City of Kent, Estados Unidos
An application of two-dimensional 31P NMR spectroscopy is demonstrated through the characterization of linkage isomers of tetraammine(triphosphato)cobalt(III) chelates and metal-promoted hydrolysis of inorganic triphosphate ion. Unambiguous assignments of 31P resonances for two isomers, α,γ and β,γ chelates, were achieved by the direct through-bond connectivities among the three phosphate groups. The lack of such connectivity also helped to identify cobalt(III)-catalyzed hydrolysis products, orthophosphate and pyrophosphate ions. The experiment provides background information on 2-D NMR spectroscopy including the significance of pulse calibration, relaxation, evolution and mixing times, data processing, and finally, hands-on training for performing 2-D NMR experiments. The experiment is ideally suited for a senior laboratory course and may be included in the core inorganic curriculum required for a certified ACS B.S. degree.
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