844
I.A.d Carcer, D.M. Heinekey / Journal of Organometallic Chemistry 694 (2009) 840–844
residue of S0(SiSH)2. Chromatography of the residue on a silica gel
column (particle size 40–63
ane afforded the product as a colorless viscous oil which solidified
Appendix A. Supplementary material
l
m; 4 cm ꢁ 25 cm) eluting with hex-
Supplementary data associated with this article can be found, in
upon standing. Yield: 4.2 g (80%).
2.4. [Fe(CO)2(S0SiS2)]2 (2)
References
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An ethereal solution (10 mL) containing 37 mg (0.14 mmol) of
[Fe(CO)3(PhCH@CHCOMe)] and 58 mg (0.14 mmol) of S’SiS2 was
stirred briefly, then set aside for 3 days. The red-brown crystals
which formed were washed twice with small portions of cold ether
(yield 60%). IR m
(CO): 2028, 1987 cmꢀ1(KBr). 1H NMR (CD2Cl2, d)
8.02 (d, 2H), 7.82 (d, 2H), 7,43 (d, 2H), 7.36 (t, 2H), 7.17 (d, 2H),
6.98 (t, 2H), 0.36 (s, 18H) and 0.14 (s, 18H). Anal. Calc. for C40H48O4-
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2.5. [Fe(CO)(S SiS2)]2 (3)
An ethereal solution (10 mL) containing 100 mg (0.4 mmol) of
[Fe(CO)3(PhCH@CHCOMe)] and 160 mg (0.4 mmol) of S’SiS2 was
degassed. The red solution was stirred overnight, with the color
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of pentane (yield 55%). IR(KBr) m .
(CO): 1980 cmꢀ1 1H NMR (CD2Cl2
d) 7.79(d, 2H), 7.68(d, 2H), 7.62(d, 2H), 7.49(d, 2H), 7.14(t, 2H),
7.11(t, 2H), 0.51(s, 18H), and 0.47 (s, 18H). Anal. Calc. for C38H48O2-
Fe2S6Si2: C, 47.87; H, 5.07; S, 20.18. Found: C, 47.73; H, 5.21; S,
19.95%.
Acknowledgement
This work was supported by the US National Science
Foundation.
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