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FULVENE-PLATINUM COMPLEXES: X-RAY CRYSTAL STRUCTURE OF 2-C5H4CPh2)(PPh3)2>
Christofides, Aristides,Howard, Judith A.K.,Spencer, John L.,Stone, F.Gordon A.
, p. 279 - 292 (2007/10/02)
Bis(cycloocta-1,5-diene)platinum reacts with 2,3,4,5-tetraphenylfulvene to afford the complex 2CH2=C5Ph4)(cod)> (cod = C8H12) in which the metal atom is coordinated to the exo-cyclic double bond of the fulvene.Related compounds 2-CH2=C5Ph4)L2> (L = PPh3, PMePh2, Pme2Ph, AsPh3 or CNBut) have also been prepared and characterised.Reaction of the complexes (L = P(cyclo-C6H11)3, PPh3 or AsPh3) with 2,3,4,5-tetraphenylfulvene yields the compounds 2-CH2=C5Ph4)(L)>.NMR data for the new species are reported and discussed. 6,6-Diphenylfulvene reacts with and PPh3 (1/2 mol ratio) to give the complex 2-C5H4CPh2)(PPh3)2> in which the metal atom is bonded to carbon atoms C(2) and C(3) of the fulvene ring.This was established by an X-ray diffraction study.Crystals are monoclinic, space group P21/n, with Z = 4 in a unit cell of dimensions a = 13.761(4), b = 21.653(13), c = 17.395(6) Angstroem, β = 104.46(2) deg.The structure has been solved and refined to R = 0.064 (R' = 0.064) for 3139 independent diffracted intensities measured at room temperature.The platinum atom is in a trigonal environment formed by the two ligated phosphorus atoms and the C-C bond of the fulvene which is elongated to 1.52(3) Angstroem.The C5 fulvene ring is planar, and makes an angle of 108 deg with the coordination plane around the platinum.In this plane the metal atom is slightly asymmetrically bonded with Pt-C 2.15(2) and 2.24(2) Angstroem, and Pt-P 2.280(6) and 2.301(6) Angstroem.
