S. Suravajjala et al., BIS(ARENE) COMPLEXES OF RU(II) - SYNTHESIS, CRYSTAL-STRUCTURE AND ELECTROCHEMICAL-BEHAVIOR OF [BIS(ETA(6)-P-ISOPROPYLTOLUENE)RU][BF4](2), Journal of organometallic chemistry, 461(1-2), 1993, pp. 201-205
Cleavage of the chloro-bridged Ru-II dimer, [(p-isopropyltoluene)Ru(Cl
)(2)](2) with AgBF4 in acetone and refluxing the product in trifluoroa
cetic acid with an excess of p-isopropyltoluene leads to the formation
of the dicationic bis(arene) Ru-II complex, [(p-isopropyltoluene)(2)R
u][BF4](2), in nearly quantitative yield. Strong upfield shifts are ob
served in the C-13 NMR spectrum of the arene carbon atoms of p-isoprop
yltoluene following coordination and an investigation of the electroch
emistry of this complex shows that it undergoes an irreversible reduct
ion in nitromethane solvent at -0.78 V versus an Ag/AgCl reference ele
ctrode. An X-ray crystal structure determination of the complex shows
that the complex consists of a Run center located between two p-isopro
pyltoluene ligands that are coordinated in an eta(6) manner. The arene
rings are separated by a distance of 3.450 Angstrom and are essential
ly coplanar with a dihedral angle of 178.4 degrees. The crystals are m
onoclinic, space group P2(1)/n wth lattice constants a = 10.094(2) Ang
strom, b = 12.996(3) Angstrom, c = 17.371(3) Angstrom, beta = 94.90(1)
degrees and V = 2270.4(8) Angstrom(3). Convergence to conventional R v
alues of R = 0.0711 and R(W) = 0.0854 with a goodness-of-fit of 1.15 w
as obtained for 280 variable parameters and 2976 reflections with I >
0 sigma(I).