Synthesis and study of the cluster [Pd(AuPPh3)6(HgNO3)](NO3) by reversed-phase high-performance liquid chromatography, thermoanalysis, infrared, nuclear magnetic resonance, and fast atom bombardment mass spectrometry.
The addition reaction of Hg0 and Hg(2)2+ to the bimetallic cluster [(PPh3)Pd(AuPPh3)6](NO3)2 (I) has been studied. The reaction, monitored by HPLC, showed the time elapsed to obtain the pure cluster [Pd(AuPPh3)6(HgNO3)](NO3) (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.
Sotelo
A F
AF
Instituto de Química, Universidade de São Paulo, Brazil.
Felicissimo
A M
AM
D002851:Chromatography, High Pressure Liquid; D006358:Hot Temperature; D009682:Magnetic Resonance Spectroscopy; D009942:Organometallic Compounds / Q000138:chemical synthesis; D016339:Spectrometry, Mass, Fast Atom Bombardment; D013055:Spectrophotometry, Infrared; D013997:Time Factors
C402371:(Pd(AuPPh3)6(HgNO3))(NO3); D009942:Organometallic Compounds