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.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.