The intermetallic ternary nitride, Ni 2 Mo 3 N, has been synthesized by the ammonolysis of a complexed mixed-metal chloride precursor. This compound crystallizes in the cubic space group P4 1 32 [213] with Z β«Ψβ¬ 4 and a lattice parameter of a β«Ψβ¬ 6.6340(2) A s , as determined from powder X-ray and neutron di4raction experiments and the Rietveld re5nement of the neutron data collected at room temperature. The re5nement converged with R wp β«Ψβ¬ 0.032, R p β«Ψβ¬ 0.025, R I β«Ψβ¬ 0.059, and 2 β«Ψβ¬ 1.48. Ni 2 Mo 3 N assumes a 5lled -manganese structure, ideally consisting of a lattice of corner-sharing Mo 6 N octahedra in a 5vemembered ring arrangement and an interpenetrating net-like lattice of nickel atoms which occupy the pentagonal holes formed by the molybdenum nitride polyhedral rings. Electrical and magnetic characterization of Ni 2 Mo 3 N indicate that it is a metallic conductor which antiferromagnetically orders at 14.7 K. Neutron di4raction conducted at 10 K suggests that the size of the magnetic unit cell matches that of the crystallographic unit cell. A version of this nitride phase which is substoichiometric in nitrogen and therefore has a smaller lattice parameter also displays antiferromagnetic ordering, but with a much higher ordering temperature of 68.7 K.