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Formation of large chelate rings and cyclometallated complexes from But 2PCH2CH2CHMeCH2CH2PBut 2 and platinum and palladium chlorides. Crystal structure of [Pd2Cl4{But 2PCH2CH2CHMeCH2CH2PBUt 2}2]
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1980
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Treatment of [PdCl2(NCPh)2] with But2 PCH2CH2CHMeCH2CH2PBut2(Q) gives the binuclear complex [Pd2Cl4(But2PCH2CH2CHMeCH2CH2PBut2)2]. The crystal structure of this 16-atom ring complex shows that the two methyl substituents on the ring occupy ‘corner positions’ and the C5 chains are not in the extended conformation. The crystals are monoclinic, space group Pn, with unit-cell dimensions a= 8.616(2), b= 28.485(5), c= 12.127(2)Å, β= 109.35(2)°, and Z= 2, final R= 0.07. A variable-temperature 31P n.m.r. study shows the ring to be fluxional. With [PtCl2(NCPh)2], Q gives a complex [(PtCl2Q)x](also fluxional) and a cyclometallated complex [graphic omitted]But2)] abbreviated to [PtCl(P–C–P)], [PtCl2Q] with CF3COOH gives [Pt(OOCCF3)(P–C–P)], and [PtCl(P–C–P)] with Na[BH4] gives [PtH(P–C–P)]. Infrared and 1H and 31P n.m.r. data are given.