Nanosized [Pd69(CO)36(PEt3)18]: Metal-core geometry containing a linear assembly of three face-sharing centered Pd33 icosahedra inside of a hexagonal-shaped Pd30 tube

Angewandte Chemie - International Edition

Volumn 42, Issue 30, 2003, Pages 3533-3537

  Tran, Nguyet T ^a   Dahl, Lawrence F ^a  

^a UNIVERSITY OF WISCONSIN MADISON   (United States)

Author keywords

Carbonyl ligands; Cluster compounds; Palladium; Phosphane ligands; Structure elucidation

Indexed keywords

CONDENSATION; PALLADIUM COMPOUNDS; STEREOCHEMISTRY;

LINEAR ASSEMBLY;

NANOSTRUCTURED MATERIALS;

CARBON MONOXIDE; PALLADIUM;

ARTICLE; CHEMICAL ANALYSIS; CHEMICAL STRUCTURE; CRYSTALLOGRAPHY; GEOMETRY; NANOPARTICLE; STRUCTURE ANALYSIS;

EID: 0041965886     PISSN: 14337851     EISSN: None     Source Type: Journal    
DOI: 10.1002/anie.200351738     Document Type: Article

References (41)

1. a) E. G. Mednikov, N. K. Eremenko, Izv. Akad. Nauk SSSR Ser. Khim. 1982, 2540; [Russ. Chem. Bull. 1982 31 2240 (Engl. Trans.)];
2. a) E. G. Mednikov, N. K. Eremenko, Izv. Akad. Nauk SSSR Ser. Khim. 1982, 2540; [Russ. Chem. Bull. 1982 31 2240 (Engl. Trans.)];
3. b) E. G. Mednikov, N. K. Eremenko, Yu. L. Slovokhotov, Yu. T. Struchkov, S. P. Gubin, J. Organomet. Chem. 1983, 258, 247.
4. D. M. P. Mingos, C. M. Hill, Croat. Chem. Acta 1995, 68, 745.
5. E. G. Mednikov, Yu. T. Struchkov, Yu. L. Slovokhotov, J. Organomet. Chem. 1998, 566, 15.
6. M. Kawano, J. W. Bacon, C. F. Campana, B. E. Winger, J. D. Dudeck, S. A. Sirchio, S. L. Scruggs, U. Geiser, L. F. Dahl, Inorg. Chem. 2001, 40, 2554.
7. E. G. Mednikov, N. K. Eremenko, Yu. L. Slovokhotov, Yu. T. Struchkov, J. Organomet. Chem. 1986, 301, C35; E. G. Mednikov, Metalloorg. Khim. 1991, 4, 885; [Organomet. Chem. USSR 1991, 4, 433 (Engl. Trans.)].
8. E. G. Mednikov, N. K. Eremenko, Yu. L. Slovokhotov, Yu. T. Struchkov, J. Organomet. Chem. 1986, 301, C35; E. G. Mednikov, Metalloorg. Khim. 1991, 4, 885; [Organomet. Chem. USSR 1991, 4, 433 (Engl. Trans.)].
9. E. G. Mednikov, N. K. Eremenko, Yu. L. Slovokhotov, Yu. T. Struchkov, J. Organomet. Chem. 1986, 301, C35; E. G. Mednikov, Metalloorg. Khim. 1991, 4, 885; [Organomet. Chem. USSR 1991, 4, 433 (Engl. Trans.)].
10. a) J. Wittayakun, N. T. Tran, D. R. Powell, L. F. Dahl, unpublished results;
11. b) E. G. Mednikov, S. A. Ivanov, J. Wittayakun, L. F. Dahl, J. Chem. Soc. Dalton Trans. 2003, 1686.
12. 10][5] but with two fewer CO ligands. A comparative qualitative molecular analysis[6a] favors the existence of both clusters, which have different crystal forms.[6]
13. N. T. Tran, M. Kawano, D. R. Powell, L. F. Dahl, J. Chem. Soc. Dalton Trans. 2000, 4138.
14. E. G. Mednikov, S. A. Ivanov, L. F. Dahl, Angew. Chem. 2003, 115, 337; Angew. Chem. Int. Ed. 2003, 42, 323.
15. E. G. Mednikov, S. A. Ivanov, L. F. Dahl, Angew. Chem. 2003, 115, 337; Angew. Chem. Int. Ed. 2003, 42, 323.
16. N. T. Tran, M. Kawano, L. F. Dahl, J. Chem. Soc. Dalton Trans. 2001, 2731.
17. E. G. Mednikov, Yu. L. Slovokhotov, Yu. T. Struchkov, Metalloorg. Khim. 1991, 4, 123; [Organomet. Chem. USSR 1991, 4, 65 (Engl. Trans.)].
18. E. G. Mednikov, Yu. L. Slovokhotov, Yu. T. Struchkov, Metalloorg. Khim. 1991, 4, 123; [Organomet. Chem. USSR 1991, 4, 65 (Engl. Trans.)].
19. E. G. Mednikov, N. I. Kanteeva, Izv. Akad. Nauk SSSR Ser. Khim. 1995, 167; [Russ. Chem. Bull. 1995, 44, 163 (Engl. Trans.)].
20. E. G. Mednikov, N. I. Kanteeva, Izv. Akad. Nauk SSSR Ser. Khim. 1995, 167; [Russ. Chem. Bull. 1995, 44, 163 (Engl. Trans.)].
21. N. T. Tran, M. Kawano, D. R. Powell, L. F. Dahl, J. Am. Chem. Soc. 1998, 120, 10986.
22. N. T. Tran, D. R. Powell, L. F. Dahl, Angew. Chem. 2000, 112, 4287; Angew. Chem. Int. Ed. 2000, 39, 4121.
23. N. T. Tran, D. R. Powell, L. F. Dahl, Angew. Chem. 2000, 112, 4287; Angew. Chem. Int. Ed. 2000, 39, 4121.
24. a) B. K. Teo, H. Zhang, X. Shi, J. Am. Chem. Soc. 1990, 112, 8552;
25. b) B. K. Teo, H. Zhang, Proc. Natl. Acad. Sci. USA 1991, 88, 5067, and references therein;
26. c) B. K. Teo, H. Zhang, Coord. Chem. Rev. 1995, 143, 611;
27. d) H. Zhang, B. K. Teo, Inorg. Chim. Acta 1997, 265, 213;
28. e) B. K. Teo, A. Strizhev, R. Elber, H. Zhang, Inorg. Chem. 1998, 37, 2482.
29. 2O) at room temperature for one day.
30. 3 ligands. One independent carbonyl ligand is disordered at two orientations (namely, CO(12)/CO(12′) with refined occupancies of 0.59/0.41). All carbon atoms of one independent phosphane ligand are disordered (occupancies of 0.49/0.51). Non-hydrogen atoms were refined anisotropically except for all carbon atoms of the disordered phosphane ligand. Restraints were applied to the positional and displacement parameters of the ethyl carbon atoms in order to achieve convergence. CCDC-208518 (1) and -208519 (1a) contain the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/conts/ retrieving.html (or from the Cambridge Crystallographic Data Centre, 12, Union Road, Cambridge CB21EZ, UK; fax: (+44)1223-336-033; or deposit@ccdc.cam.ac.uk).
31. All software and sources of the scattering factors are contained in the SHELXTL (version 5.1) program library (G. Sheldrick, Bruker Analytical X-Ray Systems, Madison, WI).
32. J. Donohue, The Structures of the Elements, Wiley, New York, 1974, p. 236.
33. a) A. L. Mackay, Acta Crystallogr. 1962, 15, 916;
34. b) S. Ino, J. Phys. Soc. Jpn. 1966, 21, 346;
35. c) J. Farges, M. F. de Feraudy, B. Raoult, G. Torchet, Acta Crystallogr. Sect. A 1982, 38, 656.
36. a) E. G. Mednikov, N. K. Eremenko, Yu. L. Slovokhotov, Yu. T. Struchkov, Zh. Vses. Khim. O-va. im. D. I. Mendeleeva 1987, 32, 101 (in Russian);
37. b) E. G. Mednikov, Izv. Akad. Nauk SSSR Ser. Khim. 1993, 1299; [Russ. Chem. Bull. 1993, 42, 1242 (Engl. Trans.)].
38. b) E. G. Mednikov, Izv. Akad. Nauk SSSR Ser. Khim. 1993, 1299; [Russ. Chem. Bull. 1993, 42, 1242 (Engl. Trans.)].
39. In contrast to 1, six out of 18 triply bridging CO ligands in 1 are doubly bridging in la with the longest connectivity being nonbonding (> 2.5 Å).
40. a) B. K. Teo, M. Hong, H. Zhang, D. Huang, X. Shi, J. Chem. Soc. Chem. Commun. 1988, 204;
41. b) B. K. Teo, H. Zhang, X. Shi, J. Am. Chem. Soc. 1990, 112, 8552.