Metal-ion Selectivity by Macrocyclic Ligands. Part 1. The Interaction of NiII and CuII with Pyridinyl-derived N3O2 Macrocycles; The X-Ray Structures of a Free Macrocycle, its Endomacrocyclic Complexes of NiII and CuII and an Exomacrocyclic Nickel(II) Complex

DOI: 10.1039/DT9910000627

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 627 - 637 (1991)

Update date:2022-08-17

Topics:

Authors:

Bailey, Neil A.

Fenton, David E.

Kitchen, Simon J.

Lilley, Terence H.

Williams, Mark G.

et al. et al.

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Article abstract of DOI:10.1039/DT9910000627

The interaction of Cu^II and Ni^II with two macrocycles L¹ and L², each containing an N3O2 donor set, has been investigated.Spectrophotometric studies in dimethyl sulphoxide reveal the formation of complexes with 1:1 and 1:2 metal:ligand ratios and conductometric studies in the same solvent indicated that all of the complexes were 1:2 electrolytes.Conductometric titration of the 1:1 copper(II) complexes with chloride in each case indicated the formation of a 1:1 electrolyte, presumably through co-ordination of a chloride ion to the central copper of each complex.Similar titration of the nickel(II) complexes gave evidence for the formation of dinuclear species; each of these was postulated to contain a bridging chloride anion.The stability constants of the complexes together with their enthalpies of co-ordination have been determined in 95percent methanol.Extraction and related transport experiments were carried out and under the conditions employed Cu^II was favoured over Ni^II.The X-ray crystal structures of the free macrocycle L¹, the 1:1 complexes 1(H2O)>2 and 1(I)>I*MeOH, and the 1:2 complex 1₂(NO3)>NO3*2MeOH have been determined.The metal in 1(H2O)>2 is six-co-ordinate and lies within the folded macrocyclic cavity.The donor set comprises the five macrocyclic donor atoms and a water molecule.Overall, the co-ordination sphere corresponds to a restricted tetragonal rhombic arrangement.The complex 1(I)>*MeOH also has all donors of the macrocycle co-ordinated with an iodide anion occupying the sixth site to yield a distorted-octahedral geometry.The structure of 1₂(NO3)>NO3*2MeOH shows that the nickel is again six-co-ordinated, to the aliphatic nitrogen atoms from two macrocycles (each showing exo co-ordination) and a bidentate nitrate anion.

Full text of DOI:10.1039/DT9910000627

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