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207Pb NMR of minium, Pb3O4: evidence for the [Pb2]4+ ion and possible relativistic effects in the Pb–Pb bond

✍ Scribed by S.P. Gabuda; S.G. Kozlova; V.V. Terskikh; C. Dybowski; G. Neue; D.L. Perry

Publisher
Elsevier Science
Year
1999
Tongue
English
Weight
132 KB
Volume
15
Category
Article
ISSN
0926-2040

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✦ Synopsis

207

Ž . 207 Solid Pb O has been studied with Pb nuclear magnetic resonance NMR spectroscopy. The Pb NMR chemical-shift 3 4 tensor of the Pb 2q site has principal values of d s 1980 " 5 ppm, d s 1540 " 5 ppm, and d sy1108" 10 ppm; 11 22 33 d s 804 " 10 ppm. The chemical-shift tensor of the Pb 4q site is axial, with principal values d sy1009" 3 ppm and iso 5 d s 1132 " 3 ppm; d sy1091" 3 ppm. The Pb 4q -Pb 2q scalar coupling constant J s 2.3 " 0.1 kHz. The main H iso Pb -Pb contribution to the Pb 2q chemical-shift anisotropy is proposed to arise from an exchange interaction in the Pb 2q -Pb 2q w x 4q pairs, conventionally regarded as molecular Pb ions.

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The reactions of UO 3 and I 2 O 5 with RbCl, TlCl, SrCl 2 , or Pb(NO 3 ) 2 at 2003 3C for 3 days in aqueous media result in the formation of A 2 [(UO 2 ) 3 (IO 3 ) 4 O 2 ] (A ‫؍‬ Rb (1), Tl (2)) and AE[(UO 2 ) 2 (IO 3 ) 2 O 2 ](H 2 O) (AE ‫؍‬ Sr (3), Pb, (4)). Compounds 1 and 2 are isostructural wit