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Herein, we report a new acylamide ligand and its application in the construction of a metal–organic framework. The resultant acylamide metal–organic framework, namely [Zn2(L)(OH)(btc)]n (1, L = N1,N4-bis(pyridin-3-ylmethyl) naphthalene-1,4-dicarboxamide, H3btc = benzene-1,3,5-tricarboxylic acid), was obtained by hydrothermal synthesis. The outstanding structural feature of it is the 0D + 2D → 2D polycatenation array containing a self-catenated feature which has never previously been observed. To the best of our knowledge, the coexistence of self-catenation and polycatenation phenomena is highly exceptional.
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