The oxonitridophosphate SrP3N5O has been synthesized by heating a multicomponent reactant mixture that consisted of phosphoryl triamide OP(NH2)3, thiophosphoryl triamide SP(NH 2)3, SrS, and NH4Cl 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. SrP3N5O 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=1/2. The corrugated layers ${{{hfill 2atop hfill infty }}}${(P 3N5O)2-} consist of linked, triangular columns built up from P(O,N)4 tetrahedra with 3-rings and triply binding nitrogen atoms. The Sr2+ ions are located between the layers and exhibit six-, eight-, and ninefold coordination. FTIR and solid-state NMR spectra of SrP3N5O are discussed as well. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

SrP3N5O: A Highly Condensed Layer Phosphate Structure Solved from a Nanocrystal by Automated Electron Diffraction Tomography

MUGNAIOLI, E.;
2011-01-01

Abstract

The oxonitridophosphate SrP3N5O has been synthesized by heating a multicomponent reactant mixture that consisted of phosphoryl triamide OP(NH2)3, thiophosphoryl triamide SP(NH 2)3, SrS, and NH4Cl 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. SrP3N5O 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=1/2. The corrugated layers ${{{hfill 2atop hfill infty }}}${(P 3N5O)2-} consist of linked, triangular columns built up from P(O,N)4 tetrahedra with 3-rings and triply binding nitrogen atoms. The Sr2+ ions are located between the layers and exhibit six-, eight-, and ninefold coordination. FTIR and solid-state NMR spectra of SrP3N5O are discussed as well. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
2011
Sedlmaier, S. J.; Mugnaioli, E.; Oeckler, O.; Kolb, U.; Schnick, W.
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11568/1131346
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