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The triiron trihydride complex Fe 3 H 3  L ( 1 ) [where L  3- is a tris(β-diketiminate)cyclophanate] reacts with CO and with BF 3 ·OEt 2 to afford (Fe I CO) 2 Fe II (μ 3 -H) L ( 2 ) and Fe 3 F 3  L ( 3 ), respectively. Variable-temperature and applied-field Mössbauer spectroscopy support the assignment of two high-spin (HS) iron(i) centers and one HS iron(ii) ion in 2 . Preliminary studies support a CO-induced reductive elimination of H 2 from 1 , rather than CO trapping a species from an equilibrium mixture. This complex reacts with H 2 to regenerate 1 under a dihydrogen atmosphere, which represents a rare example of reversible CO/H 2 exchange and the first to occur at high-spin metal centers, as well as the first example of a reversible multielectron redox reaction at a designed high-spin metal cluster. The formation of 3 proceeds through a previously unreported net fluoride-for-hydride substitution, and 3 is surprisingly chemically inert to Si-H bonds and points to an unexpectedly large difference between the Fe-F and Fe-H bonds in this high-spin system.

chemical science

Reactivity of hydride bridges in a high-spin [Fe3(μ-H)3]3+ cluster: reversible H2/CO exchange and Fe–H/B–F bond metathesis