Toggle Main Menu Toggle Search

Open Access padlockePrints

Synthesis and Structure of the Alkoxido-Titanium Pentamolybdate (nBu4N)3[(iPrO)TiMo5O18]: An Entry into Systematic TiMo5 Reactivity

Lookup NU author(s): Dr John ErringtonORCiD, Paul Middleton, Christopher Murphy, Emeritus Professor Bill CleggORCiD, Dr Ross Harrington


Full text for this publication is not currently held within this repository. Alternative links are provided below where available.


The alkoxido-titanium pentamolybdate [((PrO)-Pr-i)TiMo5O18](3-) (1) has been obtained as its tetrabutylammonium (TBA) salt by hydrolysis of a mixture containing (TBA)(2)[Mo2O7], (TBA)(4)[Mo8O26] and Ti((OPr)-Pr-i)(4) in MeCN and has been characterised by H-1, C-13, O-17, Ti-49 and Mo-95 NMR and FTIR spectroscopy, electrospray ionisation mass spectrometry, elemental microanalysis and single-crystal X-ray crystallography. The Lindqvist-type structure is derived from No6O19](2-) by replacement of (Mo=O)(4+) by {((PrO)-Pr-i)Ti}(3+) and shows bond alternation in the TiMo3O4 rings, with average bond distances of 1.956(8) angstrom for Ti-O(Mo), 1.832(7) angstrom for Mo-O(Ti), 1.943(7) angstrom for Mo-eq-O(Mo-ax) and 1.910(6) angstrom for Mo-ax-O(Mo-eq), while the increase in charge results in a decrease in 170 NMR chemical shift for terminal Mo=O groups from delta 933 for [Mo6O19](2-) to delta 875 and 857 for 1 and a shift in nu(Mo=O) from 951 cm(-1) for [Mo6O19](2-) to 930 cm(-1) for 1. The main peaks in the negative-ion electrospray ionisation mass spectrum of (TBA)31 could be assigned to ion aggregates containing 1 or fragments derived from 1, including {(TBA)(2)[(iPrO)TiMo5O18]}, {(TBA){((PrO)-Pr-i)TiMo5O18]}(2-), {((PrO)-Pr-i)TiMo2O8}(-) (TiMo5O18}(2-), (TiMo4O15}(2-) and (Mo3O10}(2-).

Publication metadata

Author(s): Errington RJ, Coyle L, Middleton PS, Murphy CJ, Clegg W, Harrington RW

Publication type: Article

Publication status: Published

Journal: Journal of Cluster Science

Year: 2010

Volume: 21

Issue: 3

Pages: 503-514

Print publication date: 24/05/2010

ISSN (print): 1040-7278

ISSN (electronic): 1572-8862

Publisher: Springer New York LLC


DOI: 10.1007/s10876-010-0329-3


Altmetrics provided by Altmetric