Malon Michal, Imakubo Tatsuro, Koshino Hiroyuki
RIKEN (Institute of Physical and Chemical Research), 2-1 Hirosawa, Wako, Saitama 351-0198, Japan.
Magn Reson Chem. 2008 Feb;46(2):150-5. doi: 10.1002/mrc.2147.
A series of substituted tetraselenafulvalenes (TSeFs) was studied in solution using 1H, 13C and 77Se NMR spectroscopy. Chemical shifts and heteronuclear coupling constant values were determined and assigned. Novel two-dimensional H(Se)C and H(C)Se triple-resonance correlation experiments were applied at natural abundance in order to accomplish 13C and 77Se signal assignments. Using this approach, all the signals were unambiguously assigned and atom connectivity was established in the studied TSeF derivatives. These experiments, allowing signal assignments of quaternary carbons, may find wide application in the study of substituted TSeF and other organoselenium compounds. To the best of our knowledge, triple-resonance experiments with proton detection have been applied to organoselenium compounds for the first time.
利用¹H、¹³C和⁷⁷Se核磁共振光谱在溶液中研究了一系列取代四硒富瓦烯(TSeFs)。测定并归属了化学位移和异核耦合常数的值。为了完成¹³C和⁷⁷Se信号归属,在天然丰度下应用了新型二维H(Se)C和H(C)Se三共振相关实验。采用这种方法,在研究的TSeF衍生物中明确归属了所有信号并确定了原子连接性。这些能够对季碳进行信号归属的实验,可能在取代TSeF和其他有机硒化合物的研究中得到广泛应用。据我们所知,质子检测三共振实验首次应用于有机硒化合物。