4 S. Top, M. Gunn, G. Jaoen, J. Vaissermann, J.-C. Daran and J. R.
0.137 mmol) was dissolved in 10 ml chloroform. Upon addition
of equimolar amounts of [MCl(PPh3)] (M = Au, 68 mg; Ag, 56
mg; Cu, 49 mg) solution changed from pale to deep yellow.
After 30 min the solvent was removed and the residue separated
by PLC [eluent dichloromethane–n-hexane (1:1)]. The major
yellow band gave [Re2(MPPh3)(µ-S(2-naph))(CO)8] (M = Au 5a,
Ag 5b or Cu 5c) in the following yield (mg, %): 140, 87; 100, 65;
58, 39 (Found: C, 35.41; H, 1.81. C36H22AuO8PRe2S 5a requires
C, 35.59; H, 1.83). (Found: C, 38.47; H, 2.10. C36H22AgO8-
PRe2S 5b requires C, 38.40; H, 1.97). (Found: C, 40.04; H, 1.93.
C36H22CuO8PRe2S 5c requires C, 39.98; H, 2.05%).
Thornback, J. Organomet. Chem., 1991, 414, C22.
5 P. O. Nubel and T. L. Brown, J. Am. Chem. Soc., 1984, 106, 644.
6 C. G. Kreiter, K.-H. Franzreb and W. S. Sheldrick, J. Organomet.
Chem., 1984, 270, 71.
7 H.-J. Haupt, A. Merla and U. Flörke, Z. Anorg. Allg. Chem., 1994,
620, 999; H.-G. Beckers, U. Flörke and H.-J. Haupt, Angew. Chem.,
1995, 107, 1464; H.-J. Haupt, U. Siefert and U. Flörke,
Z. Kristallogr., 1996, 211, 695; H.-J. Haupt, M. Schwefer, H. Egold
and U. Flörke, Inorg. Chem., 1997, 36, 184; H. Egold, M. Schraa
and U. Flörke, J. Organomet. Chem., 1999, 582, 345.
8 R. Wittbecker, Ph.D. Thesis, University of Paderborn, 1997.
9 T. Beringhelli, G. D’Alfonso, G. Ciani, M. Moret and A. Sironi,
J. Chem. Soc., Dalton Trans., 1993, 1101; R. D. Adams, L. Chen and
W. Wu, Organometallics, 1993, 12, 4962.
Crystal structure determinations
10 G. A. Foulds, B. F. G. Johnson and J. Lewis, J. Organomet. Chem.,
1985, 296, 147; R. D. Adams, T. Barnard, A. Rawlett and J. M. Tour,
Eur. J. Inorg. Chem., 1998, 429; P. Braunstein, J. R. Galsworthy, B. J.
Hendan and H. C. Marsmann, J. Organomet. Chem., 1998, 551, 125;
S.-M. Lee, K. K. Cheung and W.-T. Wong, J. Cluster Sci., 1996, 7,
435; E. W. Ainscough, A. M. Brodie, R. K. Coll, A. J. A. Mair and
J. M. Waters, J. Organomet. Chem., 1996, 509, 259; M. Monari,
R. Pfeiffer, U. Rudsander and E. Nordlander, Inorg. Chim. Acta,
1996, 247, 131.
11 H. Egold, D. Schwarze and U. Flörke, unpublished results.
12 V. Küllmer and H. Vahrenkamp, Chem. Ber., 1977, 110, 3810.
13 R. D. Adams, J. E. Cortopassi and S. B. Falloon, Organometallics,
1992, 11, 3794.
14 H.-J. Haupt, C. Heinekamp and U. Flörke, Z. Anorg. Allg. Chem.,
1990, 585, 168; A. Merla, U. Flörke and H.-J. Haupt, Z. Anorg. Allg.
Chem., 1994, 620, 999.
15 H.-J. Haupt, C. Heinekamp and U. Flörke, Inorg. Chem., 1990,
29, 2955; C. Heinekamp, Ph.D. Thesis, University of Paderborn,
1990.
16 C. A. Dullaghan, G. B. Carpenter, D. A. Sweigart, D. S. Choi, S. S.
Lee and Y. K. Chung, Organometallics, 1997, 16, 5688.
17 U. Flörke and H.-J. Haupt, unpublished results.
18 H.-J. Haupt, M. Schwefer and U. Flörke, Z. Anorg. Allg. Chem.,
1995, 621, 1098.
19 J. Powell, J. C. Brewer, G. Gulia and J. F. Sawyer, J. Chem. Soc.,
Dalton Trans., 1992, 2503.
20 G. Brauer, Handbuch der präparativen Anorganischen Chemie,
F. Enke Verlag, 3rd edn., vol. 3, 1981, p. 2019.
Pertinent crystallographic data for compounds 2c, 2g, 5a and
5b are summarised in Table 2. All data sets were collected on a
Bruker AXS P4 diffractometer with graphite monochromated
Mo-Kα radiation. Standard reflections monitored after every
400 showed only random deviations. Intensities were corrected
for Lorentz-polarisation effects and absorption corrections via
ψ-scans were applied. The structures were solved by direct and
conventional Fourier methods. Full-matrix least-squares struc-
ture refinement based on F2 anisotropically; geometrically
placed hydrogen atoms were refined with a riding model. The
µ-H atom of structure 2c was determined from the ∆F map and
refined, that of 2g was not located and not included in the
refinement. Programs used for calculations: SHELX 97.23
CCDC reference number 186/1594.
graphic files in .cif format.
Acknowledgements
We thank Degussa for the generous loan of HAuCl4ؒ3H2O.
References
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