X-ray characterization of Hnacnac^R and the first vanadium β-diiminate dimer (R  = mesityl)

Abstract

The synthesis, characterization, and X-ray crystal structure of Hnacnac R (R ¼ mesityl) 1 as well as the structure of the first vanadium -diiminate dimer, di--hydroxodi(nacnac R )divanadyl(IV) (R ¼ mesityl) 2 are reported. The reported -diimine, 1, is prepared through a condensation reaction between 2,4,6-trimethylaniline and 2,4-pentanedione. Compound 1 crystallizes in the P " 1 space group with Z 0 ¼ 8; 2 also crystallizes in P " 1 with Z 0 ¼ 1. The vanadium(IV) in 2 has the expected distorted square pyramidal geometry. Although the hydroxide hydrogen atoms can be found in the electron difference map, the existence of the bridging hydroxide in 2 was further confirmed through bond distance comparisons and bond valence sum analysis. Compound 1 was characterized by NMR, IR, and X-ray crystallography. (Hnacnac R (R ¼ mesityl) ¼ 4-(2,4,6-trimethylphenylimino)-2-(2,4,6-trimethylphenylamino)-pent-2-ene; mesityl ¼ 2,4,6-trimethylphenyl).