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Reaction of CuX₂ (X = NO₃, Cl, (SO₄)_1/2) salts and Hpymo·HX (Hpymo = 2-hydroxypyrimidine; X = Cl, NO₃) in aqueous amine solutions (amine = NH₃, CH₃NH₂) leads to formation of the poorly crystalline three-dimensional open-framework coordination polymer [Cu(pymo-N1,N3)₂]_∞ (1). Under the same reaction conditions, but in the presence of amine and group 1 metal salts of single charged voluminous anions, highly crystalline clathrates of the type {[Cu(pymo-N1,N3)₂]·(AX)_1/3}_∞ (1·AX with A = NH₄, CH₃NH₃, Li, K, Rb; X = ClO₄, BF₄, PF₆) are obtained. The X-ray crystal structure of 1·NH₄ClO₄ reveals that the combination of square-planar Cu²⁺ ion with 120° bond angles provided by Hpymo generates a three-dimensional porous [Cu(pymo-N1,N3)₂]_∞ framework with ammonium and perchlorate ions and water molecules included in the pores. 1 possesses a rich host−guest chemistry. Indeed, N₂ sorption at …