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Journal of Chemical Crystallography

, Volume 39, Issue 11, pp 812–819 | Cite as

Spectroscopic and X-ray Diffraction Data on Three Novel Trimetallic Clusters from Thermally Promoted Ligand Substitution in the Tetrahedrane Clusters MeCCo2MoCp(CO)8 and PhCCo2Mo(η5-C5H4CHO)(CO)8

  • Weiqiang Zhang
  • William H. Watson
  • Michael G. Richmond
Original Paper
  • 50 Downloads

Abstract

The reaction between the ethylidyne-substituted cluster MeCCo2MoCp(CO)8 (1) and the diphosphine ligand 2,3-bis(diphenylphosphino)maleic anhydride (bma) in refluxing CH2Cl2 has been investigated and found to afford the new mixed-metal clusters MeCCo2MoCp(CO)6[trans-2,3-bis(diphenylphosphino)succinic anhydride] (2) and Co2MoCp(CO)5[μ-C(Me)C=C(PPh2)C(O)OC(O)](μ-PPh2) (3), with the latter cluster representing the principal reaction product. Refluxing 1 with bma in either 1,2-dichloroethane or toluene yields only 3. The tetrahedrane cluster PhCCo2Mo(η5-C5H4CHO)(CO)8 (4), which contains a formyl-substituted cyclopentadienyl ring, has also been examined with added bma in refluxing CH2Cl2 and found to give only Co2Mo(η5-C5H4CHO)(CO)5[μ-C(Ph)C=C(PPh2)C(O)OC(O)](μ-PPh2) (5). All three products have been isolated and characterized spectroscopically in solution, and each molecular structure has been determined by X-ray crystallography. Cluster 2 contains a bridging diphosphine ligand with a succinic anhydride ring that results from the formal reduction of the maleic anhydride platform of the bma ligand, while clusters 3 and 5 each exhibit triangular Co2Mo cores, whose one face is capped by a 6e- C(R)C=C(PPh2)C(O)OC(O) [where R = Me (3), Ph (5)] ligand. The observed substitution products are discussed as a function of the capping carbyne group, ancillary polyene ligand, and related derivatives prepared by our groups.

Graphical Abstract

Thermolysis of the mixed-metal cluster MeCCo2MoCp(CO)8 (1) with bma in CH2Cl2 furnishes the new clusters MeCCo2MoCp(CO)6[trans-2,3-bis(diphenylphosphino)succinic anhydride] (2) and Co2MoCp(CO)5[μ-C(Me)C=C(PPh2)C(O)OC(O)](μ-PPh2) (3) as the minor and major products, respectively. The reaction between bma and the related benzylidyne-capped cluster PhCCo2Mo(η5-C5H4CHO)(CO)8 (4), which contains a formyl-substituted cyclopentadienyl ring, has also been examined and found to afford only Co2Mo(η5-C5H4CHO)(CO)5[μ-C(Ph)C=C(PPh2)C(O)OC(O)](μ-PPh2) (5) in moderate yield.

Keywords

Mixed-metal clusters Tetrahedrane clusters Diphosphine ligand P–C bond activation Carbyne ligand reactivity 

Notes

Acknowledgments

Financial support from the Robert A. Welch Foundation (Grants P-0074-WHW and B-1093-MGR) is appreciated.

References

  1. 1.
    Albano VG, Braga D, Ros R, Scrivanti A (1985) Chem Commun 866Google Scholar
  2. 2.
    Bruce MI, bin Shawkataly O, Snow MR, Tiekink ERT (1986) Aust J Chem 39:1109Google Scholar
  3. 3.
    Yang K, Bott SG, Richmond MG (1993) J Organomet Chem 454:273CrossRefGoogle Scholar
  4. 4.
    Acum GA, Mays MJ, Raithby PR, Solan GA (1996) J Organomet Chem 508:137CrossRefGoogle Scholar
  5. 5.
    Choi YY, Wong WT (1997) J Organomet Chem 542:121CrossRefGoogle Scholar
  6. 6.
    Hui BKM, Wong WT (1998) J Chem Soc Dalton Trans 447Google Scholar
  7. 7.
    Bott SG, Yang K, Huang SH, Richmond MG (2004) J Chem Crystallogr 34:883CrossRefGoogle Scholar
  8. 8.
    Watson WH, Wu G, Richmond MG (2005) Organometallics 24:5431CrossRefGoogle Scholar
  9. 9.
    Richmond MG, Kochi JK (1987) Organometallics 6:254CrossRefGoogle Scholar
  10. 10.
    Shiu KB, Peng SM, Cheng MC (1993) J Organomet Chem 453:133CrossRefGoogle Scholar
  11. 11.
    Farrugia LJ, McDonald N, Peacock RD (1994) J Cluster Sci 5:341CrossRefGoogle Scholar
  12. 12.
    Watson WH, Kandala S, Richmond MG (2005) J Chem Crystallogr 35:157CrossRefGoogle Scholar
  13. 13.
    Watson WH, Kandala S, Richmond MG (2006) J Chem Crystallogr 36:813CrossRefGoogle Scholar
  14. 14.
    Yang K, Smith JM, Bott SG, Richmond MG (1993) Organometallics 12:4779CrossRefGoogle Scholar
  15. 15.
    Xia CG, Yang K, Bott SG, Richmond MG (1996) Organometallics 15:4480CrossRefGoogle Scholar
  16. 16.
    Bott SG, Yang K, Talafuse KA, Richmond MG (2003) Organometallics 22:1383CrossRefGoogle Scholar
  17. 17.
    Bott SG, Yang K, Richmond MG (2005) J Organomet Chem 690:3067CrossRefGoogle Scholar
  18. 18.
    Bott SG, Yang K, Richmond MG (2006) J Organomet Chem 691:3771CrossRefGoogle Scholar
  19. 19.
    Zhang W, Watson WH, Richmond MG (2008) J Chem Crystallogr 38:437CrossRefGoogle Scholar
  20. 20.
    Seyferth D, Rudie CN, Merola JS (1978) J Organomet Chem 162:89CrossRefGoogle Scholar
  21. 21.
    Nestle MO, Hallgren JE, Seyferth D (1980) Inorg Synth 20:226CrossRefGoogle Scholar
  22. 22.
    Beurich H, Blumhofer R, Vahrenkamp H (1982) Chem Ber 115:2409CrossRefGoogle Scholar
  23. 23.
    Blumhofer R, Fischer K, Vahrenkamp H (1986) Chem Ber 119:194CrossRefGoogle Scholar
  24. 24.
    Jensen S, Robinson BH, Simpson J (1983) Chem Commun 1081Google Scholar
  25. 25.
    Wu HP, Yin YQ, Huang XY (1997) Inorg Chim Acta 255:167CrossRefGoogle Scholar
  26. 26.
    Hart WP, Macomber DW, Rausch MD (1980) J Am Chem Soc 102:1196CrossRefGoogle Scholar
  27. 27.
    Fenske D, Becher HJ (1975) Chem Ber 119:2115CrossRefGoogle Scholar
  28. 28.
    Shriver DF (1969) The manipulation of air-sensitive compounds. McGraw-Hill, New YorkGoogle Scholar
  29. 29.
    SAINT Version 6.02, Bruker advanced analytical X-ray systems, Inc. Copyright 1997–1999Google Scholar
  30. 30.
    SHELXTL Version 5.1, Bruker advanced analytical X-ray systems, Inc. Copyright 1998Google Scholar
  31. 31.
    PLATON—a multipurpose crystallographic tool (2001) Spek AL, Utrecht University, Utrecht, The NetherlandsGoogle Scholar
  32. 32.
    Coltrup NB, Daly LH, Wiberly SE (1990) Introduction to infrared and Raman spectroscopy. Academic Press, New YorkGoogle Scholar
  33. 33.
    Avey A, Schut DM, Weakley TJR, Tyler DR (1993) Inorg Chem 32:233CrossRefGoogle Scholar
  34. 34.
    Shen H, Wang JC, Bott SG, Richmond MG (1997) J Chem Crystallogr 27:649CrossRefGoogle Scholar
  35. 35.
    Watson WH, Chen T, Richmond MG (2004) J Chem Crystallogr 34:797CrossRefGoogle Scholar
  36. 36.
    Mingos DMP, Wales DJ (1990) Introduction to cluster chemistry. Prentice-Hall, New JerseyGoogle Scholar
  37. 37.
    Beurich H, Vahrenkamp H (1982) Chem Ber 115:2385CrossRefGoogle Scholar
  38. 38.
    Shimomura H, Lei X, Shang M, Fehlner TP (1997) Organometallics 16:5302CrossRefGoogle Scholar
  39. 39.
    Zhang YH, Liu P, Xia CG, Hu B, Yin YQ (2003) J Organomet Chem 676:55CrossRefGoogle Scholar
  40. 40.
    Song LC, Zhu WF, Hu QM, Wu H, Yu GA (2003) J Organomet Chem 667:143CrossRefGoogle Scholar
  41. 41.
    Huang H, Hughes RP, Landis CR, Rheingold AL (2006) J Am Chem Soc 128:7454CrossRefGoogle Scholar
  42. 42.
    Adams H, Guio LVY, Morris MJ, Spey SE (2002) J Chem Soc Dalton Trans 2907Google Scholar
  43. 43.
    Zhang J, Zhang YH, Chen XN, Ding ER, Yin YQ (2000) Organometallics 19:5032CrossRefGoogle Scholar
  44. 44.
    Sutin KA, Li L, Frampton CS, Sayer BG, McGlinchey MJ (1991) Organometallics 10:2362CrossRefGoogle Scholar
  45. 45.
    Lingham SL, Mays MJ, Raithby PR, Solan GA, Sundavadra BV, Conole G, Kessler M (1994) J Chem Soc Dalton Trans 3607Google Scholar
  46. 46.
    Fenske D, Bensmann W (1985) Z Naturforsch B Chem Sci 40:1093Google Scholar
  47. 47.
    Bott SG, Yang K, Richmond MG (2004) J Organomet Chem 689:791CrossRefGoogle Scholar
  48. 48.
    Fenske D (1979) Chem Ber 112:363CrossRefGoogle Scholar
  49. 49.
    Lewis JS, Heath SL, Powell AK, Zweit J, Blower PJ (1997) J Chem Soc Dalton Trans 855Google Scholar
  50. 50.
    Mao F, Philbin CE, Weakley TJR, Tyler DR (1990) Organometallics 9:1510CrossRefGoogle Scholar
  51. 51.
    Yang K, Bott SG, Richmond MG (1995) Organometallics 14:2387CrossRefGoogle Scholar
  52. 52.
    Orpen AG, Brammer L, Allen FH, Kennard O, Watson DG, Talyor R (1989) J Chem Soc Dalton Trans S1Google Scholar
  53. 53.
    Richter F, Beurich H, Muller M, Gartner N, Vahrenkamp H (1983) Chem Ber 116:3774CrossRefGoogle Scholar
  54. 54.
    Kamiguchi S, Chihara T (2000) J Cluster Sci 11:483CrossRefGoogle Scholar
  55. 55.
    Curtis MD, Han KR, Butler WM (1980) Inorg Chem 19:2096CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC 2009

Authors and Affiliations

  1. 1.Department of ChemistryTexas Christian UniversityFort WorthUSA
  2. 2.Department of ChemistryUniversity of North TexasDentonUSA

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