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Crystal Structure and Reactivity of with ?-Acid Ligands
Anillo, Adela,Barrio, Cipriano,Garcia-Granda, Santiago,Obeso-Rosete, Ricardo
, p. 1125 - 1130 (2007/10/02)
The structure of the compound 1 has been established from X-ray analysis by direct and Fourier methods and refined by full-matrix least squares to R = 0.071 for 3288 observed reflections: monoclinic, space group P21/n, a = 18.70(1), b = 13.171(6), c = 23.06(2) Angstroem, β 99.86(6) deg and Z = 4.This complex reacts with an excess of ethylene or styrene and with P(OMe)3 (molar ratio 1:1) in hot toluene to yield the complexes .With a slight excess of the diphosphines (Ph2P)2X , refluxed in toluene, the complexes (PPh3)(diphosphine)> 6-10 were obtained as dark purple crystalline solids.An excess of PMe3 in hot toluene solutions of compound 1 afforded brown prismatic crystals of (PMe3)3> 11, whereas with PEt3 under the same conditions only partial substitution products are obtained, (PEt3)(PPh3)2> 12 and 13.When toluene solutions of (CO)(PPh3)2> 2 were boiled with diphosphines the complexes were isolated.The complex (CO)2(PPh3)> 19 was also detected as a reaction product of carbonylation of toluene solutions of 1.All complexes have been characterized by elemental analysis and by IR and NMR spectroscopy.
