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Addition of 2,2′-bipyridine (bipy) to [Ni(NO)(bipy)][PF₆] (1) results in formation of a rare five-coordinate nickel nitrosyl [Ni(NO)(bipy)₂][PF₆] (2). This complex exhibits a bent NO^– ligand in the solid state. On standing in acetonitrile, 2 furnishes the NO coupled product, [Ni(κ²-O₂N₂)(bipy)] (8) in moderate yield. Subsequent addition of 2 equiv of acetylacetone (H(acac)) to 8 results in formation of [Ni(acac)₂(bipy)], N₂O, and H₂O. Preliminary mechanistic studies suggest that the N–N bond is formed via a bimetallic coupling reaction of two NO^– ligands.