Abstract
The complexes [(OC)4Os(PbMe2)]2 (3) and [(OC)4OsSnBu ′2 ]2 (4) have been prepared from be reaction of Na2[Os(CO)4] with Me2PbCl2 and Bu ′2 SnCl2, respectively, in THF and their X-ray crystal structures determined. The red derivative,3, was light-sensitive in solution. The reactions or [(OC)4 Os(SnMe2)]2 (2), or its decarbonylated derivative [Os3(CO)7(SnMe2)2]2 (7), with olefins or phosphorus donor ligands have also been investigated, and the structures of two derivatives, viz. [Os2(CO)7(SnMe2)2(C2H4)] (5a) and [Os2(CO)7(SnMe2)2(PMe3)] (6a), have been determined; the noncarbonyl ligand occupies an equatorial site in each case. The X-ray crystal structures of all these compounds, like those of [(OC)4Os(EMe2)]2 (E=Ge (1), Sn (2)) which have been reported previously, show leaning of the axial carbonyl ligands toward the metal tetracycle, i.e., an “umbrella” effect. Crystallographic data for compound3: space group, P21/a;a=13.4404(13) Å,b=10.7494(14) A,c=148967(18) A,β=98.204(9)°,R=0.035, 1983 observed reflections. For compound4: space group,P1;a=9.016(1) Å,b=9.370(1),c=11.334(1) A, α=103.67(1)°,β=100.30(1)°, γ=115.03(1)°, R=0.046, 2026 observed reflections. For compound5a: space group,P1;a=9.2933(11)Å,b=9.7181(3),c=12.2508(15) A, α=89.21(1)°,β=87.61(1)°, γ=86.13(1)°,R=0.038, 2770 observed reflections. For compound6a space groupP1:a=8.7244(9)Å,b=10.9318(6),c=13.2560(13) A, α=87.815(6)°,β=83.655(8)°, γ=82.343(6)°, R=0.030, 3497 observed reflections.
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Leong, W.K., Einstein, F.W.B. & Pomeroy, R.K. Synthesis and structure of [(OC)4Os(PbMe2)]2 and some derivatives of the type Os2(CO)7(SnMe2)2(L). J Clust Sci 7, 121–143 (1996). https://doi.org/10.1007/BF01166052
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DOI: https://doi.org/10.1007/BF01166052