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CO 2 insertion into tri(μ-hydrido)triiron(II) clusters ligated by a tris(β-diketiminate) cyclophane is demonstrated to be balanced by sterics for CO 2 approach and hydride accessibility. Time-resolved NMR and UV-vis spectra for this reaction for a complex in which methoxy groups border the pocket of the hydride donor (Fe 3 H 3  L   2  , 4 ) result in a decreased activation barrier and increased kinetic isotope effect consistent with the reduced sterics. For the ethyl congener Fe 3 H 3  L   1  ( 2 ), no correlation is found between rate and reaction solvent or added Lewis acids, implying CO 2 coordination to an Fe center in the mechanism. The estimated hydricity (50 kcal/mol) based on observed H/D exchange with BD 3 requires Fe-O bond formation in the product to offset an endergonic CO 2 insertion. μ 3 -hydride coordination is noted to lower the activation barrier for the first CO 2 insertion event in DFT calculations.

inorganic chemistry

Access to Metal Centers and Fluxional Hydride Coordination Integral for CO2 Insertion into [Fe3(μ-H)3]3+ Clusters