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Reaction of CuX 2 ·nH 2 O (X = Cl,  n  = 2; X = Br,  n  = 0) with 2-amino-5-methylpyridine (5MAP) in acetonitrile yielded [(5MAP) 2 CuX 2 ] 2  ( 1 , Cl;  2 , Br). The compounds are isomorphous and crystallize in the monoclinic space group  P 2 1/n  as bihalide bridged dimers. Variable temperature magnetic measurements show very weak exchange in the two compounds (-2.1(1) K) which may correlate with previously proposed magnetostructural correlations for bihalide bridged Cu(II) dimers. In attempts to prepare  2  in 2-butanone as solvent, [(3-Br-2-Et-5-Mepyrpy)(CH 3 CO 2 ) 4 Cu 2 ] ( 3 ) was serendipitously isolated (3-Br-2-Et-5-Mepyrpy = 3-bromo-2-ethyl-5-methyl-7H-pyrrolido[2,3-b]pyridinium). The bicyclic ligand was synthesized  in situ  by condensation of 5MAP with the solvent; the acetate ions were generated by copper(II) catalyzed Baeyer-Villiger oxidation of the solvent. A mechanism for the synthesis is proposed. The resulting Cu-paddlewheel compound exhibits strong (-400 K) antiferromagnetic interactions.

journal of coordination chemistry

Synthesis of copper(II) halide dimers with 2-amino-5-methylpyridine and serendipitous copper catalyzed synthesis of 3-bromo-2-ethyl-5-methyl-1 H -pyrrolo[2,3- b ]pyridine