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Zirconium‐containing metal‐organic framework (MOF) with UiO‐66 topology is an extremely versatile material, which finds applications beyond gas separation and catalysis. However, after more than 10 years after the first reports introducing this MOF, understanding of the molecular‐level mechanism of its nucleation and growth is still lacking. By means of in situ time‐resolved high‐resolution mass spectrometry,...