Synthesis of isotopic forms of dilithiomethane [(ch₂⁶li₂)_n and (cd₂li₂)_n] and preliminary structural information obtained by x-ray powder and solid-phase ¹³c nmr techniques

New synthetic methods have been developed to alter the Ziegler procedure1 for synthesis of dilithiomethane of various isotopic compositions. [CH2(6Li2)]n has been prepared to facilitate solid 13C NMR spectra. (CD2Li2)n has been prepared, and preliminary X-ray powder pattern data are reported. The first solid-state 13C NMR spectrum on any organolithium compound has been obtained. The l3C NMR spectra of solid samples of [CH3(6Li)]4 and [CH2(6Li2)]n are discussed. © 1984, American Chemical Society. All rights reserved.