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A simple synthetic method to access a wide range of [Rh(acac)(CO)(NHC)] complexes is described. In situ infra‐red monitoring provides insights into the mechanism of the reaction, including the identification of a key intermediate. An understanding of the reaction mechanism leads to the discovery of novel pathways to commonly used congeners. [ABSTRACT FROM AUTHOR]

An operationally simple, user and eco‐friendly synthetic protocol for the synthesis of [Rh(acac)(CO)(NHC)] complexes is described. Insights into the mechanism are provided using operando spectroscopy. The spectroscopic fingerprints of these complexes are correlated to NHCs reported electron‐donating descriptor values, highlighting a new strategy to evaluate carbenes' electronic properties. An assessment of these complexes in catalytic applications is also reported, showing promising results in the catalytic hydrogenation of aromatic ketones. [ABSTRACT FROM AUTHOR]