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Salt metathesis of [Cp′FeI]2 [1, Cp′ = η5‐1,2,4‐(Me3C)3C5H2] and NaBH4 (2 equiv.) in tetrahydrofuran yields the low‐spin iron complex [Cp′Fe(η3‐BH4)] (2), which is thermally unstable and degrades slowly to the trimeric complex [Cp′FeBH2]3 (3) and H2. Both molecules have been fully characterized by various spectroscopic techniques. An X‐ray structure analysis of 3 confirms its nature and reveals rather...
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