Complexes of a new N<inf>3</inf>S<inf>2</inf> macrocycle: Synthesis, structure and electrospray mass spectrometry

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Journal Article
Journal of Coordination Chemistry, 2003, 56 (11), pp. 923 - 932
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The silver(I) complex of a 15-membered macrocyclic ligand with an N 3S2 donor set (L1) has been prepared by the reaction of 2,6-diacetylpyridine with 1,8-diamino-3,6-dithiaoctane in the presence of silver(I) ions. A reduced form (L2) of the ligand, in which the imine groups are converted to amines, was prepared by the reduction of the silver(I) complex by sodium borohydride. The ligand L2 has been characterised by various spectroscopic techniques and the copper(II) complex has been prepared. The metal complexes of L1 and L2 have been characterised by electrospray mass spectrometry and UV-visible spectroscopy. The copper(II) complex of L1 has been synthesised from [AgL1]+ via metal exchange. [CuL1](CIO 4)2 crystallises in the orthorhombic space group Pna2 1 with a= 14.374(5)Å, b = 12.947(3)Å, c= 11.824(3) Å with Z=4. The geometry about the metal centre approximates trigonal bipyramidal with the pyridinyl nitrogen and the sulfur donors in the equatorial positions and the imine nitrogen donors in the axial positions. Metal ion exchange and the relative stabilities of metal complexes of the macrocyclic ligands were studied by electrospray mass spectrometry.
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