Toward the solution synthesis of the tetrahedral Au 20 cluster

Journal of Physical Chemistry B

Volumn 108, Issue 33, 2004, Pages 12259-12263

  Zhang, Hai Feng ^a,b   Stender, Matthias ^a   Zhang, Rui ^a   Wang, Chongmin ^a   Li, Jun ^a   Wang, Lai Sheng ^a,b  

^a PACIFIC NORTHWEST NATIONAL LABORATORY   (United States)

^b WASHINGTON STATE UNIVERSITY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

CATALYTIC PROPERTIES; CLUSTERS; COLLISION-INDUCED DISSOCIATION; LIGANDS;

CATALYSIS; COMPLEXATION; FULLERENES; GOLD COMPOUNDS; MASS SPECTROMETRY; MOLECULAR WEIGHT; POSITIVE IONS; SYNTHESIS (CHEMICAL);

ORGANOMETALLICS;

EID: 4344651324     PISSN: 15206106     EISSN: None     Source Type: Journal    
DOI: 10.1021/jp048636q     Document Type: Article

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37. All reagents used in the synthesis were commercially available. Chlorotriphenylphospine gold(I) was purchased from Strem Chemicals; tetraoctylammonium bromide, from Fluka; and sodium borohydride, from Aldrich. Toluene was purchased from Aldrich and was packed under nitrogen in a Sure/Seal bottle. Deionized water was used in the reaction and in the subsequent washes. The water was sparged with argon. All reagents were used as received without further purification. All manipulations were carried out under an atmosphere of argon using standard Schlenk and cannula techniques.
38. 3 clusters was carried out on an FTICR mass spectrometer equipped with a 9.4-T superconducting magnet. This instrument was manufactured by Broker Daltonics (Billerica, MA), and it is the latest model in the BioAPEX series (APEX-Q), which has an Apollo ESI source and a quadrupole/hexapole interface to allow external ion generation, selection, and fragmentation. The instrument was mass calibrated prior to sample analysis using a Hewlett-Packard calibration mixture (Flanagan, J. M. U.S. Patent 5,872,357, 1999). The average mass measurement error in the mass range up to m/z 4000 was <2 ppm. The mass spectral data were acquired using a 1-MB data set, and the peak resolution (ΔM/M) at m/z 1000 exceeded 100 000. At such high resolution, the isotopic information of the analyte ions was totally resolved.
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41. 2+, the estimated average energy was ∼0.64 eV.
42. 2+ dication theoretically and confirmed its stability. Our preliminary calculations showed that the structure of the dication is very similar to that of the neutral.
43. In the negative-ion mode, only a few low-intensity singly charged anions below m/z 2500 were observed. The m/z values and the isotope distributions of these ions indicated that they were very small Au-containing clusters with fragmented ligands most likely due to extensive dissociations from larger and positively charged parent clusters during electrospray.