Silylation of 1,1′-diaminoferrocene afforded 1,1′-Fc(NHSiMe 3 ) 2 (LH 2 ) as red air-sensitive crystals. Reaction with M(CH 2 Ph) 4 (M ) Ti, Zr) afforded the corresponding LM(CH 2 Ph) 2 (M ) Zr; Ti), where the Fc(NSiMe 3 ) 2 2group serves as a diamide ligand. Alternatively, the magnesium salt LMg(THF) 2 was reacted with TiCl 4 (THF) 2 to give LTiCl 2 as purple airsensitive crystals. Methylation of the latter with MeLi affords LTiMe 2 .
An X-ray structure determination of {CyNC-[N(SiMe 3 ) 2 ]NCy}Zr(CH 2 Ph) 3 , crystallized from pentane, differs from the solid-state structure previously reported for the same compound crystallized from toluene. In contrast to the earlier report, we find no evidence for the presence of an η 2 interaction in the solid state by X-ray crystallography or in solution by means of 1 H or 13 C NMR spectroscopy.
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