Abstract

Single crystalline γ'-Fe 4N is obtained by chemical transport from iron over [Fe(NH 3) 6]I 2 in supercritical ammonia ( p( NH 3) = 6–8 kbar, 460 °C ⩽ T ⩽ 580 °C. X-ray structure determination gave the following results: a = 3.790(1) A ̊ , Fm3m, Z = 1, Z( F o 2) ⩾ 3 σ ( F o 2) = 59, R = 0.016. Nitrogen is distributed statistically. The minimum R-value is obtained with the scattering factors for elemental iron and nitrogen. At 580 °C the autoclave material is attacked and crystals of Fe 3NiN with a = 3.781(1) A ̊ are also formed.

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