Km. Carlsonday et al., THE SYNTHESIS AND CHARACTERIZATION OF ALPHA-RE2CL4(DEPE)(2) AND ALPHA-W2CL4(DEPE)(2), Inorganica Chimica Acta, 271(1-2), 1998, pp. 49-56
The synthesis of both alpha-Re2Cl4(depe)(2), where depe is the bidenta
te phosphine 1,2-bis(diethylphosphino)ethane, and alpha-W2Cl4(depe)(2)
allows the comparison of the crystallographic and spectroscopic prope
rties of these two new compounds. Characterization methods for alpha-R
e2Cl4(depe)(2) and alpha-W2Cl4(depe)(2) include P-31{H-1} NMR spectros
copy, UV-Vis spectroscopy and X-ray crystallography. In addition to al
pha-W2Cl4(depe)(2), both cationic and anionic tungsten complexes witho
ut metal-metal bonding were isolated and structurally characterized. C
rystallographic data for alpha-Re2Cl4(depe)(2), alpha-W2Cl4(depe)(2) a
nd [WOCl(depe)(2)](2)[(WOCl4(OP(CH2CH3)(2)CH2))(2)] are as follows: P2
(1)/c (No. 14) with a=10.416(2), b=16.315(3), c=10.176(2) Angstrom, be
ta=119.15(1)degrees, V=1510.2(5) Angstrom(3), Z=2, R1=0.0340 and wR2=0
.0875; C2/c (No. 15) with a=18.6359(6), b=10.2959(3), c=16.0190(5) Ang
strom, beta=91.129(1)degrees, V=3073.0(2) Angstrom(3), Z=2, R1=0.0488
and wR2=0.0948; and P2(1)/n (No. 14) with a=14.563(3), b=14.893(2), c=
20.330(4) Angstrom, beta=93.54(2)degrees, V=4401(1) Angstrom(3), Z=4,
R1=0.0522 and wR2=0.1354, respectively. (C) 1998 Elsevier Science S.A.