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Single Nanoscale Cluster Species Revealed by 1H NMR Diffusion-Ordered Spectroscopy and Small-Angle X-ray Scattering


  • This work was generously supported by the NSF Center for Sustainable Materials Chemistry (grant numbers CHE-0847926 and CHE-1102637), an NSF GK12 fellowship to A.F.O. (DGE-0742540), the Air Force Research Laboratory (under grant number FA8650-05-1-5041) and the M. J. Murdock Charitable Trust. The authors thank Profs. Douglas A. Keszler and Sophia E. Hayes for helpful suggestions in writing this manuscript. The University of Oregon NMR facilities are supported by NSF CHE-0923589. D.W.J. is a Scialog Fellow of Research Corporation for Science Advancement and gratefully acknowledges additional support provided to assist this project.


original image

A solved structure: The hydrated Ga13 cluster, [Ga133-OH)6(μ-OH)18(H2O)24](NO3)15], persists as a discrete nanoscale structure in an aqueous polar solvent at millimolar concentration. SAXS data confirm the presence of Ga13 in dimethyl sulfoxide (DMSO). In aqueous [D6]DMSO 1H NMR signals for the hydroxo and aquo ligands of Ga13 were detected, thus showing a cluster with a hydrodynamic radius of (11.2±0.8) Å (see picture).