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- Johnson, Brian F G, et al.
(författare)
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Systematic Synthesis of Substituted Phosphido-bridged Osmium Clusters
- 1996
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Ingår i: Journal of the Chemical Society, Dalton Transactions. - 0300-9246. ; , s. 755-763
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Tidskriftsartikel (refereegranskat)abstract
- The labilised clusters [Os3(CO)11–nLn(NCMe)][n= 1, L = PMe3 or CNBut; n= 2, L = P(OMe)3] have been prepared. The reaction of [Os3(CO)11 –nLn(NCMe)] or [Os3(CO)10{P(OMe)3}(NCMe)] with either [Os3(CO)11(PH3)] or [Os3(µ-H)(CO)10(µ-PH2)] led to the formation of the phosphide-bridged clusters [Os6(µ-H)(CO)21{P(OMe)3}(µ-PH2)], [Os6(µ-H)(CO)21(PMe3)(µ-PH2)], [Os6(µ-H)(CO)21(CNBut)(µ-PH2)], [Os6(µ-H)(CO)20{P(OMe)3}2(µ-PH 2)] and the corresponding phosphinidene-bridged clusters [Os6(µ-H)2-(CO)21 –nLn(µ3-PH)][n= 1, L = CNBut; n= 2, L = P(OMe)3] in good yield. The Os6 clusters have been fully characterised on the basis of their spectroscopic data and the molecular structures of three have been established by single-crystal X-ray analysis. The structures of [Os6(µ-H)(CO)20{P(OMe)3}2(µ-PH 2)] and [Os6(µ-H)2(CO)19{P(OMe)3}2(µ3-PH)] differ from those of previously studied hexanuclear phosphide- and phosphinidene-bridged clusters; this difference is attributed to the steric influence of the relatively bulky phosphite ligands. Proton and phosphorus NMR spectroscopy indicate that both these clusters exist in two isomeric forms in solution.
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2. |
- Nordlander, Ebbe, et al.
(författare)
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The Crystal and Molecular Structure of HOs6(CO)21(NCMe)PH2
- 1997
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Ingår i: Polyhedron. - 0277-5387. ; 16:19, s. 3463-3467
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Tidskriftsartikel (refereegranskat)abstract
- The crystal structure of the phosphide-bridged cluster [Os6(μ-H)(CO)12(NCMe)(μ-PH2)] 4 has been determined. The cluster consists of two Os3 triangles which are linked by a PH2 moiety which is terminally bound to each triangle. The acetonitrile ligand is axially coordinated and the hydride bridges the Os---Os edge to which the phosphide moiety and the acetonitrile are coordinated. The molecular structure of 4 resembles those of the related clusters [Os6(μ-H)(CO)22(μ-PH2)] 1 and [Os6(μ-H)(CO)21(CNBut)(μ-PH2)] 2 although the dihedral angles between the two osmium triangles vary for 1, 2 and 4. The relative orientation of the two linked metal triangles in 4 (as well as 1 and 2) differs from that of the phosphite-substituted analogue [Os6(μ-H)(CO)20{P(OMe)3}2(μ-PH2)]3; this difference is attributed to steric factors.
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