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Two new coordination polymers have been synthesized with 2,5-furandicarboxylic acid upon base modification. The resulting structures are dependent on the base added. When KOH was used as base, potassium was incorporated into the two-dimensional coordination polymer, acting as a metallolinker to give [Pr 2 K 2 (OH) 2 (C 6 H 2 O 5 ) 3 (H 2 O) 3 ]·H 2 O (1). Synthesis with other alkali hydroxides produced a three-dimensional [a]

Two new coordination polymers have been synthesized with 2,5‐furandicarboxylic acid upon base modification. The resulting structures are dependent on the base added. When KOH was used as base, potassium was incorporated into the two‐dimensional coordination polymer, acting as a metallolinker to give [Pr2K2(OH)2(C6H2O5)3(H2O)3]·H2O (1). Synthesis with other alkali hydroxides produced a three‐dimensional metal‐organic framework, [Pr8(OH)6(C6H2O5)9(H2O)15]·3H2O (2), and the alkali metal cations were not incorporated into the structure. Hole‐size effects with bite‐angle analyses indicate that metallolinker formation depends on the cation size. The resulting compounds were characterized by single‐crystal X‐ray diffraction, powder X‐ray diffraction, elemental analysis, and thermogravimetric analysis.