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Synthesis and nmr-spectroscopy characteristics of carbonylhydridovanadium complexes stabilized by oligotertiary phosphines

Authors
Journal
Journal of Organometallic Chemistry
0022-328X
Publisher
Elsevier
Publication Date
Volume
185
Issue
2
Identifiers
DOI: 10.1016/s0022-328x(00)85899-4

Abstract

Abstract Hydridocarbonylvanadium complexes are stabilized by the tri- and tetratertiary phosphines (L) PhP(CH 2CH 2PPh 2) 2 (p 3) MeC(CH 2PPh 2) 3 (cp 3), [Ph 2PCH 2CH 2PPhCH 2] 2 (p 4) and P(CH 2CH 2PPh 2) 3 (pp 3). The stable complexes HV(CO) 3L and the labile intermediates HV(CO) 4L have been prepared by chomatography of the anionic parent compounds on silica gel. Irradiation of HV(CO) 3pp 3 and HV(CO) 3p 4 affords cis-[HV(CO)[ 2pp 3] and trans-[HV(CO) 2P 4], respectively. The complexes are characterized by their IR, 1H, 31P and 51V NMR spectra. A model of restricted dynamic behaviour based on the face-capped octahedron is proposed on the basis of the hydride NMR pattern. The dinuclear ligand-bridged {HV(CO) 4} 2μ-p 4 is obtained by treatment of [Et 4N] 2n- [{V(CO) 4} 2n (μ-p 4) n] with t-BuCl/H 2O. An improved synthesis for the [ν 5-C 5H 5-VH(CO) 3]- anion is described; 1H and 51V NMR data indicate that the local symmetry of the {VH(CO) 3} moiety is probably C 3v1.

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