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Snapshot and crystallographic observations of kinetic and thermodynamic products for NO 2 S 2 macrocyclic complexes.
IUCrJ 2018 January 2
Direct observation and structural characterization of a kinetic product and a thermodynamic product for complexes with an NO2 S2 macrocycle ( L ) are reported. L reacts with copper(I) iodide to give a mononuclear complex [Cu( L )]2 (Cu2 I4 )·2CH2 Cl2 ( 1 ), featuring three separate units. When cadmium(II) iodide was reacted with L , an anion-coordinated complex [Cd( L )I]2 (Cd2 I6 )·4CH3 CN ( 2 ) with a needle-type crystal shape was formed as the kinetic product. Interestingly, when the needle-type kinetic product was left undisturbed in the mother solution it gradually transformed to the pseudo-dimer complex [Cd2 ( L )2 I2 ](Cd2 I6 ) ( 3 ) with a brick-type crystal shape as the thermodynamic product. The dissolution-recrystallization process resulted in the elimination of the lattice solvent molecules (aceto-nitrile) in 2 and the contraction of two neighboring macrocyclic complex units [Cd( L )I]+ , forming the pseudo-dimer 3 via an intermolecular Cd⋯I interaction between two monomers. For the entire process from kinetic to thermodynamic products, it was possible to obtain sequential photographic snapshots, single-crystal X-ray structures and powder X-ray diffraction patterns. For the copper(I) and cadmium(II) complexes, competitive NMR results agree with the solid-state data that show copper(I) has a higher affinity for L than does cadmium(II).
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