Reversible solvent-triggered single-crystal-to-single-crystal (SCSC) transformations are observed between two copper(II) azamacrocyclic complexes: [Cu(C16H38N6)(H2O)2](C12H6O4) (1) and [Cu(C16H38N6)(C12H6O4)] (2). Complex (1) was prepared via self-assembly of a copper(II) azamacrocyclic complex containing butyl pendant groups, [Cu(C16H38N6)(ClO4)2], with 2,7-naphthalenedicarboxylic acid. When monomeric compound (1) was immersed in CH3OH, coordination polymer (2) was obtained, indicating a solvent-triggered SCSC transformation. Furthermore, when (2) was immersed in water, an reverse SCSC transformation from (2) to (1) occurred. Complex (1) presents a 3D supramolecular structure formed via intermolecular hydrogen-bonding interactions, whereas complex (2) features a 1D zigzag coordination polymer. The reversible SCSC transformation of (1) and (2) was characterized using single-crystal X-ray diffraction and in situ powder X-ray diffraction techniques. Despite its poor porosity, complex (2) displayed interesting CO2 adsorption behaviour under CO2 gas.
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