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On-surface synthesis (OSS) involving relatively high energy barriers remainschallenging due to a typical dilemma: firm molecular anchor is required toprevent molecular desorption upon the reaction, whereas sufficient lateralmobility is crucial for subsequent coupling and assembly. By locking themolecular precursors on the substrate then unlocking them during the reaction,we present a strategy to address this challenge. High-yield synthesis based onwell-defined decarboxylation, intermediate transition and hexamerization isdemonstrated, resulting in an extended and ordered network exclusively composedof the newly-synthesized macrocyclic compound. Thanks to the steric hindranceof its maleimide group, we attain a preferential selection of the coupling.This work unlocks a promising path to enrich the reaction types and improve thecoupling selectivity hence the structual homogeneity of the final product forOSS.

On-Surface Decarboxylation Coupling Facilitated by Lock-to-Unlock Variation of Molecules upon the Reaction