The Synthesis, Properties, and the Crystal and Molecular Structures of Five-co-ordinate Copper(I) and Silver(I) Complexes of a Quinquedentate Macrocyclic Ligand having an 'N3S2' Donor Set

DOI: 10.1039/DT9800002020

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 2020 - 2027 (1980)

Update date:2022-08-03

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Authors:

Drew, Michael G.B.

Cairns, Colin

McFall, Stephen G.

Nelson, S. Martin

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Article abstract of DOI:10.1039/DT9800002020

The 17-membered macrocyclic ligand L¹ containing the 'N2S3' donor set has been synthesised by the template action of silver(I) salts on the cyclic Schiff-base condensation of 2,6-diacetyl-pyridine with 1,10-diamine-4,7-dithiadecane. The copper(II) ion was ineffective as a template for the synthesis.However, copper(II) complexes of L¹ could be obtained from 1>(1+) via metal exchange (transmetallation).Sodium tetraphenylborate is a reducing agent for IIL¹>(2+), affording IL¹>(1+) in good yield.Possible mechanisms for the reducing action of (1-) are discussed.Hydrogenation of 1>(1+) salts using Na give the free reduced macrocycle RL¹ (i.e.L¹ + 4H) from which a new range of macrocyclic complexes may be obtained.Infrared and electronic spectra of the silver(I) and copper(I) complexes of L¹ are reported.The copper(I) complexes are unreactive to both O2 and CO.Crystals of 1> are orthorhombic with a = 6.844(7), b = 12.361(11), c = 24.072(21) Angstroem, Z = 4, and space group P2₁2₁2₁.Crystals of 1> are monoclinic with a = 13.132(11), b = 25.001(12), c = 12.479(12) Angstroem, β = 105.7(1) deg, Z = 4, and space group P2₁/c.The two structures were solved by Patterson and Fourier methods from 927 and 2621 reflections above background measured by diffractometer and refined by full-matrix least squares to R 0.077 and 0.071 respectively.While the co-ordination geometry of both complexes is a distorted trigonal bipyramid there are marked differences in the macrocycle conformations in the two cases and, for the copper(I) complex, in the metal-nitrogen bond lengths.These are discussed in relation to the sizes of the two metal ions and of the macrocycle hole size.

Full text of DOI:10.1039/DT9800002020

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