suspension After stirring over night, the solution was filtered
and subsequent removal of solvents in vacuo initially left a
orange/amber syrup in which a solid amber precipitate
formed, but eventually a dry, bright yellow solid remained.
The solid was washed with 3 ꢂ 5 cm3 portions of dry pentane
and dried thoroughly under vacuum. The freshly prepared
solid product would re-dissolve in aromatic solvents, was
soluble in chlorinated hydrocarbons and was insoluble in ether
and alkanes. However, after standing for several days, it could
only be re-dissolved if some more P(OMe)3 was added to the
solvent. The product became slightly more amber coloured
upon standing in air. Yield 1.43 g (70.9%). Mp 127.5 1C.
1H NMR d (ppm) 4.44 (q, 2H, CH3CH2O), 3.49 (s, 49H,
CH3OP) and 1.06 (t, 3H, CH3CH2O). 13C NMR d (ppm)
227.80 (1C, OCS2), 69.03 (1C, CH3CH2O), 50.65 (43C,
CH3OP) and 14.07 (1C, CH3CH2). 31P NMR d (ppm) 3.87
(s, free P(OMe)3) and 1.30 (s, 1P, Cu–P(OMe)3). Mass spectrum
(FAB) m/z 922, 800, 551 (Cu3(EtOCS2)3(P(OMe)3)n; n = 3, 2, 0
respectively); 617 (Cu2(EtOCS2)2(P(OMe)3)2); 559, 435, 311, 187
(Cu(P(OMe)3)n; n = 4, 3, 2, 1, respectively). Elemental analysis,
calc. for C6H14CuO4PS2: C, 23.3; H, 4.6%; Found: C, 23.3; H, 4.6%.
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2
CH3CH2O) and 1.26 (d, JH–P = 5.44 Hz, pH, PCH3). 13C
NMR d (ppm) 69.47 (1C, CH3CH2O), 15.97 (d, 1JC–P = 72.16
Hz, 3C, PCH3) and 14.21 (1C, CH3CH2O). 31P NMR d (ppm)
39.63 (br. s, 1P, Cu–PMe3). Elemental analysis, calc. for
C6H14CuOPS2: C, 27.6; H, 5.4%; Found: C, 27.7; H, 5.2%.
Acknowledgements
The authors would like to thanks EPSRC, UK for financial
assistance. This paper was written whilst POB was a Distin-
guished Visiting Fellow at the Institute of Advanced Study,
Durham University. He thanks the Institute and the University
for their hospitality and support. M. A. would like to thank
Center of Research Excellence in Renewable Energy, KFUPM
for the support.
c
2780 New J. Chem., 2011, 35, 2773–2780
This journal is The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2011