Jl. Eglin et al., THE SYNTHESIS AND CHARACTERIZATION OF TRANS-RECL2(DPPE)(2) AND ALPHA-RE2CL4(DPPE)(2), Inorganica Chimica Acta, 268(1), 1998, pp. 151-157
Two rhenium compounds, alpha-Re2Cl4(dppe)(2) and trans-ReCl2(dppe)(2),
were isolated during the study of the reactivity of Re2Cl6-(P(n-Bu)(3
))(2) with the bidentate phosphine 1,2-bis(diphenylphosphino) ethane (
dppe) in the presence of acetonitrile, and a high yield synthetic rout
e was developed for alpha-Re2Cl4(dppe)(2). The structures of alpha-Re2
Cl4(dppe)(2) .(C6H6)(4), alpha-Re2Cl4(dppe)(2) .(dppe), and trans-ReCl
2(dppe)(2) . ((CH3)(2)CO)(2) were determined by X-ray crystallography
and the following data obtained: alpha-Re2Cl4(dppe)(2) .(C6H6)(4), mon
oclinic P2(1)/c, with a = 14.841(3), b = 12.161(4), c = 18.628(7) Angs
trom, beta = 95.33(3)degrees, V = 3348(2) Angstrom(3), Z = 2, R1 = 0.0
418, and wR2 = 0.1046; alpha-Re2Cl4(dppe)(2) .(dppe), monoclinic P2(1)
/c, with a = 10.695(3), b = 16.858(7), c = 19.710(7) Angstrom, beta =
101.78(1)degrees, V = 3479(2) Angstrom(3), 2=2, R1=0.0450, and wR2=0.1
023; trans-ReCl2(dppe)(2) .((CH3)(2)CO)(2), monoclinic P2(1)/c, with a
=11.507(3), b=13.519(3), c = 17.243(4) Angstrom, beta = 96.08(2)degree
s, V = 2667.3(11) Angstrom(3), Z = 2, R1 = 0.0369, wR2 = 0.0887. Addit
ional characterizations of alpha-Re2Cl4(dppe)(2) were performed with P
-31 NMR and UV-Vis spectroscopy. (C) 1998 Elsevier Science S.A.