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The NOE experiment is demonstrated here as a viable tool in the NMR analyses of substituted borane and heteroborane compounds. We demonstrate that the saturation of 1 H NMR signals assigned to a substituent ligand can give rise to enhancements of signals arising from B-H's within a borane cage. These enhancements, though small (ca. 1-2%), are clearly detectable and have been used to confirm...