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DOI: 10.1039/A805137B (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1998, 3961-3968

Cadmium(II), bismuth(III), lead(II) and thallium(I) crown thioether chemistry: synthesis and crystal structures of [(CdI2)2([24]aneS8)], [(BiCl3)2([24]aneS8)], [Pb2([28]aneS8)][ClO4]4 and [Tl([24]aneS8)]PF6 ([24]aneS8 = 1,4,7,10,13,16,19,22-octathiacyclotetracosane; [28]aneS8 = 1,4,8,11,15,18,22,25-octathiacyclooctacosane)

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Alexander J. Blake, Dieter Fenske, Wan-Sheung Li, Vito Lippolis and Martin Schröder

Abstract

The complexes [(CdI2)2([24]aneS8)], [(BiCl3)2([24]aneS8)], [Pb2([28]aneS8)][ClO4]4 and [Tl([24]aneS8)]PF6 ([24]aneS8 = 1,4,7,10,13,16,19,22-octathiacyclotetracosane, [28]aneS8 = 1,4,8,11,15,18,22,25-octathiacyclooctacosane) have been prepared, characterized and their crystal structures determined. In [(CdI2)2([24]aneS8)] two CdI2 units are bound to the macrocycle forming a discrete centrosymmetric binuclear complex, Cd(1)–I(1) 2.7551(11), Cd(1)–I(2) 2.6944(8), Cd(1)–S(1) 2.817(2), Cd(1)–S(4) 2.615(2), Cd(1)–S(7) 2.927(2) Å. In [(BiCl3)2([24]aneS8)] two BiCl3 units are weakly bonded to the thioether crown, Bi–S 3.134(2)–3.313(2) Å, to give a discrete centrosymmetric binuclear complex with the two metal centres disposed on opposite sides of the mean plane of the macrocycle. In [Pb2([28]aneS8)][ClO4]4 an S4O4 co-ordination is realized at each PbII sitting in the macrocyclic cavity. The two PbII are bridged by two ClO4– ions, Pb–S 2.861(2)–2.998(2), Pb–O 2.701(7)–2.936(6) Å. In contrast, [Tl([24]aneS8)]PF6 adopts a polymeric structure in which each TlI bridges two thioether crowns to give an infinite sinusoidal chain. The [S4 + S4] co-ordination sphere at the metal centre is satisfied by two half ligands in a sandwich arrangement, Tl–S 3.2413(11)–3.4734(14) Å.

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