A trinuclear carbonylruthenium complex, [Ru 3 (CO) 12 ], was treated with diynes bearing ester, phenyl, or trimethylsilyl groups on the alkyne termini to give rise to various complexes. A diyne diester afforded a dinuclear ruthenacycle complex similar to known iron ferrole complexes and a mononuclear ruthenacyclopentadiene complex. The selectivity for the formation of these products varied depending on the ratio of the diyne diester toward [Ru 3 (CO) 12 ]. When a phenyl-substituted diyne was employed, a cyclopentadienone complex was formed together with the expected dinuclear ruthenacycle complex. In contrast, a bis(trimethylsilyl)diyne gave the corresponding cyclopentadienone complex as the only product. Treatment of the obtained ruthenabicycle complex with trimethylamine oxide (Me 3 NO) gave a mono(trimethylamine) complex, which was further converted into various phosphane complexes upon reaction with phosphanes in refluxing THF. The corresponding monophosphane complexes
Hydrogenated nanostructured graphite has been reported to exhibit a characteristic peak at around 600–800 K in thermal desorption spectroscopy (TDS). The origin of this peak is still controversial. We have reexamined it based on a combination Fourier transform infrared (FT-IR), electron diffraction, and electron energy-loss spectroscopy (EELS) study. The FT-IR spectrum of HNG exhibited an unknown broad absorption band at very low frequencies around 660 cm−1, which almost disappeared by annealing up to 800 K. Electron diffraction as well as plasmon peaks in EELS detected unusual shrinkage and subsequent expansion of the graphene interlayer distance by hydrogen incorporation and desorption with annealing, which were well correlated with the change in intensity of the 660 cm−1 IR band. An energetically stable configuration was found by theoretical model calculations based on GAUSSIAN03. All the present results are consistent with our previous studies, which suggested that hydrogen is loosely trapped between graphene layers [S. Muto et al., Jpn. J. Appl. Phys. 44, 2061 (2005); T. Kimura et al., J. Alloys Compd. 413, 150 (2006)].
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