View PDF Version
 
DOI: 10.1039/A806158K (Paper) Reference Section for: Chem. Commun., 1998, 2351-2352

A powerful new oxidation agent towards metallic gold powder: N,N′-dimethylperhydrodiazepine-2,3-dithione (D) bis(diiodine). Synthesis and X-ray structure of [AuDI2]I3

(Note: The full text of this document is currently only available in the PDF Version )

Francesco Bigoli, Maria Angela Pellinghelli, Paola Deplano, Maria Laura Mercuri, Gloria Pintus, Angela Serpe and Emanuele F. Trogu

Abstract

The oxidation of gold powder by a new safe and powerful oxidising reagent, the bis-diiodine adduct of N,N′-dimethylperhydrodiazepine-2,3-dithione (D), to produce [AuI2D]I3 under ambient conditions is described.

References

  1. N. Bricklebank, S. M. Godfrey, C. A. McAuliffe, A. G. Mackie and R. G. Pritchard, J. Chem. Soc., Chem. Commun., 1992, 944 RSC; S. M. Godfrey, C. A. McAuliffe and R. G. Pritchard, J. Chem. Soc., Dalton Trans., 1993, 371 and 2875 RSC; S. M. Godfrey, D. G. Kelly, C. A. McAuliffe and R. G. Pritchard, ibid., 2053 Search PubMed; S. M. Godfrey, C. A. McAuliffe and R. G. Pritchard, J. Chem. Soc., Chem. Commun., 1994, 45 RSC; N. Bricklebank, S. M. Godfrey, C. A. McAuliffe and R. G. Pritchard, J. Chem. Soc., Dalton Trans., 1996, 157 RSC.
  2. S. M. Godfrey, N. Ho, C. A. McAuliffe and R. G. Pritchard, Angew. Chem., Int. Ed. Engl., 1996, 33, 2344 CrossRef.
  3. F. Bigoli, P. Deplano, F. A. Devillanova, V. Lippolis, M. L. Mercuri, M. A. Pellinghelli and E. F. Trogu, Inorg. Chim. Acta, 1998, 267, 115 CrossRef CAS and references therein.
  4. Prepared according to R. Isaksson, T. Liljefors and J. Sandstrom, J. Chem. Res. (S), 1981, 43 Search PubMed.
  5. (a) T. J. Marks, Ann. NY Acad. Sci., 1970, 313, 594; (b) J. R. Ferraro, Coord. Chem. Rev., 1982, 43, 205 CrossRef CAS; (c) P. Deplano, F. A. Devillanova, J. R. Ferraro, F. Isaia, V. Lippolis and M. L. Mercuri, Appl. Spectrosc., 1992, 46, 1625 CAS; (d) F. Bigoli, P. Deplano, M. L. Mercuri, M. A. Pellinghelli, A. Sabatini, E. F. Trogu and A. Vacca, J. Chem. Soc., Dalton Trans., 1996, 3583 RSC.
  6. In fact the strong peak of uncoordinated diiodine (v= 180 cm–1in solid I2[d(I–I)= 2.715 Å, F. van Bolhuis, P. B. Koster and T. Migehelsen, Acta Crystallogr., 1967, 23, 90]) is shifted to lower frequencies upon coordination as a consequence of the lowering of the force constant of the I–I vibration in a CT adduct Search PubMed.
  7. Crystal data: C7H12AuI5N2S2, M= 1019.77, crystal dimensions: 0.16 × 0.16 × 0.20 mm, triclinic, space group, P[1 with combining macron], a= 8.204(6), b= 15.994(5), c= 8.080(6)Å, α= 96.68(2), β= 112.40(2), γ= 92.20(2)°, V= 969.6(1.1)Å3, Z= 2, Dc= 3.493 Mg m–3, µ= 15.747 mm–1, F(000) 888; 4249 reflections collected (3.09≤θ≤ 27.05°) at T= 293(2) K, 4249 independent, R1= 0.0430 [I > 2σ(I)], wR2= 0.1172(all data), gof = 0.878 for 158 parameters, largest difference peak/hole 1.974/2–1.286 e Å–3, Data were collected from a Siemens AED diffractometer (graphite-monochromated Mo-Kα radiation, λ= 0.71073 Å) with θ–2θ scan technique. An empirical absorption correction8 was applied (transmission coefficients: 0.8808, 1.2731). The structure was solved by direct methods using SIR929 and refined by full-matrix least-squares against F2(SHELXL-9710). Anisotropic refinement of all non-H atoms. R values R1=Σ||Fo| – |Fc||/Σ|Fo|, wR2=[Σw(Fo2–Fc2)2/Σw(Fo2)2]½.
  8. N. Walker and D. Stuart, Acta Crystallogr., Sect. A, 1983, 39, 158 CrossRef.
  9. A. Altomare, C. Cascarano, C. Giacovazzo, A. Guagliardi, M. C. Burla, G. Polidori and M. Camalli, J. Appl. Crystallogr., 1994, 27, 435 CrossRef.
  10. G. M. Sheldrick, SHELX-97: Program for Crystal Structure Determination, Universität Göttingen, Germany, 1997.
Click here to see how this site uses Cookies. View our privacy policy here.