Synthesis, characterization, X-ray crystal and molecular structure of [(PPh 3)Pd(AuPPh 3) 6](PF 6) 2

• Published in: Inorganica Chimica Acta 2003-05, Vol.348, p.63-68
• Main Authors: Sotelo, Adriana F, Felicissimo, Anna Maria P, Sal, Pilar Gomez
• Format: Article
• Language: English
• Subjects: Cluster; Palladium; Triphenylphosphine; X-ray crystal structure
• ISSN: 0020-1693; 1873-3255
• DOI: 10.1016/S0020-1693(02)01476-7

Although obtained by different methods the cluster [(PPh 3)Pd(AuPPh 3) 6] 2+ was always collected as a microcrystalline product. Attempts to get crystals of this cluster for X-ray determination were successfully made changing the counter-ion NO 3 − to PF 6 − . This new compound was characterized by elemental analysis, IR, and 31P NMR spectroscopy in solution. The crystal and molecular structure was determined by a single crystal X-ray analysis. The compound crystallizes in the triclinic space group P 1 ̄ with a=17.138 (3) Å, b=27.263 (5) Å, c=27.543 (6) Å, α=101.70 (3)°, β=105.80 (3)°, γ=90.19 (3)° T=273 °C, Z=4, V=12 102 Å 3, R=0.1149 and R w=0.2669 for 23 620 observations. The structure consists of part of an icosahedron Pd centered. The Pd atom is bound to one PPh 3 molecule and six gold atoms. The PPh 3 is attached to the gold atom and the structure is isoelectronic and isostructural to the [(PPh 3)Pt(AuPPh 3) 6] 2+ cluster. The cluster compound [(PPh 3)Pd(AuPPh 3) 6](PF 6) 2 has been prepared and structurally characterized. The compound crystallizes in the triclinic group P 1 ̄ with a=17.138(3) Å, b=27.263(5) Å, c=27.543(6) Å, α=101.70(3)°, β=105.80(3)°, γ=90.19°. The structure consists of part of an icosahedral Pd centered. The Pd atom is bound to one PPh 3 molecule and six gold atoms. The PPh 3 is attached to the gold atom and the structure is isoeletronic and isostructural to the cluster [(PPh 3)Pt(AuPPh 3) 6] 2+.