SYNTHESIS AND SPECTROSCOPIC CHARACTERIZATION OF (CO)(6)FE-2(MU-EC(H)=C(H)E') (E-NOT-EQUAL-E' E,E'=S, SE, TE) AND (CO)(6)FE-2(MU-TEC(H)=C(H)TE) - STRUCTURAL CHARACTERIZATION OF (CO)(6)FE-2(MU-SC(PH)=C(H)SE) AND(CO)(6)FE-2(MU-SC(H)=C(PH)TE)
P. Mathur et al., SYNTHESIS AND SPECTROSCOPIC CHARACTERIZATION OF (CO)(6)FE-2(MU-EC(H)=C(H)E') (E-NOT-EQUAL-E' E,E'=S, SE, TE) AND (CO)(6)FE-2(MU-TEC(H)=C(H)TE) - STRUCTURAL CHARACTERIZATION OF (CO)(6)FE-2(MU-SC(PH)=C(H)SE) AND(CO)(6)FE-2(MU-SC(H)=C(PH)TE), Organometallics, 15(5), 1996, pp. 1356-1361
When acetylene gas was bubbled through methanol solutions containing t
he mixed-chalcogenide compounds (CO)(6)Fe-2(mu-EE') (E not equal E'; E
, E' = S, Se, Te), the acetylene adducts (Co)(6)Fe-2{mu-EC(H)=C(H)E'}
(1, 52%, E, E' = S, Se; 2, 46%, Et E' = S, Te; 3, 38%, E, E' = Se, Te)
were obtained, In addition, trace amounts of the homochalcogenide der
ivatives (CO)(6)Fe-2-{mu-EC(H)=C(H)E} (E = S, Se, Te) were also obtain
ed. The Te-2 compound (CO)(6)Fe-2{mu-TeC-(H)=C(H)Te) (4) was obtained
in 32% yield from the reaction of (CO)(6)Fe-2(mu-Te-2) with acetylene.
Compounds 1-4 were characterized by IR and H-1, C-13, Se-77, and Te-1
25 NMR spectroscopy. Crystallographic analysis of the phenylacetylene
adducts (CO)(6)Fe-2{mu-SC(Ph)=C(H)Se} (5) and (CO)(6)Fe-2(CO)(6)Fe-2{m
u-SC(H)=C(Ph)Te) (6) were carried out. The structures of both 5 and 6
can be described as Fe(2)SE (E = Se, Te) tetrahedral butterfly cores c
ontaining the phenylacetylene as a bridge between the two wingtip chal
cogen atoms, with three terminally bonded carbonyl groups on each Fe a
tom.