Fox Thomas, Hausmann Heike, Günther Harald
University of Siegen, FB 8, OCII, D-67068 Siegen, Germany.
Magn Reson Chem. 2004 Sep;42(9):788-94. doi: 10.1002/mrc.1443.
1H, 6Li and 13C NMR spectroscopy were used to determine the structure of aggregates formed in mixtures of methyllithium, H3CLi, and lithium bromide and iodide in diethyl ether and tetrahydrofuran. From the chemical shifts, the signal intensity distribution and the isotope shifts observed for partially deuterated systems, it was shown that generally tetrameric structures with different halogen contents dominate. For methyllithium-lithium bromide (1:1) in THF a considerable concentration of an H3CLi-LiBr dimer was found. For the first time, deuterium-induced 6Li isotope shifts over four bonds were observed.
利用1H、6Li和13C核磁共振光谱法测定了甲基锂、H3CLi与溴化锂和碘化锂在乙醚和四氢呋喃中的混合物所形成聚集体的结构。从化学位移、信号强度分布以及部分氘代体系中观察到的同位素位移可知,一般来说,具有不同卤素含量的四聚体结构占主导。对于四氢呋喃中的甲基锂-溴化锂(1:1),发现有相当浓度的H3CLi-LiBr二聚体。首次观察到了跨越四个键的氘诱导6Li同位素位移。