Template synthesis of a tetraazamacrocyclic ligand with two pendant pyridinyl groups: properties of the isomers of the metal-free ligand and of their first-row transition metal compounds

Inorganic Chemistry
P CombaA Vielfort

Abstract

The one-step reaction of [Cu(en)(2)](2+) (en = 1,2-diaminoethane) with formaldehyde, ethyl 2-pyridyl acetate, and base produces a mixture of [Cu(s-pypymac)](2+) and [Cu(a-pypymac)](2+) (s-pypymac = syn-6,13-bis(2-pyridinyl)-1,4,8,11-tetraazacyclotetradecane, a-pypymac = anti-6,13-bis(2-pyridinyl)-1,4,8,11-tetraazacyclotetradecane; syn-to-anti ratio approximately 1:9) in low yield (6%). Ion exchange chromatography is used for isomer separation, and the two isomers of the metal-free ligand are obtained by reduction of the copper(II) complexes and subsequent ion exchange chromatography. Crystal structure analyses of the metal-free a-pypymac ligand, of two isomeric copper(II) compounds of a-pypymac and one of s-pypymac, and of the cobalt(III) complexes of a- and s-pypymac and nickel(II), as well as zinc(II) complexes of a-pypymac, are reported and discussed on the basis of the expectations from force field calculations and from published experimental data of the transition metal compounds of the bis-pendant amine derivative diammac.

Citations

Nov 1, 2005·Spectrochimica Acta. Part A, Molecular and Biomolecular Spectroscopy·Sulekh Chandra, Rajiv Kumar
Dec 12, 2012·Dalton Transactions : an International Journal of Inorganic Chemistry·Peter CombaHolger Stephan

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