Synthesis, characterization and reactivity of some mono- and dinuclear chlororuthenium complexes containing chelating ditertiary phosphines (PP) with PP:Ru=1

  • Joshi A
  • Thorburn I
  • Rettig S
 et al. 
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Abstract

Mixed-valence complexes of the type (PP)ClRu(μ-Cl)3RuCl(PP), and the [RuCl(PP)]2(μ-Cl)2products formed by their reduction with H2, are synthesized, where PP is a chelating ditertiary phosphine Ph2P(CH2)nPPh2(n=3-6) or some related chiral analogues such as diop, chiraphos, dppcp, dpcycp, bdpp, binap, phenop or norphos (diop=Ph2PCH2CHOCMe2OCHCH2PPh2; chiraphos=Ph2PCH(Me)CH(Me)PPh2; dppcp=Ph2PCH(CH2)3CHPPh2; dpcycp=(C6H11)2PCH(CH2)3CHP(C6H11)2; bdpp(skewphos)=Ph2PCH(Me)CH2CH(Me)PPh2; binap=2,2′-bis(diphenylphosphine)-1,1′-binaphthyl; phenop=Ph2PN(Et)CH(CH2Ph)CH2OPPh2; norphos=Ph2P CHCHCHCHCH(CH2)CHPPh2). The [RuCl(binap)]2(μ-Cl)2species is also formed in solution by dissociation of PPh3from RuCl2(binap)(PPh3) which is synthesized by phosphine exchange with RuCl2(PPh3)3. From the [RuCl(PP)]2(μ-Cl)2complex (PPPh2(CH2)4PPh2), a range of L(P-P)Ru(μ-Cl)3RuCl(PP) species is readily formed, where L includes an amine, acetone, N,N-dimethylacetamide, MeI, PhCN, CO, N2or H2; the LNEt3adduct is made also from RuCl2(dppb)(PPh3), while the corresponding dimethyl sulfoxide adduct (LDMSO), 17e, is synthesized directly from cis- RuCl2(DMSO)4and the phosphine.31P{1H} NMR data are presented for the Ru(II) species, while characterization of 17e includes an X-ray crystallographic analysis that confirms the trichloro-bridged formulation. Crystal data are as follows: triclinic, P1, a=12.796(1),b=14.559(1), c=18.429(1) Å, a=103.983(5), β=99.634(6), γ=99.634(6)°, Z=2, R=0.037 and Rw=0.046 for 9088 reflections with I ≥ 3σ(I). © 1992.

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Authors

  • Ajey M. Joshi

  • Ian S. Thorburn

  • Steven J. Rettig

  • Brian R. James

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