(2){(P(3)N(5)O)(2-)}由连接的三角形柱组成，这些三角形柱由具有 3 元环和三重配位氮原子的 P(O,N)(4)四面体构成。Sr(2+)离子位于层之间，呈现六、八和九配位。还讨论了 SrP(3)N(5)O 的 FTIR 和固态 NMR 谱。
