Homonuclear scalar 6Li6Li spin–spin coupling: First direct observation and detection via the 6Li,6Li INADEQUATE experiment,

A homonuclear 6Li,6Li spin–spin coupling has been directly measured in the case of the dimer of (E)‐2‐lithio‐1‐phenyl‐1‐o‐lithiophenylpent‐1‐ene. This constitutes the first direct observation of such a parameter. The well known INADEQUATE experiment in its one‐ and two‐dimensional versions is applied for the first time to a spin system of spin‐1 nuclei. It is demonstrated that the experiment is very sensitive for the detection of 6Li,6Li spin–spin interactions, and thus provides a promising alternative to the COSY experiment and an additional tool for structural studies on organolithium compounds in solution.