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Issue 22, 2012
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Ni(II), Pd(II) and Pt(II) complexes of PNP and PSP tridentate amino–phosphine ligands

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Abstract

The ligands D((CH2)2NHPiPr2)2 (D = NH 1, S 2) react with (dme)NiCl2 or (PhCN)2MCl2 (M = Pd, Pt) to give complexes of the form [D((CH2)2NHPiPr2)2MX]X (X = Cl, I; M = Ni, Pd, Pt) which were converted to corresponding iodide derivatives by reaction with Me3SiI. Reaction of 1 or 2 with (COD)PdMeCl affords facile routes to [κ3P,N,P-NH((CH2)2NHPiPr2)2PdMe]Cl (8a) and [κ3P,S,P-S((CH2)2NHPiPr2)2PdMe]Cl (9a) in high yields. An alternative synthetic approach involves oxidative addition of MeI to a M(0) precursor yielding [κ3P,N,P-HN(CH2CH2NHPiPr2)2NiMe]I (10), [κ3P,N,P-HN(CH2CH2NHPiPr2)2MMe]I (M = Pd 8b Pt 11) and [κ3P,S,P-S(CH2CH2NHPiPr2)2MMe]I (M = Pd 9b, Pt 12). Alternatively, use of NEt3HCl in place of MeI produces the species [κ3P,N,P-HN(CH2CH2NHPiPr2)2MH]X (X = Cl, M = Ni 13a, Pd 14a, Pt 16a). The analogs containing 2; [κ3P,S,P-S((CH2)2NHPiPr2)2MH]X (M = Pd, X = PF615: M = Pt, X = Br, 17a, PF617b) were also prepared in yields ranging from 74–93%. In addition, aryl halide oxidative addition was also employed to prepare [κ3P,N,P-HN(CH2CH2NHPiPr2)2MC6H4F]Cl (M = Ni 18, Pd 19) and [κ3P,S,P-S((CH2)2NHPiPr2)2Pd(C6H4F)]Cl (20). Crystal structures of 3a, 4a, 5a, 6a, 8a, 9a, 14b and 16b are reported.

Graphical abstract: Ni(ii), Pd(ii) and Pt(ii) complexes of PNP and PSP tridentate amino–phosphine ligands

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Publication details

The article was received on 16 Feb 2012, accepted on 21 Mar 2012 and first published on 25 Apr 2012


Article type: Paper
DOI: 10.1039/C2DT30373F
Citation: Dalton Trans., 2012,41, 6791-6802
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    Ni(II), Pd(II) and Pt(II) complexes of PNP and PSP tridentate amino–phosphine ligands

    M. J. Sgro and D. W. Stephan, Dalton Trans., 2012, 41, 6791
    DOI: 10.1039/C2DT30373F

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