Journal of the Chemical Society, Dalton Transactions p. 1133 - 1144 (1996)
Update date:2022-09-26
Topics:
Cardin, Christine J.
Cardin, David J.
Convery, Maire A.
Dauter, Zbigniew
Fenske, Dieter
Devereux, Michael M.
Power, Michael B.
Title full: New ruthenium-tin clusters with bulky ligands. Crystal and molecular structures of [Ru2(CO)6(μ-SnR2)(μ-Ph 2PCH2PPh2)], [Ru3(CO)9(μ-SnR′2)3], [Ru3(CO)9(μ-SnR2)μ-SnR′ 2]2 and [Ru3(CO)9(μ-SnR2) 2(μ-SnR′2)] [R = CH(SiMe3)2, R′= C6H2Pri3-2,4,6]. The first heterometallic clusters containing the SnR′2 (R′ = 2,4,6-triisopropylphenyl) moiety have been prepared. Triruthenium dodecacarbonyl reacted at low temperatures with SnR′2 or, at higher temperatures, with its trimer (SnR′2)3 to give both [Ru3(CO)10(μ-SnR′2)2] 1 and [Ru3(CO)9(μ-SnR′2)3] 2. Reaction of the pentametallic species [Ru3(CO)10(μ-SnL2)2] [L = R = CH(SiMe3]2 3 or R′] with SnR′2 or SnR2 respectively afforded the hexametallic clusters [Ru3(CO)9(μ-SnR2)(μ-SnR′ 2)2] 4 and [Ru3(CO)9(μ-SnR2) 2(μ-SnR′2)] 5. In the reaction of [Ru3(CO)12] with SnR2 the hexametallic cluster [Ru3(CO)9(μ-SnR2)3] 6 has now been isolated in addition to the previously reported Ru3Sn2 cluster. The trimer (SnR′2)3 also reacted with [Ru3(CO)10(dppm)] (dppm = Ph2PCH2PPh2) to give [Ru3(CO)8(μ-SnR′2)2(dppm)] 7, whereas with SnR2 the product was [Ru2(CO)6(μ-SnR2)(μ-dppm)] 8. Compound 7 can also be obtained by the reaction of 2 with dppm, using sodium-benzophenone to activate the cluster. Reaction of the dodecacarbonyl with Sn[CH(PPh2)2]2 or its lead analogue surprisingly did not yield a mixed cluster, but afforded a rapid and quantitative route to [Ru3(CO)10(dppm)]. Compound 2 behaves similarly, yielding 7 again in high yield. The crystal and molecular structures of 2,4, 5 and 8 have been determined. In compounds 2,4 and 5, the ruthenium triangle and the three tin atoms form a planar array. A detailed comparison of ligand steric effects is made. In 8 the metal atoms and the two P atoms are coplanar, with a long Ru-Ru vector bridged by the R2Sn group and the diphosphine [2.954(2) A]. The structure of 4 is unusual, the characteristic aryltin twist on only two of the three tin atoms generating chirality, resulting in a spiral packing in space group P65. This structure was determined both diffractometrically and using two different image-plate systems, and the results are remarkably consistent in all three cases.
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