1784
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5.2. Formation of 5
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Inorg. Chem. 44 (2005) 1263;
To a freshly prepared sample of 0.52 g (0.68 mmol) of 3 in CHCl3
was added 0.18 g of PPh3 (0.68 mmol). A clear solution of 4 was
formed. 31P NMR of the solution: 28.2 ppm (d, PPh2, 3J(P,P) =
12.7 Hz), 32.2 ppm (t, PPh3, 1J(Pt,P) = 3670 Hz, 3J(P,P) = 12.7 Hz).
After addition of n-pentane a microcrystalline material was ob-
tained which was dried in vacuum. For crystal growth the material
was dissolved in CHCl3 and layered with n-pentane; a viscous oil
formed which could not be crystallized. After about 3 months
and apparently admission of humidity by a leaking stopcock few
crystals have grown from the oil which were separated mechani-
cally and which turned out to be the carbonyl complex 5. 31P
NMR (CH2Cl2): 41.5 ppm (s, 2J(Pt,P) = 64.9 Hz). IR (Nujol): 2000 s
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(m CO), 1572 m, 1480 m, 1437 s, 1335 w, 1314 w, 1186 w, 1157
w, 1105 s, 1096 s, 1026 m, 990 m, 918 w, 909 m, 741 s, 730 s,
691 s, 532 m, 513 s, 484 m (cmꢀ1).
Acknowledgements
[18] W. Petz, C. Kutschera, B. Neumüller, Organometallics 24 (2005) 5038.
[19] (a) S. Marrot, T. Kato, H. Gornitzka, A. Baceiredo, Angew. Chem. 118 (2006)
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127 (2005) 5314.
We thank the Deutsche Forschungsgemeinschaft for financial
support. W.P. is also grateful to the Max-Planck-Society, Munich,
Germany, for supporting this research project.
Appendix A. Supplementary data
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(b) J. Vicente, M.T. Chicote, C. MacBeath, J. Fernandez-Baeza, D. Bautista,
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CCDC 804171, 804172 and 804173 contain the supplementary
crystallographic data for 3ꢁ2CDCl3, 3ꢁ1.5CH2Cl2, and 5. These data
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