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The growth and sustainable development of humanity is heavily dependent upon N<sub>2</sub> fixation. Herein we discover ambient catalyst-free disproportionation of N<sub>2</sub> by water plasma which occurs <i>via</i> the distinctive HONH-HNOH<sup>+</sup><sup>•</sup> intermediate to yield economically valuable nitroxyl (HNO) and hydroxylamine (NH<sub>2</sub>OH) products. Calculations suggest that the reaction is prompted by the coordination of electronically excited N<sub>2</sub> with water dimer radical cation, (H<sub>2</sub>O)<sub>2</sub><sup>+</sup><sup>•</sup>, in its two-center-three-electron configuration. The reaction products are collected in a 76-needle array discharge reactor with product yields of 1.14 μg cm<sup>–2 </sup>h<sup>–1</sup> for NH<sub>2</sub>OH and 0.37 μg cm<sup>–2 </sup>h<sup>–1</sup> for HNO. Potential applications of these compounds are demonstrated to make ammonia (for NH<sub>2</sub>OH), as well as to chemically react and convert cysteine, and serve as a neuroprotective agent (for HNO). The conversion of N<sub>2</sub> into HNO and NH<sub>2</sub>OH by water plasma could offer great profitability and reduction of polluting emissions, thus giving an entirely look and perspectives to the problem of green N<sub>2</sub> fixation.
