Vanadate complexes bearing an imidazolidine-bridged bis(aryloxido) ligand: synthesis and solid state and solution structureCCDC 855050 for H2L. For crystallographic data in CIF or other electronic format see 10.1039/c2dt30153a

A new imidazolidine-bridged bis(aryloxido) ligand precursor ( H 2 L ) [ H 2 L = 2,2-(imidazolidine-1,3-diylbis(methylene))bis(4-(1,1,3,3-tetramethylbutyl-2-yl)phenol)] was prepared in a relatively high yield (60%) via a single-step Mannich condensation of 4-(1,1,3,3-tetramethylbutyl)phenol, ethylene...

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Hauptverfasser: Kober, Ewa, Nerkowski, Tomasz, Janas, Zofia, Jerzykiewicz, Lucjan B
Format: Artikel
Sprache:eng
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Zusammenfassung:A new imidazolidine-bridged bis(aryloxido) ligand precursor ( H 2 L ) [ H 2 L = 2,2-(imidazolidine-1,3-diylbis(methylene))bis(4-(1,1,3,3-tetramethylbutyl-2-yl)phenol)] was prepared in a relatively high yield (60%) via a single-step Mannich condensation of 4-(1,1,3,3-tetramethylbutyl)phenol, ethylenediamine and paraformaldehyde at 2:1:3 molar ratio and characterized by chemical and physical techniques including X-ray crystallography. Reactions of H 2 L with [VO(OEt) 3 ] at 1:1 and 1:2 molar ratios in toluene afforded [V(L- 3 O,N,N,O)(O)(OEt)] ( 1 ) and [V 2 (-L- 4 O,N,N,O)(-OEt) 2 (O) 2 (OEt) 2 ] ( 2 ), respectively. Alcoholysis of 1 with EtOH enables elimination of one molecule of H 2 L and the formation of 2 . Compounds 1 and 2 were characterized by IR and NMR spectroscopy as well as ES-MS experiments. The definitive molecular structure of 2 was provided by a single-crystal analysis and revealed its dinuclear nature, featuring two octahedral vanadium centres bridged by both OEt groups and the L ligand. The 51 V, 1 H and 13 C NMR spectra as well as ES-MS showed that 2 does not stay intact in solution and undergoes dissociation to give 1 and [VO(OEt) 3 ]. The synthesis, structure and spectroscopic characteristics of the 2,2-(imidazolidine-1,3-diylbis(methylene))bis(4-(1,1,3,3-tetramethylbutyl-2-yl)phenol and its corresponding vanadate complexes are reported.
ISSN:1477-9226
1477-9234
DOI:10.1039/c2dt30153a