Research paperPreparation, characterization, X-ray crystal structures, and isomerization equilibria and kinetics of cis- and trans-bis(5-imino-2,2-dimethyl-3-hexanonato-N,O)palladium(II)

Add time:08/29/2019    Source:sciencedirect.com

The palladium(II) β-ketoenaminate complexes cis- and trans-bis(5-imino-2,2-dimethyl-3-hexanonato-N,O)palladium(II), Pd(admh)2, have been prepared by reaction of PdCl2 and 5-amino-2,2-dimethylhex-4-en-3-one, Hadmh, in aqueous NaOH and have been separated by column chromatography on Florisil. The square-planar complexes were characterized in solution by 1H NMR chemical shifts, the nuclear Overhauser effect, and electric dipole moments, which showed that the first-eluted isomer from Florisil is trans and the second-eluted isomer is cis. X-ray crystal structures of the solid complexes confirm the isomer assignments and reveal close NH ⋯ HN contacts between the two ligands in the cis isomer and close NH ⋯ O contacts in the trans isomer. Isomerization equilibria favor the trans isomer in chlorobenzene and favor the cis isomer in pyridine. The kinetics of trans-to-cis isomerization in pyridine was studied in the range 55.8–100.6 °C: ΔH‡ = 100 ± 2 kJ/mol and ΔS‡ = −50 ± 6 J/(K mol). 1H NMR spectra of Ni(admh)2 in CHClF2 down to −170 °C suggests that only one isomer (probably trans) exists in solution.

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