figshare
Browse
om500342z_si_003.xyz (22.46 kB)

Palladium(II) Complexes of 1,2,4-Triazole-Based N‑Heterocyclic Carbenes: Synthesis, Structure, and Catalytic Activity

Download (22.46 kB)
dataset
posted on 2014-06-23, 00:00 authored by Jan Turek, Illia Panov, Miloslav Semler, Petr Štěpnička, Frank De Proft, Zdeňka Padělková, Aleš Růžička
Six palladium­(II) complexes bearing three different triazole-based N-heterocyclic carbene (NHC) ligands, [1-tert-butyl-4-{2-[(N,N-dimethylamino)­methyl]­phenyl}-3-phenyl-1H-1,2,4-triazol-4-ium-5-ide, 1-tert-butyl-4-(2-methoxyphenyl)-3-phenyl-1H-1,2,4-triazol-4-ium-5-ide, and 1-tert-butyl-4-(4-methylphenyl)-3-phenyl-1H-1,2,4-triazol-4-ium-5-ide], were synthesized and fully characterized. NMR spectroscopy and X-ray diffraction analysis revealed that the amino-group-substituted NHC ligand is coordinated in bidentate fashion, forming a monocarbene chelate complex with an additional intramolecular Pd ← N bond with the nitrogen donor atom. The 4-methylphenyl- and 2-methoxyphenyl-substituted NHC ligands coordinate as C-monodentate donors, forming simple biscarbene Pd­(II) complexes. The evaluation of the catalytic performance in the Suzuki–Miyaura cross-coupling reaction revealed very promising performance of the intramolecularly coordinated monocarbene complexes under relatively mild conditions even in direct comparison with the commercially available PEPPSI catalyst. In contrast, the biscarbene complexes proved inactive in this catalytic process. According to theoretical calculations (EDA and NOCV analysis), functionalization of the 1,2,4-triazole-based NHC with the 2-[(N,N-dimethylamino)­methyl]­phenyl group has a significant effect on the stability of the NHC–metal bond.

History