Synthesis and characterization of GeH2Cp*2 and its structural comparison with SiXHCp*2(X=Cl, H) and SnCl2Cp*2

Abstract

The organogermane GeH2Cp*2 (1) was synthesized by the reaction of GeCl2Cp*2 (A) with LiAlH4 in quantitative yield, whereas the synthesis of the previously reported compounds SiCl2Cp*2 (B), SnCl2Cp*2 (C), SiClHCp*2 (D) and SiH2Cp*2 (E) followed established routes. The molecular structures of the Cp*M(IV) derivatives 1, B, D and E are reported. In addition, compound 1 was characterized by spectroscopic methods such as 1H and 13C{1H} NMR spectroscopy, ATR-FTIR spectroscopy and EI-mass spectrometry. The thermal behavior of the germanes 1 and A was investigated by thermogravimetric analysis (TGA, DSC) and PXRD. The decomposition of compounds A and 1 starts at 270°C (A) and 200°C (1), respectively. The formation of crystalline Ge upon heating these compounds in sealed quartz glass capillaries was observed at 270°C (A) and 500°C (1).

Keywords

• crystal structure
• decomposition behavior
• germanium
• pentamethylcyclopentadienyl
• silicon
• tin