Producción Científica Profesorado

Synthesis, single crystal X-ray structure determination and NMR studies of Cp2Fe(PPh2)2PtPh2 and Cp2Fe(PPh2)2PtI2



Alvarado Rodríguez, José Guadalupe

1998

Synthesis, single crystal X-Ray structure determination and NMR studies of Cp2Fe(PPh2)2PtPh2 and Cp2Fe(PPh2)2PtI2. Thomas J. Colacot, Richard A. Teichman, Raymundo Cea-Olivares, José Guadalupe Alvarado-Rodríguez, Rubén A. Toscano, Walter J. Boyko Journal of Organometallic Chemistry (1998) 557, 169.


Abstract


Diphenyl[1,1?-bis(diphenylphosphino)ferrocene]platinum(II), Cp2Fe(PPh2)2PtPh2 (1) and diiodo[1,1?-bis(diphenylphosphino)ferrocene]platinum(II), Cp2Fe(PPh2)2PtI2 (2) were synthesized in nearly quantitative yield, with excellent purity by allowing Cp2Fe(PPh2)2 to react with (COD)PtPh2 and (COD)PtI2 (COD=1,5-cyclooctadiene), respectively. Compounds 1 and 2 have been well characterized by various analytical and spectroscopic techniques and also by single crystal X-ray diffraction. Platinum in both the complexes seemed to have a distorted square planar geometry. Interestingly, the respective bite angles (PPtP bond angle) in 1 (101.2(1) Å) and 2 (100.6(1) Å) deviate from the ideal 90 situation and are larger than in the reported structure, dppfPtCl2 [dppf=1,1?-bis(diphenylphosphino)ferrocene]. A detailed NMR study, including 2D and simulation experiments has been performed on these compounds for complete structural assignment. The compounds 1 and 2 crystallized in triclinic space groups P and P with a=12.268(2) Å, 10.089 (1); b=13.043(2) Å, 10.856 (1); c=13.649(1), 17.787(1) Å; ?=100.49(1), 86.75(1); ?=93.12(1), 77.52(1); ?=103.44(1), 64.91(1); V=2078.0(5), 1721.3(3) Å3 and Z=2 and 2, respectively. The final refinements of 1 and 2 converged at R=0.0388 and 0.0580, respectively.






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