138260-05-6Relevant articles and documents
(Diphenylphosphino)methyl complexes of titanium and zirconium: Synthesis and characterization. Molecular structure of CpCp*Ti(CH2PPh2)2 (Cp = C5H5; Cp* = C5Me5)
Cuenca, Tomàs,Flores, J. Carlos,Royo, Pascual,Larsonneur, Anne-Marie,Choukroun, Robert,Dahan, Fran?oise
, p. 777 - 780 (1992)
The reaction of [C5(CH3)5](C5H5)MCl 2 (M = Ti, Zr) with 2 equiv of LiCH2PPh2·TMEDA offers a convenient method for the preparation of the corresponding dialkyl derivatives [C5(CH3)5](C5H 5)M-(CH2PPh2)2 where M = Ti and Zr in 95-100% yield. However, when this reaction is carried out with 1 equiv of LiCH2PPh2·TMEDA in the same conditions, the chloro alkyl complex of titanium [C5-(CH3)5](C5H 5)TiCl(CH2PPh2) is formed, whereas a mixture of the starting material and the dialkyl derivative is obtained for zirconium. These new complexes have been characterized by 1H, 13C, and 31P{1H} NMR measurements and elemental analysis. The 1H NMR spectra show a clear diastereotopic behavior for the methylene protons of the CH2 groups. The molecular structure of [C5(CH3)5](C5H 5)Ti(CH2PPh2)2 as determined by X-ray diffraction methods is reported. The complex crystallizes in the space group P21/c (No. 14), a = 17.323 (2) A?, b = 12.549 (1) A?, c = 16.497 (2) A?, β = 103.71 (2)°, Z = 4. The geometry around the Ti atom is normal. A weak agostic interaction Ti?H(4) can be proposed to be present in the structure of the solid state of this compound.