Preparation and Precise Structural Determination of a Second Ga 84 Cluster Compound. A First Hint for Cluster Doping and Its Fundamental Consequences in the Field of Chemistry and Physics of Nanoscaled Metalloid Cluster Material

Inorganic Chemistry

Volumn 42, Issue 24, 2003, Pages 7731-7733

  Schnepf, Andreas ^a   Jee, Bettina ^a   Schnöckel, Hansgeorg ^a   Weckert, Edgar ^b   Meents, Alke ^b   Lubbert, Daniel ^b   Herrling, Erik ^a   Pilawa, Bernd ^a  

^a UNIVERSITY OF KARLSRUHE   (Germany)

^b DESY   (Germany)

Author keywords

[No Author keywords available]

Indexed keywords

ANION; METAL;

ARTICLE; CHEMISTRY; CONDUCTANCE; CRYSTAL STRUCTURE; NANOPARTICLE; OXIDATION REDUCTION POTENTIAL; PHYSICS; STRUCTURE ANALYSIS; SYNCHROTRON RADIATION;

EID: 0345448764     PISSN: 00201669     EISSN: None     Source Type: Journal    
DOI: 10.1021/ic035031k     Document Type: Article

References (19)

1. Cluster and Colloides; Schmid, G., Ed.; VCH: Weinheim. New York. 1994.
2. Braunstein, P.; Oro, L. A.; Raithby, P. R. Metal Clusters in Chemistry; VCH: Weinheim, New York, 1999.
3. Schnepf, A.; Stösser, G.; Schnöckel, H. J. Am. Chem. Soc. 2000, 122, 9178.
4. Cotton, F. A. Q. Rev. Chem. Soc. 1966, 20, 389.
5. Schmid, G. Inorg. Synth. 1990, 7, 214.
6. Tran, N. T.; Kawano, M.; Powell, D. R.; Dahl, L. F. J. Am. Chem. Soc. 1998, 120, 10986.
7. Tran, N. T.; Powell, D. R.; Dahl, L. F. Angew. Chem., Int. Ed. 2000, 39, 4121.
8. Mednikov, E. G.; Ivanov, S. A.; Dahl, L. F. Angew. Chem., Int. Ed. 2003, 42, 323.
9. Ecker, A.; Weckert, E.; Schnöckel, H. Nature 1997, 387, 379.
10. Schnepf, A.; Schnöckel, H. Angew. Chem., Int. Ed. 2001, 40, 712.
11. Bakharev, O. N.; Zelders, N.; Brom, H. B.; Schnepf, A.; Schnöckel, H. de Jongh, L. J. Eur. Phys. J. 2003, D24, 101.
12. Hagel, J.; Kelemen, M. T.; Fischer, G.; Pilawa, B.; Wosnitza, J.; Dormann, E. v. Löhneysen, H.; Schnepf, A.; Schnöckel, H.; Neisel, U.; Beck, J. J. Low Temp. Phys. 2002, 314, 133.
13. Dohmeier, C.; Loos, D.; Schnöckel, H. Angew. Chem., Int. Ed. Engl. 1996, 35, 129. Schnepf, A.; Schnöckel, H. Angew. Chem., Int. Ed. 2002, 41, 3533. Schnepf, A.; Schnöckel, H. Adv. Organomet. Chem. 2001, 47, 235.
14. Dohmeier, C.; Loos, D.; Schnöckel, H. Angew. Chem., Int. Ed. Engl. 1996, 35, 129. Schnepf, A.; Schnöckel, H. Angew. Chem., Int. Ed. 2002, 41, 3533. Schnepf, A.; Schnöckel, H. Adv. Organomet. Chem. 2001, 47, 235.
15. Dohmeier, C.; Loos, D.; Schnöckel, H. Angew. Chem., Int. Ed. Engl. 1996, 35, 129. Schnepf, A.; Schnöckel, H. Angew. Chem., Int. Ed. 2002, 41, 3533. Schnepf, A.; Schnöckel, H. Adv. Organomet. Chem. 2001, 47, 235.
16. 2 (1.8 g, 10 mmol) was added to toluene (35 mL) and cooled to -78 °C. A GaBr solution (27 mL. 8.3 mmol of a 0.3 M solution in toluene/THF (4:1)) was added to this solution slowly at -78 °C with a steel cannula. The reaction mixture was then slowly heated to room temperature under stirring, and an almost black solution was obtained. The solution was then warmed to 55 °C for 20 h. After the solution had been cooled to room temperature, black metallic shining crystals of 2 (75 mg, 0.007 mmol, 26%) were obtained on the glass wall.
17. The EPR spectra were measured on an X-band spectrometer (Bruker ESP300E. ; v = 9.74 GHz). At 6.7 K, an EPR signal at 3414.2 G is found.
18. 3, R1/wR2 = 3.66/8.85 for the 113 391 observed reflections (I > 2σ).
19. 3Bi structure (analogous to 2), such doping cannot be excluded via X-ray structure determination.