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Single phase Li 5 NBr 2  was prepared by the reaction of Li 3 N and dry, OH-free LiBr under inert gas at 430 °C. In the quasi-binary system Li 3-2x N 1-x Br x , Li 5 NBr 2  is the second most nitride rich compound after Li 10 N 3 Br. Following unit cell indexing using laboratory X-ray powder data the previously unknown structure of Li 5 NBr 2  was solved from neutron powder diffraction data recorded at the flat-cone and powder diffractometer E2 at the rebuilt reactor BER II  in Berlin. The title compound crystallizes in the orthorhombic space group Immm (No. 71), a = 603.79(4), b = 1181.3(1), c = 390.14(3) pm with two formula units per unit cell. The L i-N -sublattice comprises linear chains of vertex sharing Li 6 N-octahedra which are aligned along the short c-axis and are separated by chains of bromine atoms. The N-Br arrangement may be regarded as an ordered AX 2  variant of a cubic close packing involving two kinds of atoms. Lithium atoms occupy the tetrahedral holes formed by one nitrogen and three bromine atoms, as well as the N - N edges of the N 2 Br 2  tetrahedra.

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Reindarstellung und Kristallstruktur von Lithiumnitriddibromid, Li 5 NBr 2  / Preparation and Crystal Structure of Lithium Nitride Dibromide, Li 5 NBr 2