Issue 11, 1984

Reactions of olefin complexes with nitrene precursors. Synthesis of triazoline and aziridine complexes of palladium(II); crystal and molecular structure of trans-dichlorobis(11-phenyl-9,10,11-triazabicyclo-[6.3.0]undec-9-ene-N9)palladium–chloroform(1/2)

Abstract

By reaction at 70 °C of phenyl azide with a suspension of PdCl2 and cis-cyclo-octene, the complex [PdCl2{[graphic omitted]H2}2]·2CHCl3 has been isolated, and its crystal and molecular structure determined. This compound crystallizes in triclinic space group P[1 with combining macron] with a= 9.258(2), b= 10.702(3), c= 11.156(2)Å, α= 113.94(3), β= 99.60(2), γ= 104.87(3)°, and Z= 1. The metal lies on a symmetry centre and the complex configuration is trans planar. The chloroform molecules are hydrogen bonded to the co-ordinated chloride ions. The reaction of phenyl azide with cis-cyclo-octene at 70 °C in the absence of PdCl2 leads to the corresponding anil, N-cyclo-octylideneaniline, PhN[double bond, length half m-dash][graphic omitted]H2. Preformed [{PdCl2(cis-C8H14)}2] reacts with phenyl azide in cyclo-octene at 70 °C to give [PdCl2{[graphic omitted]H2}2]. By comparison, [{PdCl2[PhN[double bond, length half m-dash][graphic omitted]H2]}2] has been synthesized from the reaction of [PdCl2(PhCN)2] with N-cyclo-octylideneaniline.

Article information

Article type
Paper

J. Chem. Soc., Dalton Trans., 1984, 2409-2414

Reactions of olefin complexes with nitrene precursors. Synthesis of triazoline and aziridine complexes of palladium(II); crystal and molecular structure of trans-dichlorobis(11-phenyl-9,10,11-triazabicyclo-[6.3.0]undec-9-ene-N9)palladium–chloroform(1/2)

F. Porta, M. Pizzotti, G. La Monica, L. A. Finessi, S. Cenini, P. L. Bellon and F. Demartin, J. Chem. Soc., Dalton Trans., 1984, 2409 DOI: 10.1039/DT9840002409

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