A simultaneous reduction of copper(II) to copper(I) by pyridinecarboxylate and the substitution of carboxylato groups by iodo nucleophiles in a self-assembly process under hydrothermal conditions afforded a new iodine-inclusion coordination polymer [CuI(C(5)H(3)NI(2)).(1)/(2)I(2)]. The synthetic studies of the substitution process produced a new supramolecular compound [IC(5)H(3)NCOOH] 2 and revealed that the catalytic properties of copper ions in redox and substitution reactions under hydrothermal conditions are attractive, Crystal data for [CuI(C(5)H(3)NI(2)).(1)/(2)I(2)]: triclinic, space group F; cell dimensions a = 4.216(1) Angstrom, b = 11.254(2) Angstrom, c = 12,196(2) Angstrom, alpha = 80.34(3)degrees, beta = 88.44(3)degrees, gamma = 83.10(3); V = 566.2(2) Angstrom(3), Z = 2. Crystal data for [IC(5)H(3)NCOOH]: monoclinic, space group P2(1)/c, cell dimensions a = 5.041(1) Angstrom, b = 17.313(2) Angstrom, c = 8,639(1) Angstrom, beta = 95.042(2)degrees; V = 751.02(13) Angstrom(3), Z = 4.
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