Abstract:The complex [Au2(p,-dppm)(C=Ct-Bu),], 1, dppm = Ph,PCH,PPh,, is formed by reaction of [AuC=Ct-Bu] with dppm. Compound 1, as an acetone solvate, crystallizes in the monoclinic space group P2,lc with cell dimensions a = 14.047(1), b = 16.124(1), c = 17.140(3) A, P = 103.17(2)" and four formula units per cell. The crystal and molecular structures of this salt were solved by X-ray diffraction techniques using 2634 counter data with I > 2u(I). Refinement of 278 variables by full-matrix least squares converged at an agreement factor R = 0.023. Thermolysis of complex 1 in refluxing toluene led to intermolecular elimination of t-Bu-CH, by combination of a t-BuC--C ligand of one molecule of 1 with a proton from the CH,P, group of a second, and formation of the stable tetragold(1) complex [Au,(p,,-Ph,PCHPPh,)(p,-dppm)(C=Ct-Bu),] 2, which was characterized by its spectroscopic properties.Key words: acetylide complexes, gold complexes, X-ray crystallography, nmr spectroscopy, bis(dipheny1phos-phino)methane. Mots cl6s : complexes dlacCtylures, complexe d'or, cristallographie par rayons X, spectroscopie rmn, bis(diph6-ny1phosphino)mCthane.[Traduit par la rkdaction]