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Hydrogen Activation by Arene Ruthenium Complexes in Aqueous Solution. Part 2. Build-up of Cationic Tri- and Tetra-nuclear Ruthenium Clusters with Hydrido Ligands

DOI: 10.1039/DT9940003215

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 3215 - 3224 (1994)

Update date:2022-08-16

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Authors:

Meister, GoetzMeister, Goetz

Rheinwald, GerdRheinwald, Gerd

Stoeckli-Evans, HelenStoeckli-Evans, Helen

Suess-Fink, GeorgSuess-Fink, Georg

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Article abstract of DOI:10.1039/DT9940003215

The low-pressure hydrogenation of the hydrolysis mixture of 6-C6H6)2Cl4> in water (1.5 atm, 20 deg C) led, in the presence of NaClO4, to the oxo-capped trinuclear cluster cation 6-C6H6)3(μ-Cl)(μ3-O)(μ-H)2>(1+) 1 which crystallized as the perchlorate salt.The chloro-capped trinuclear cluster cation 6-C6H2Me-1,2,4,6)3(μ3-Cl)H3>(2+) 2, crystallized as the dichloride, was accessible from the durene derivative 6-C6H2Me-1,2,4,6)2Cl4> by high-pressure hydrogenation (60 atm, 55 deg C) in water.In hot aqueous solution, the chloro-capped cluster 2 underwent hydrolysis to give the oxo-capped cluster 6-C6H2Me4-1,2,4,6)3(μ3-O)H3>(1+) 3.In the presence of NaBF4, the low-pressure hydrogenation (1.5 atm, 20 deg C) of the hydrolysis mixture of 6-C6H6)2Cl4> led to the tetranuclear tetrahydrido cluster cation 6-C6H6)4H4>(2+) 4 which precipitated as the tetrafluoroborate salt.Under high-pressure conditions (60 atm, 55 deg C) and in the absence of an additional salt, the hexahydrido cluster cation 6-C6H6)4H6>(2+) 5 was formed and obtained as the dichloride.By analogy, the p-cymene derivative 6-C6H4MePri-p)2Cl4> gave 6-C6H4MePri-p)4H6>(2+) 6.In contact with air, the hexahydrido clusters 5 and 6 were transformed into the corresponding tetrahydrido clusters 6-C6H6)4H4>(2+) 4 and 6-C6H4MePri-p)4H4>(2+) 7.The hexahydrido cluster 5 is capable of hydrogenating fumaric acid to give succinic acid and 4; the latter adds molecular hydrogen to regenerate the hexahydrido species 5.The crystal and molecular structures of the cluster salts 6-C6H6)3(μ-Cl)(μ3-O)(μ-H)2>ClO4 (cation 1), 6-C6H2Me4-1,2,4,6)3(μ3-O)H3>BF4 (cation 3), 6-C6H6)4H4>Cl2 (cation 4) and 6-C6H4MePri-p)4H6>2 (cation 6) have also been determined.

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