Palladium(II) complexes with R(2)edda derived ligands. Part III. Diisobutyl (S,S)-2,2 '-(1,2-ethanediyldiimino)di(4-methylpentanoate) and its palladium(II) complex: synthesis and characterization

Abstract

A new R(2)edda-type ester, diisobutyl (SS)-2,2'-(1,2-ethane-diyldiimino)di(4-methylpentanoate) dihydrochloride, [(S,S)-H(2)iBu(2)eddl]Cl-2, 1, and its palladium(II) complex, dichloro(diisobutyl (SS)-2,2'-(1,2-ethanediyldiimino)di(4-methylpentanoate))palladium(II), [PdCl2{(S,S)-iBu(2)eddl}], 2, were synthesized and characterized by elemental analysis, as well as IR and NMR spectroscopy. It was found that complex 2 was obtained as mixture of two diastereoisomers, observed in NMR spectra. The crystal structure of compound I was determined by X-ray diffraction studies and is described. The isolated crystals consisted of one dicationic species [(SS)-H(2)iBu(2)eddl](2+) and two Cl-. The crystal system was tetragonal with the space group P4(2). Hydrogen bonds significant for the manner of packing are N-H1N center dot center dot center dot Cl, 3.049(3) angstrom, 159(3)degrees and N-H2N center dot center dot center dot Cl, 3.100(3) angstrom, 164(3)degrees. An infinite chain was formed building a one layer structure, usual for these types of compounds. The C-2 symmetry axis of the compound passes through the Cl-Cl-i bond vector and lies perpendicular to the plane N2Cl2.

Novi estar R2edda-tipa diizobutil-(S,S)-2,2'-(1,2-etandiildiimino)-di(4-metilpen-tanoat)-dihidrohlorid [(S,S)-H2iBu2eddl]Cl2,1, i njegov kompleks paladijuma(II), dihlorodiizobutil-(S,S)-2,2'-(1,2-etandiildiimino)-di(4-metilpentanoat)-paladijum(II) [PdCl2{(S,S)-iBu2eddl}], 2, sintetisani su i okarakterisani uz pomoć elementalne analize, IR i NMR spektroskopije. Nađeno je da je kompleks 2 dobijen kao smeša dva dijastereoizomera, što je primećeno u NMR spektrima. Kristalna struktura 1 je rešena i opisana. Izolovani kristali se sastoje iz jedne dikatjonske vrste [(S,S)-H2iBu2eddl]2+ i dva Cl-. Kristalni sistem je tetragonalan sa prostornim grupom P42. Značajne vodonične veze za način pakovanja su N-H1N•••Cl, 3,049(3) Å, 159(3)°i N-H2N...Cl, 3,100(3) Å, 164(3)°. Time se formira beskonačan lanac i jednoslojna struktura, koji su uobičajeni za ove tipove struktura. Osa simetrije C2 jedinjenja prolazi kroz C1-C1i vektor veze i leži normalno na N2Cl2 ravan. PR Projekat Ministarstva nauke Republike Srbije, br. 142010.