Synthesis and crystal structures of chlorometalates [M = V(III), Mo(V)]

Citation
S. Chitsaz et al., Synthesis and crystal structures of chlorometalates [M = V(III), Mo(V)], Z NATURFO B, 56(8), 2001, pp. 759-764
Citations number
36
Categorie Soggetti
Chemistry
Journal title
ZEITSCHRIFT FUR NATURFORSCHUNG SECTION B-A JOURNAL OF CHEMICAL SCIENCES
ISSN journal
09320776 → ACNP
Volume
56
Issue
8
Year of publication
2001
Pages
759 - 764
Database
ISI
SICI code
0932-0776(200108)56:8<759:SACSOC>2.0.ZU;2-P
Abstract
[(THF)(2)LiCl2VCl2(THF)(2)] (1) and [Li(THF)(4)][OMOCl4(THF)] (2) can be pr epared by the reactions of VCl3 with LiCl in THF and of Li(H)(PBu)-Bu-t wit h OMoCl4 in THF, respectively. 1 and 2 were characterized by IR spectroscop y, MS spectrometry (2) and X-ray crystallography. 1 can be obtained in two modifications depending on the temperature of crystallization. At -30 degre esC a triclinic form, 1a, was isolated from THF solution with one unique mo lecule per asymmetric unit. However, at 20 degreesC, 1b crystallized in the monoclinic space group P2/c. It possesses four independent molecules per a symmetric unit. According to the structure analyses 1 consists of a dinucle ar complex with a planar LiCl2V four-membered ring while 2 consists of sepe rate ions [Li(THF)4](+) and [OMOCl4(THF)](-).