24. Electrochemistry of Carbidopenta-ruthenium Complexes of C60 and Related Clusters

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author A. J. Babcock, J. Li, K. Lee, and J. R. Shapley
journal Organometallics, 2002, 21, 3940
link http://pubs.acs.org/doi/abs/10.1021/om020553d
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The electrochemical behavior of the face-coordinated C60-carbidopentaruthenium cluster complexes Ru5C(CO)11(PPh3)(μ3222-C60) (1), Ru5C(CO)10(μ-η11-dppf)(μ3222-C60) (2) (dppf = 1,1‘-bis(diphenylphosphino)ferrocene), and PtRu5C(CO)112-dppe)(μ3222-C60) (3) (dppe = 1,2-bis(diphenylphosphino)ethane) has been examined by cyclic voltammetry, rotating disk electrode voltammetry, and differential pulse voltammetry methods. The behavior of compounds Ru5C(CO)15 (4), Ru5C(CO)14(PPh3) (5), Ru5C(CO)13(μ-η11-dppf) (6), PtRu5C(CO)16 (7), and PtRu5C(CO)142-dppe) (8) was studied also for comparison. For both 1and 3, the voltammetric scans show an initial irreversible two-electron reduction feature, followed by three quasi-reversible, one-electron reductions of the C60 ligand. In contrast, similar scans for indicate an initial quasi-reversible, one-electron reduction of the C60 ligand that is dynamically coupled with a second one-electron, irreversible reduction. Stepwise reduction of the C60 ligand proceeds at more negative potentials. Interpretation of the electrochemical behavior of compounds 18 has been enhanced by studying their chemical reduction with cobaltocene. In all cases uptake of two electrons results in irreversible loss of a CO ligand from the cluster, and the resulting dianionic complexes have been characterized by their IR (νCO) spectra.

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    J. Am. Chem. Soc., 2003, 125, 6844
    A three-dimensional networked osmium nanomaterial (N-Os) was prepared by a thermal decomposition of Os3(CO)12 within mesopores of MCM-48. The novel N-Os species shows high catalytic activity and excellent reusability in the oxidat...
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    Adv. Mater., 2003, 15, 795
    Highly crystalline and monodisperse In2O3 nanoparticles have been prepared by thermal decomposition of In(acac)3 in oleylamine under inert atmosphere. The particle size of In2O3 can be easily manipulated by changing the experimental cond...
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    Thermal decomposition of W(CO)6 in oleylamine in the presence of mild oxidant Me3NO·2H2O produces tungsten oxide nanorods with diameters ranging from 3 to 6 nm. The size of nanorods can be easily varied by the employed surfactant ratio...
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    27. [60]Fullerene-Metal Cluster Complexes: Novel Bonding Modes and Electronic Communication

    K. Lee, H. Song, and J. T. Park
    Acc. Chem. Res., 2003, 36, 78
    [60]Fullerene can bind a variety of metal clusters via η2-C60, μ-η2:η2-C60, and μ3-η2:η2:η2-C60 π-type bonding modes. Multiple C60 additions to a single cluster core have also been demonstrated. Modification of the coordination sphere of clu...
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  14. 26. The first observation of four-electron reduction in [60]fullerene-metal cluster self-assembled monolayers (SAMs)

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    Chem. Commun., 2002, 2966
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  15. 25. Substitution Reaction of a m3-h1:h2:h1-C60 triosmium Cluster Complex and Formation of a Novel m3-h1:h1:h2-C60 Bonding Mode

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  16. 24. Electrochemistry of Carbidopenta-ruthenium Complexes of C60 and Related Clusters

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    The electrochemical behavior of the face-coordinated C60-carbidopentaruthenium cluster complexes Ru5C(CO)11(PPh3)(μ3-η2,η2,η2-C60) (1), Ru5C(CO)10(μ-η1,η1-dppf)(μ3-η2,η2,η2-C60) (2) (dppf = 1,1‘-bis(diphenylphosphino)ferrocene), and PtRu...
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  17. 23. Ligand-Induced Conversion of p to s C60-Metal Cluster Complexes: Full Characterization of the m3-h1,h2,h1-C60 Bonding Mode

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    The reaction of Os3(CO)9(μ3-η2:η2:η2-C60) (1) with PhCH2NPPh3 in chlorobenzene affords the benzyl isocyanide substituted product Os3(CO)8(CNR)(μ3-η2:η2:η2-C60) (2a, R = CH2Ph) in 76% yield. Photolysis of 1 in the presence of an excess of...
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  18. 22. [60]Fullerene as a Versatile Four-Electron Donor Ligand

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  19. 21. The First Fullerene-Metal Sandwich Complex: An Unusually strong Electronic Communication between Two C60 Cages

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  20. 20. Reversible Interconversion between m,h2,h2- and m3,h2,h2,h2-C60 on a Carbido Pentaosmium Cluster Framework

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    Decarbonylation of Os5(CO)14(PPh3) by 2 equiv of Me3NO/CH3CN at room temperature followed by reaction with C60 in refluxing chlorobenzene produces Os5C(CO)11(PPh3)(μ3,η2:η2:η2-C60) (1) in 44% yield. Thermal treatment of 1 at 80 °C under ...
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  21. 19. Synthesis and Characterization of m3-h2,h2,h2-C60 trirhenium Hydrido Cluster Complexes

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    The reaction of C60 with Re3(μ-H)3(CO)11(NCMe) in refluxing chlorobenzene produces Re3(μ-H)3(CO)9(μ3-η2,η2,η2-C60) (1) in 50% yield. Initial decarbonylation of 1 with Me3NO/MeCN followed by reaction with PPh3 in boiling chlorobenzene aff...
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  22. 18. First Example of the μ3-η1,η2,η1-C60 Bonding Mode: Ligand-Induced Conversion of π to σ C60–Metal Complexes

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    A boat-shaped 1,4-cyclohexadiene-like ring is present in the C60 molecule with a novel σ-typeμ3-η1,η2,η1 bonding mode in the clusters 2 a and 2 b. The change in coordination mode was induced by insertion of an RNC ligand into an Os−Os bo...
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    Reaction of GaMe3 with N,N-dimethylethylenediamine (DMEDA) produces adducts, Me3Ga:NH2C2H4NMe2 (1:1, 1) and Me3Ga:NH2C2H4NMe2:GaMe3 (2:1, 2). A fast concerted intermolecular exchange of the two inequivalent GaMe3 moieties occurs in 2 at ...
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    14. Fluxional Processes and Structural Characterization of m3-h2,h2,h2-C60 triosmium Cluster Complexes, Os3(CO)9-n(PMe3)n(m3-h2,h2,h2-C60) (n=1,2,3)

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  29. 11. Synthesis, Structure, and Electrochemical Studies of m3-h2,h2,h2-C60 triosmium Complexes

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    Two μ3-η2,η2,η2-C60 complexes, Os3(CO)8(PPh3)(μ3-η2,η2,η2-C60) (8) and Os3(CO)7(PMe3)2(μ3-η2,η2,η2-C60) (9), have been prepared by decarbonylation of Os3(CO)9(μ3-η2,η2,η2-C60) (6) with Me3NO/MeCN in the presence of phosphine ligands. The...
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  30. 10. Substitution Site Specificity on the Ru10C2 Cluster Framework. Multiple Convergent Pathways to the Mixed Hydrocarbon Ligand Derivative Ru10C2(CO)21(NBD)(C2Ph2)

    K. Lee and J. R. Shapley
    Organometallics, 1998, 17, 4368-4373
    The substitution of carbonyl ligands in the edge-shared bioctahedral cluster [PPN]2[Ru10C2(CO)24] by two types of 4e donor π-bonding ligands, viz., a diene (norbornadiene) and an alkyne (diphenylacetylene), has been investigated under va...
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  31. 9. Reversible transformation between Methylene and Methylidyne-Hydride on the Ru10C2 Framework

    K. Lee, S. R. Wilson, and J. R. Shapley
    Organometallics, 1998, 17, 4113
    Oxidative substitution of [Ru10C2(CO)22(NBD)]2- with ferrocenium/diazomethane forms a methylene derivative, Ru10C2(CO)22(NBD)(CH2), in which the methylene ligand symmetrically bridges two adjacent apical ruthenium centers in the e...
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  32. 8. Substitution of [Ru10C2(CO)24]2- with Allene. Reversible Formation of [Ru10C2(CO)22(C3H4)2- and [Ru10C2(CO)20(C3H4)2]2

    K. Lee and J. R. Shapley
    Organometallics, 1998, 17, 4030
    Substitution of carbonyl ligands in [Ru10C2(CO)24]2- (1) by allene proceeds cleanly in diglyme at 90 °C (1 atm) to afford the monosubstituted derivative [Ru10C2(CO)22(μ-η2:η2-C3H4)]2- (2). Treatment of either 1 or 2 with allene at...
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  33. 7. Face Coordinated C60 Complexes with Carbido Pentaruthenium Cluster Cores including a Bimetallic Platinum-Pentaruthenium Complex

    K. Lee and J. R. Shapley
    Organometallics, 1998, 17, 3020
    Interaction of C60 with Ru5C(CO)15 or PtRu5C(CO)14(COD) in hot chlorobenzene, followed by treatment with solubilizing phosphines, provides compounds with hexahapto coordination of C60 to a Ru3 face of the square pyramidal Ru5C or octahed...
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    6. High Nuclearity Hydridodecaruthenium Clusters

    M. P. Cifuentes, M. G. Humphrey, J. R. Shapley, K. Lee
    Inorg. Synth., 1998, 32, 287
    Read More
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    5. Tri(μ-carbonyl)Nonacarbonyltetrarhodium, Rh4(μ-CO)3(CO)9

    Ph. Serp, Ph. Kalck, R. Feurer, R. Morancho, K. Lee, J. R. Shapley
    Inorg. Synth., 1998, 32, 284
    Read More
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    4. Platinum-Ruthenium Carbonyl Cluster Complexes

    R. D. Adams, T. S. Barnard, J. E. Cortopassi, W. Wu, Z. Li, J. R. Shapley, K. Lee
    Inorg. Synth., 1998, 32, 280
    Read More
  37. 3. Oxidative Substitution of [Ru10C2(CO)24]2- with Disubstituted Alkynes. Facile Formation and Reduction of Ru10C2(CO)23(C2RR')

    J. W. Benson, T. Ishida, K. Lee, S. R. Wilson, and J. R. Shapley
    Organometallics, 1997, 16, 4929
    Oxidation of the decaruthenium carbonyl cluster [Z]2[Ru10C2(CO)24] (1) (Z+ = PPN+, Et4N+) with [Cp2Fe][BF4] (2 equiv) at room temperature in the presence of disubstituted alkynes forms the neutral derivatives Ru10C2(CO)23(C2RR‘) (2, R, R...
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    2. Coordination of C60 to Penta- and Hexaruthenium Cluster Frames

    K. Lee, H.-F. Hsu, and J. R. Shapley
    Organometallics, 1997, 16, 3876
    In refluxing chlorobenzene C60 reacts with Ru5C(CO)15 or with Ru6C(CO)17 to form new complexes, which are isolated following treatment with tertiary phosphines to give the structurally characterized, facebonded derivatives Ru5C(CO)11(PPh...
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    1. Characterization and structures of intermediates in the reactivity of CpWOs3(CO)11(μ3-CTol) towards dihydrogen and water

    J. T. Park, J.-H. Chung, H. Song, K. Lee, J.-H. Lee, J.-R. Park, and I.-H. Suh
    J. Organomet. Chem., 1996, 526, 215
    Initial decarbonylation of CpWos3(Co)11(μ3-CTol) (1: Cp = η5-C5H5, Tol = p-C6H4Mc) with the Me3NO/MeCN followed by reaction with dihydrogen and water produces a dihydrido comlex CpWOs3(CO)10(μ3-CTol)(μ-H)2 (2), a ‘butterfly’ cluster with a 6...
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