Wj. Evans et al., SYNTHESIS AND STRUCTURE OF A PENTAMETHYLCYCLOPENTADIENYL THULIUMCHLORIDE COMPLEX,[(C5ME5)(2)TM(MU(3)-CL)(2)K(THF)]N, Journal of coordination chemistry, 43(2-3), 1998, pp. 199-206
The first structural data on a pentamethylcyclopentadienyl complex of
thulium, [(C5Me5)(2)Tm(mu(3)-Cl)(2)K(THF)](n),1, are reported. TmCl3 r
eacts with 2 equivalents of KC5Me5 in THF to form 1 in>80% yield. 1 cr
ystallizes from THF/hexanes in the space group Cc with a = 11.1491(13)
Angstrom, b = 28.107(2) Angstrom, c = 8.5921(8) Angstrom, beta = 102.
485(8)degrees, V = 2628.8(4) Angstrom(3), and D-calcd = 1.570 Mg/m(3)
for Z = 4. Least squares refinement of the model based on 3114 reflect
ions (F-2 > 3.0 sigma(F-2)) converged to a final R-F = 1.9%. The polym
eric structure of 1 is generated by triply bridgingchlorides, each of
which is connected to one(C5Me5)(2)Tm bent metallocene unit and two K(
THF) moieties in a T-shaped geometry around the chloride.