Main Group Metal Chemistry (Aug 2015)
The disilanes Cp*SiCl2SiH3 and Cp*SiH2SiH2Cp*
Abstract
Hydrogenation of Cp*SiCl2SiCl3 (A) (Cp*=C5Me5) with diisobutylaluminum hydride (DIBAL-H) gave partially hydrogenated disilane Cp*SiCl2SiH3 (1) with 45% yield, whereas the reaction with lithium aluminum hydride (LiAlH4) provided the well-known Cp*SiH2SiH3. The symmetric disilane Cp*SiH2SiH2Cp* (2) is accessible either by hydrogenation of Cp*SiCl2SiCl2Cp* (B) with DIBAL-H or LiAlH4 but attempts to partially hydrogenate the disilane B failed. The reaction of B with 1 eq. DIBAL-H afforded a mixture of five different molecules of the type Cp*SiR1R2SiR3R4Cp* (D, R1-R4=H, Cl) which co-crystallize in a single crystal with a H/Cl ratio of 1/3. Characterization by 1H and 29Si NMR, ATR IR spectroscopy, EI mass spectrometry and for 1 and the co-crystal D the single crystal X-ray diffraction analysis is presented. Compounds 1 and 2 are thermally stable in the solid state and do not decompose prior to evaporation.
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