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RESEARCH PRODUCT

Ba 6 P 12 N 17 O 9 Br 3 – A Column‐Type Phosphate Structure Solved from Single‐Nanocrystal Data Obtained by Automated Electron Diffraction Tomography

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Oxonitridophosphate Ba6P12N17O9Br3 was synthesized by heating a multicomponent mixture of BaBr2, BaS, phosphoryl triamide and thiophosphoryl triamide in an evacuated and sealed silica-glass ampoule to 750 °C. Ba6P12N17O9Br3 was obtained as the main product as a nanocrystalline powder. The crystal structure was determined ab initio on the basis of electron diffraction data acquired from a single needle-shaped nanocrystal by automated diffraction tomography. Ba6P12N17O9Br3 crystallizes in the hexagonal space group P63/m (no. 176) with unit cell parameters a = 14.654(19), c = 8.255(9) A and Z = 2. Its structure includes triangular, column-shaped anions of ∞1{(P12N17O9)9–}, which are built from vertex-sharing P(O,N)4 tetrahedra with 3-rings and three-coordinate nitrogen atoms. The 1D anions are separated by Ba2+ and Br– ions, which are arranged in channels parallel to the phosphate anions along [001]. The Ba2+ ions are eight- and nine-coordinated by Br– and O/N atoms, respectively.