Syntheses, Crystal Structures, and Density Functional Theory Calculations of the c loso-[1-M(CO)3(η4-E9)]4- (E = Sn, Pb; M = Mo, W) Cluster Anions and Solution NMR Spectroscopic Characterization of [1-M(CO)3(η4-Sn9)]4- (M = Cr, Mo, W) †

The closo-[1-M(CO)(3)(eta(4)-E(9))](4-) (E = Sn, Pb; M = Mo, W) anions have been obtained by extracting the binary alloys KSn(2.05) and KPb(2.26) in ethylenediamine (en) in the presence of 2,2,2-crypt or in liquid NH(3) followed by reaction with M(CO)(3).mes (M = Mo, W) or Cr(CO)(3).tol in en or liquid NH(3) solution. Crystallization of the molybdenum and tungsten salts was induced by vapor diffusion of tetrahydrofuran into the en solutions. …