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SHOSHKIN et al.
vacuum for 20 min at room temperature and for 4 h
at 150 C. Cp2Yb (0.40 g, 97%) was obtained as a
brick red diamagnetic solid unstable in air. The IR
spectrum of the product is identical to that of an
authentic sample [6]. Found Yb, %: 57.00. C10H10Yb.
Calculated Yb, %: 57.06. The hexane extracts were
combined, and the solvent was evaporated to leave
0.67 g (94%) of PPh3.
room temperature. CpSmI2(THF)2 (0.71 g, 89%) was
obtained as a yellow solid unstable in air. The effec-
tive magnetic moment (1.8 BM) corresponds to Sm3+.
1
IR spectrum, , cm : C5H5, 1430 m, 1010 s, 770 s,
620 s; coordinated THF, 1040 m, 925 m, 870 m.
Found Sm, %: 24.31. C13H21I2O2Sm. Calculated Sm,
%: 24.51. The hexane extracts were combined, and
the solvent was vacuum-evaporated to leave 0.32 g
(94%) of PPh3.
The reactions of CpCuPPh3 with Pr and Er were
performed similarly. From 0.92 g of CpCuPPh3 and
2.0 g of Pr, 0.25 g (95%) of Cp3Pr was obtained. The
IR spectrum of the product is identical to that of an
authentic sample [7]. Found Pr, %: 41.89. C15H15Pr.
Calculated Pr, %: 41.91. From 0.90 g of CpCuPPh3
and 1 g of Er, 0.20 g (74%) of Cp3Er was obtained.
The IR spectrum of the product is identical to that
of an authentic sample [7]. Found Er, %: 46.07.
C15H15Er. Calculated Er, %: 46.13.
CpCuPPh3. A colorless solution of 1.92 g of PPh3
in 10 ml of THF and 0.41 g of CpH were added to a
light yellow solution of 1.00 g of t-BuOCu in 10 ml
of THF. The mixture was kept for 5 h at room tem-
perature. The solution gradually became colorless.
The solvent was removed by vacuum evaporation, and
the residue was washed with 20 ml of hexane and
vacuum-dried. CpCuPPh3 (2.80 g, 98%) was obtained
as a colorless solid unstable in air. The IR spectrum
of the product is identical to that of an authentic
sample [4]. Found Cu, %: 16.15. C23H20CuP. Calcu-
lated Cu, %: 16.25. In the volatile products, 0.51 g
(96%) of t-BuOH was detected by GLC.
Reaction of Cp2Yb with CpCuPPh3. A colorless
solution of 0.38 g of CpCuPPh3 in 10 ml of THF was
added to a dark red solution of 0.30 g of Cp2Yb in
5 ml of THF. The reaction mixture became dark
green, and a fine black precipitate formed. The mix-
ture was kept for 12 h at room temperature for the
reaction completion. The precipitate was separated by
centrifugation. In the precipitate, 0.052 g (84%) of
metallic copper was found. From the supernatant, the
solvent was removed by vacuum evaporation, and the
residue was washed with hexane (4 20 ml) and
vacuum-dried. Cp3Yb(THF) (0.33 g, 77%) was ob-
tained as a dark green solid unstable in air. The effec-
tive magnetic moment (4.4 BM) corresponds to Yb3+.
ACKNOWLEDGMENTS
The study was financially supported by the Russian
Foundation for Basic Research (project no. 99-03-
32906).
REFERENCES
1. Bochkarev, M.N., Zakharov, L.N., and Kalinina, G.S.,
in Organoderivatives of Rare Earth Elements,
Dordrecht: Kluwer Academic, 1995.
1
IR spectrum, , cm : C5H5, 3070 m, 1430 m, 1010 s,
2. Bochkarev, L.N., Druzhkova, O.N., Zhiltsov, S.F., Za-
kharov, L.N., Fukin, G.K., Khorshev, S.Ya., Yanov-
sky, A.I., and Struchkov, Yu.T., Organometallics, 1997,
vol. 16, no. 4, pp. 500 502.
770 s, 620 s; coordinated THF, 1070 m, 925 m,
890 m, 860 m. Found Yb, %: 39.0. C19H23OYb. Cal-
culated Yb, %: 39.32. The hexane extracts were com-
bined, and the solvent was vacuum-evaporated to
leave 0.21 g (83%) of PPh3.
3. Orlov, N.A., Bochkarev, L.N., Nikitinsky, A.V., Zhil-
tsov, S.F., Zakharov, L.N., Fukin, G.K., and Khor-
shev, S.Ya., J. Organomet. Chem., 1997, vol. 547,
no. 1, pp. 65 69.
Reaction of CpCuPPh3 with SmI2(THF)4. A
colorless solution of 0.51 g of CpCuPPh3 in 10 ml of
THF was added to a dark green solution of 0.91 g of
SmI2(THF)4 in 5 ml of THF. The mixture was kept
for 10 h at room temperature. The solution became
yellow-green, and a fine black precipitate formed,
which was separated by centrifugation. In the precip-
itate, 0.075 g (91%) of metallic copper was found.
From the supernatant, the solvent was removed by
vacuum evaporation, and the residue was washed with
hexane (4 20 ml) and vacuum-dried for 20 min at
4. Cotton, F.A. and Marks, T.J., J. Am. Chem. Soc., 1970,
vol. 92, no. 17, pp. 5114 5117.
5. Protchenko, A.V. and Bochkarev, M.N., Prib. Tekh.
Eksp., 1990, no. 1, p. 194.
6. Calderazzo, F., Pappalardo, R., and Losi, S., J. Inorg.
Nucl. Chem., 1966, vol. 28, p. 987.
7. Birmingham, J.M. and Wilkinson, G., J. Am. Chem.
Soc., 1956, vol. 78, p. 42.
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 72 No. 5 2002