Issue 43, 2012

Synthesis of [PdL(NH3)2](PF6)2 (L = 1,1′-di(alkyl)-3,3′-methylenediimidazolin-2,2′-diylidene) complexes and their reactivities towards N-donors

Abstract

The reaction of neutral palladium complexes PdLBr2 (L = 1,1′-di(alkyl)-3,3′-methylenediimidazolin-2,2′-diylidene) with NH4PF6 in CH3CN afforded [PdL(NH3)2](PF6)2 (1–3, L1, alkyl = Me; L2, alkyl = Et; L3, alkyl = iso-Pr) and [PdL4(CH3CN)2](PF6)2 (4, alkyl = Mes). Treatment of [PdL(NH3)2](PF6)2 complexes with N-donors, 9-ethyl-3,6-diimidazolyl-carbazole (dicz), mercaptopyridine (HSPy), 3,5-dimethyl-1H-pyrazole (Hdmpz), and 1,2-dibenzoylhydrazine (H2dbhz) resulted in the substitution of NH3 forming dinuclear palladium complexes [PdL1(dicz)]2(PF6)4 (5), [PdL1(SPy)]2(PF6)2 (6), [PdL2(dmpz)]2(PF6)2 (7), [(PdL2)2(dbhz)] (8). Reaction of [PdL2(NH3)2](PF6)2 with hydrazine led to a mixture of [Pd(L2)2](PF6)2 (9) and [PdL2(NH2N[double bond, length as m-dash]C(CH3)NHNH2)](PF6)2 (10). The NH2N[double bond, length as m-dash]C(CH3)NHNH2 moiety was formed in situ by nucleophilic addition to CH3CN by two molecules of NH2NH2 and subsequent NH3 elimination. All of these complexes have been fully characterized by ESI-MS, NMR spectroscopy, and elemental analysis. The molecular structures of 1 and 5–10 were also studied by X-ray diffraction analysis.

Graphical abstract: Synthesis of [PdL(NH3)2](PF6)2 (L = 1,1′-di(alkyl)-3,3′-methylenediimidazolin-2,2′-diylidene) complexes and their reactivities towards N-donors

Supplementary files

Article information

Article type
Paper
Submitted
31 Jul 2012
Accepted
04 Sep 2012
First published
04 Sep 2012

Dalton Trans., 2012,41, 13405-13412

Synthesis of [PdL(NH3)2](PF6)2 (L = 1,1′-di(alkyl)-3,3′-methylenediimidazolin-2,2′-diylidene) complexes and their reactivities towards N-donors

C. Chen, W. Chen and H. Qiu, Dalton Trans., 2012, 41, 13405 DOI: 10.1039/C2DT31739G

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