Synthesis and study of the cluster [Pd(AuPPh 3) 6(HgNO 3)](NO 3) by reversed-phase high-performance liquid chromatography, thermoanalysis, infrared, nuclear magnetic resonance, and fast atom bombardment mass spectrometry

The addition reaction of Hg 0 and Hg 2 2+ to the bimetallic cluster [(PPh 3)Pd(AuPPh 3) 6](NO 3) 2 (I) has been studied. The reaction, monitored by HPLC, showed the time elapsed to obtain the pure cluster [Pd(AuPPh 3) 6(HgNO 3)](NO 3) (II). The use of 31P{ 1H} NMR, IR spectra, FABMS and thermoanalys...

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Veröffentlicht in:	Journal of Chromatography A 1999-11, Vol.862 (1), p.29-38
Hauptverfasser:	Sotelo, Adriana F, Felicissimo, Anna Maria P
Format:	Artikel
Sprache:	eng
Schlagworte:	Chemistry Chromatography, High Pressure Liquid Coordination compounds Exact sciences and technology Gold clusters Hot Temperature Inorganic chemistry and origins of life Magnetic Resonance Spectroscopy Organometallic Compounds - chemical synthesis Palladium–gold Phosphine Preparations and properties Spectrometry, Mass, Fast Atom Bombardment Spectrophotometry, Infrared Time Factors
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Beschreibung
Zusammenfassung:	The addition reaction of Hg 0 and Hg 2 2+ to the bimetallic cluster [(PPh 3)Pd(AuPPh 3) 6](NO 3) 2 (I) has been studied. The reaction, monitored by HPLC, showed the time elapsed to obtain the pure cluster [Pd(AuPPh 3) 6(HgNO 3)](NO 3) (II). The use of 31P{ 1H} NMR, IR spectra, FABMS and thermoanalysis data was very useful for confirming the results. The reaction was monitored by taking five samples after 3, 6, 17, 21 and 24 h. The process was finalised after 24 h and the pure trimetallic cluster II, free of the intermediate, appeared in the chromatogram as a large, unique peak.
ISSN:	0021-9673
DOI:	10.1016/S0021-9673(99)00913-9