Issue 6, 1990

Synthesis, crystal structure, and quasi-reversible dioxygen binding of [Cu2(tpmc)]X2[tpmc = 1,4,8,11-tetrakis(2′-pyridylmethyl)-1,4,8,11-tetra-azacyclotetradecane; X = ClO4, PF6, or CF3SO3]

Abstract

Dicopper(I) complexes of tpmc [1,4,8,11-tetrakis(2′-pyridylmethyl)-1,4,8,11-tetra-azacyclotetradecane] have been synthesized. The complexes reacted with dioxygen at low temperature (below –60 °C) to form two species of adduct quasi-reversibly, which were characterized by Resonance Raman spectra (16O–16O stretching at 820 and 771 cm–1 and Cu–16O stretching at 529 and 491 cm–1 which shifted to lower energy when 18O2 was substituted for 16O2). From an acetone solution of the dioxygen adducts bis(pyridine-2-carboxylato)copper(II) was isolated. The molecular structure of the dicopper(I) complex [Cu2(tpmc)][CF3SO3]2 was determined by X-ray diffraction analysis. The complex crystallizes in the monoclinic space group P21/n with a= 14.341(4), b= 15.392(4), and c= 9.700(2)Å, β= 93.95(2)°, and Z= 2, and the structure was refined to R= 0.055 and R′= 0.058. The complex cation has a centre of symmetry and each copper atom is co-ordinated by one nitrogen of the macrocyclic ring and two pendant pyridyl nitrogens forming a distorted trigonal plane with a Cu ⋯ Cu separation of 6.739(2)Å.

Article information

Article type
Paper

J. Chem. Soc., Dalton Trans., 1990, 1741-1746

Synthesis, crystal structure, and quasi-reversible dioxygen binding of [Cu2(tpmc)]X2[tpmc = 1,4,8,11-tetrakis(2′-pyridylmethyl)-1,4,8,11-tetra-azacyclotetradecane; X = ClO4, PF6, or CF3SO3]

E. Asato, S. Hashimoto, N. Matsumoto and S. Kida, J. Chem. Soc., Dalton Trans., 1990, 1741 DOI: 10.1039/DT9900001741

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