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Lookup NU author(s): Dr John ErringtonORCiD, Dr Sagar Petkar, Paul Middleton, Emeritus Professor William McFarlane, Professor William Clegg, Dr Ross Harrington
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The tetra-n-butylammonium (TBA) salt of [(MeO)TiW5O 18]3- 1 was reacted with alcohols ROH to give primary, secondary and tertiary alkoxide derivatives [(RO)TiW5O 18]3- (R = Et 2, iPr 3 and tBu 4), whilst hydrolysis afforded [(-O)(TiW5O18) 2]6- 5 rather than the hydroxo derivative (R = H). In reactions with iPrOH and tBuOH, impurity peaks observed at 1015 and 1020 ppm in the 17O NMR spectra indicate alkoxide degradation and TiO bond formation via reactions analogous to those occurring at the surfaces of solid heteropolyacids. Aryloxides [(ArO)TiW5O 18]3- were prepared by reacting 1 with phenols ArOH (Ar = C6H5 6, C6H4Me-4 7, C 6H4tBu-4 8, C6H4OH-4 9, C6H4OH-3 10, C6H3(OH) 2-3,5 11 and C6H4CHO-2 13). TiW 5O18 units were linked by reacting 1 with 9 to give [(-1,4-OC6H4O)(TiW5O18) 2]6- 12. 17O and 183W NMR spectra are reported and X-ray crystal structures were obtained for TBA salts of anions 3-10 and 13, which showed that the titanium is six-coordinate in all cases. Reactions were monitored by 1H NMR, including a 2D-EXSY study of methoxo exchange, and the slow rates observed are probably associated with the reluctance of titanium in these anions to achieve seven-coordination. This journal is © The Royal Society of Chemistry.
Author(s): Errington RJ, Petkar SS, Middleton PS, McFarlane W, Clegg W, Coxall RA, Harrington RW
Publication type: Article
Publication status: Published
Journal: Dalton Transactions
Year: 2007
Issue: 44
Pages: 5211-5222
Date deposited: 05/07/2010
ISSN (print): 1477-9226
ISSN (electronic): 1477-9234
Publisher: Royal Society of Chemistry
URL: http://dx.doi.org/10.1039/b709732h
DOI: 10.1039/b709732h
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