Study of Ammonolysis Reactions within SituX-Ray Diffraction: Detection and Crystal Structure of Li0.84W1.16N2

The new ternary nitride Li0.84W1.16N2was found by anin situX-ray diffraction study of the ammonolysis of a LiF–WO3mixture. The ammonolysis proceeds via Li6W2O9to LiWN2, which subsequently decomposes at 900°C to form Li0.84W1.16N2. For a larger scale synthesis of Li0.84W1.16N2, the ammonolysis of a mixture of Li2CO3and WO3was performed at 900°C. Li0.84W1.16N2crystallizes in the anti-TiP type structure with the space groupP63/mmcanda=2.8809(1) Å,c=10.3456(4) Å, andZ=2 as determined from simultaneous Rietveld refinement of X-ray and neutron powder diffraction data. The refinement converged withR(F2)=7.0% for the X-ray data and 8.3% for the neutron data with a total reducedχ2=3.54. The structure consists of alternating layers of WN6trigonal prisms andMN6octahedra (M=W, Li), with distancesW–N=2.11 Å.