Actinide complexes of the calixarenes. Part 2. Synthesis and crystal structure of a novel thorium(IV) complex of p-tert-butylcalix[8]arene
- 1 January 1991
- journal article
- research article
- Published by Royal Society of Chemistry (RSC) in J. Chem. Soc., Dalton Trans.
- No. 10,p. 2625-2632
- https://doi.org/10.1039/dt9910002625
Abstract
The synthesis and room-temperature single-crystal X-ray structure determination of a novel tetra nuclear thorium complex with p-tert-butylcalix[8]arene, H8L, has been achieved, the stoichiometry being assigned as [Th4(HL)(H2L)(dmso)4(OH)3(OH2)]·dmso·2H2O (dmso = Me2So). Crystals of the complex are triclinic, space group P, a= 29.51(2), b= 21.68(3), c= 21.16(1)Å, α= 60.94(6), β= 78.75(5), γ= 87.75(8)° and Z= 2; the structure was refined to a residual of 0.079 for 16 903 ‘observed’[I > 3σ(I)] reflections. Each calixarene unit, one with approximate 2 and the other approximate mm symmetry, is co-ordinated to two thorium atoms, the environment of each thorium comprising five ligand phenolic oxygen atoms, three being ‘monodentate’ and two bridging, with a monodentate O-bonded dmso entering through each cup of each ligand, and hydroxide groups variously bridging to the other thorium within the same ligand, and binding the two Th2L systems together. The 1H NMR spectrum has been rationalised in terms of the X-ray structure.Keywords
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