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Full Paper
Direct Synthesis and Mass Spectroscopic Observation of the {M40} Polyoxothiometalate Wheel
Article first published online: 18 OCT 2011
DOI: 10.1002/ejic.201100833
Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Additional Information
How to Cite
Miras, H. N., Zang, H. Y., Long, D.-L. and Cronin, L. (2011), Direct Synthesis and Mass Spectroscopic Observation of the {M40} Polyoxothiometalate Wheel. Eur. J. Inorg. Chem., 2011: 5105–5111. doi: 10.1002/ejic.201100833
Publication History
- Issue published online: 14 NOV 2011
- Article first published online: 18 OCT 2011
- Manuscript Received: 8 AUG 2011
Funded by
- Engineering and Physical Sciences Research Council (ESPRC)
- WestCHEM
- Royal Society of Edinburgh
- Marie Curie Actions
- University of Glasgow
Keywords:
- Molybdenum;
- Sulfur;
- Self-assembly;
- Oxothiometalates
Abstract
The nanosized, 2.2 nm, {Mo40} oxo(thio)metalate wheel was isolated in high yield using a direct synthetic procedure which involves acidification of a molybdate solution in the presence of the {Mo2O2S2}2+oxothio cation as the starting material. The [(Mo8O28)4(Mo2O2S2)4]24– wheel, 1a, was characterised by single-crystal X-ray diffraction analysis, IR, Raman, UV/Vis and flame atomic absorption spectroscopy (FAAS). Solid state and solution Raman spectroscopic studies allowed the unambiguous determination of the critical conditions by which compound 1 retains its integrity in solution. Electrospray ionisation mass spectrometry (ESI-MS) studies carried out on aqueous solutions of the crystalline material showed that the nanosized wheel retains its integrity in concentrated solutions. High resolution ESI-MS studies allowed the direct observation of the discrete wheel as well as the distinct self-assembly stages of its formation; from the fundamental building units through to the final formation of well resolved aggregations of 1D chains which is in agreement with the solid state studies.