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Guided by a second‐sphere interaction strategy, we fabricated a Tb(III)‐based metal—organic framework (MMCF‐4) for turn‐on sensing of methyl amine with ultra‐low detection limit and high turn‐on efficiency. MMCF‐4 features lanthanide nodes shielded in a nonacoordinate geometry along with secondary coordination spheres that are densely populated with H‐bond interacting sites. Nonradiative routes were...