Nc. Payne et al., GOLD ACETYLIDE CHEMISTRY - THE STRUCTURE OF THE COMPLEX [AU-2(MU-DPPM)(C-C-CME(3))(2)], Canadian journal of chemistry, 73(1), 1995, pp. 6-11
The complex [Au-2(mu-dppm)(C=Ct-Bu)(2)], 1, dppm = Ph(2)PCH(2)PPh(2),
is formed by reaction of [AuC=Ct-Bu] with dppm. Compound 1, as an acet
one solvate, crystallizes in the monoclinic space group P2(1)/c with c
ell dimensions a = 14.047(1), b = 16.124(1), c = 17.140(3) Angstrom, b
eta = 103.17(2)degrees and four formula units per cell. The crystal an
d molecular structures of this salt were solved by X-ray diffraction t
echniques using 2634 counter data with I > 2 sigma(I). Refinement of 2
78 variables by full-matrix least squares converged at an agreement fa
ctor R = 0.023. Thermolysis of complex 1 in refluxing toluene led to i
ntermolecular elimination of t-BuC=CH, by combination of a t-BuC=C lig
and of one molecule of 1 with a proton from the CH2P2 group of a secon
d, and formation of the stable tetragold(I) complex Au-4(mu(3)-Ph(2)PC
HPPh(2))(mu-dppm)((C=Ct-Bu)(3)], 2, which was characterized by its spe
ctroscopic properties.