Fr. Heirtzler et al., METALLOCENOPHANES .7. PREPARATION AND CHARACTERIZATION OF THE DISILVER(I) COMPLEXES OF CONJUGATED POLYENES WITH [2.2.2]PARACYCLOPHANYL END-GROUPS, Chemische Berichte, 128(11), 1995, pp. 1079-1082
The preparation of the disilver(I) complexes 3 and 4, polyene metal co
mplexes that are terminally substituted with [2.2.2]paracyclophanyl un
its, is described. NMR spectroscopic studies on the disilver perchlora
te complex 3b showed that (a) the sites of complexation are the cyclop
hane groups and (b) the olefinic spacers do not overly perturb the ove
rall complexation properties of the individual [2.2.2]paracyclophanyl
groups. The crystal structures of the disilver hexafluoroantimonate co
mplexes 4a-b were determined. The use of the hexafluoroantimonate coun
terion and solvent mixtures containing toluene both proved crucial in
obtaining single crystals; toluene is incorportated into the crystal l
attices.