Abstract
The reaction of cis-[Os(CO) 4Me 2] with Me 3NO in the THF or MeCN yields the complexes fac-[Os(CO) 3(L)Me 2] (where L = THF or MeCN). Whereas the THF complex is unstable and only characterised spectroscopically, fac-[Os(CO) 3(MeCN)Me 2] has been isolated as a white solid and fully characterized by both analytical and spectroscopic methods. These complexes fac-[Os(CO) 3(L)Me 2] are shown to be useful intermediates. Thus, reaction with PPh 3 gives fac-[Os(CO) 3(PPh 3)Me 2] in good yield. Reactions of fac-[Os(CO) 3(L)Me 2] (L = CO or MeCN) with CPh 3PF 6 or B(C 6F 5) 3 have been investigated. Whereas cis-[Os(CO) 4Me 2] showed no reaction with either CPh 3PF 6 or B(C 6F 5) 3, the reaction of fac-[Os(CO) 3(MeCN)Me 2] with CPh 3PF 6 in CH 2Cl 2 occurred over 16 h at room temperature to give an unstable cationic product and CPh 3Me. The reaction was monitored by both IR and NMR spectroscopies. When this reaction of fac-[Os(CO) 3(MeCN)Me 2] was carried out in the presence of a trapping ligand such as MeCN, the stable cationic product [Os(CO) 3(MeCN) 2Me] + could be isolated and identified spectroscopically.
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