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Solvothermal reaction in N,N‐dimethylformamide (DMF) between 1,6‐bis(1‐imidazolyl)‐2,4‐hexadiyne monohydrate (L1⋅H2O), isophthalic acid (H2L2), and Zn(NO3)2⋅6 H2O gives the diacetylene‐based mixed‐ligand coordination polymer {[Zn(L1)(L2)](DMF)2}n (UMON‐44) in 38 % yield. Combination of DSC with variable‐temperature single‐crystal X‐ray diffraction revealed the occurrence of two phase transitions spanning...
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