Polyhedron p. 1807 - 1815 (1996)
Update date:2022-08-05
Topics: Synthesis Properties
Doidge-Harrison, Solange M. S. V.
Irvine, John T. S.
Spencer, Gavin M.
Wardell, James L.
Ganis, Paolo
Valle, Giovanni
Tagliavini, Giuseppi
Syntheses of Ph2Pb(dmit) (3), [Q] [Ph2Pb(dmit)1] (5, Q = NEt4 or 1,4-Me2-pyridinium), (Ph3Pb)2(dmit) (4) and Pb(dmit) (6) are reported [H2-dmit = 4,5-dimercapto-1,3-dithiole-2-thione]. Compound 3 was produced from Ph2Pb(OAc)2 and [NEt4]2[Zn (dmit)2], while 4 was obtained from Ph3PbOAc and either Na2(dmit) or [NEt4]2[Zn(dmit)2]. The ionic species, 5, were obtained by addition of [Q] 1 to 3 (eg. for Q = 1,4-Me2-pyridinium) or from reaction of Ph2PbI2 with [NEt4]2[Zn(dmit)2]. Reaction of either Pb(OAc)2 or Pb(NO3)2 with [NEt4]2[Zn(dmit)2] produced 6. NMR spectra, including the solid state spectra for 3, have been obtained. X-ray crystallography revealed 4 to be a monomeric compound with each Pb atom having a distorted tetrahedral geometry. The C - Pb - S bond angles are less and the C - Pb - C bond angles greater than ideal tetrahedral angles. The dmit ligand is effectively inserted between two phenyl rings of different Ph3Pb groups in 4, with short non-bonded C - C and C - S distances of 3.4-3.7 A. Cyclic voltammetric studies of 3 and of 4 in DMF have also been carried out.
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