Application of the NOE experiment to the analysis of boron hydride derivatives: Confirming the assignments of the pseudocloso-complex [1,2-Ph₂-3-{Cp*-IrC₂B₉H₉] (Cp*=η⁵-C₅Me₅) and the closo-compounds 1-Ph-1,2-C₂B₁₀H₁₁ and 1-Ph-2-Me-1,2-C₂B₁₀H₁₀

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 of¹H 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 assignments for the pseudocloso-complex [1,2-Ph₂-3-{Cp*}-3,1,2-IrC₂B₉H ₉] (Cp*=?⁵-C₅Me₅), the mono-substituted closo-carbaborane 1-Ph-1,2-C₂B₁₀H₁₁ and the di-substituted closo-carbaborane 1-Ph-2-Me-1,2-C₂B₁₀H₁₀. We compare the results of applying three alternative experimental NOE procedures to these problems, namely phase sensitive 2D NOESY, 1D truncated driven NOE and 1D DPFGSE-NOE. The differences between the quality and relevance of these procedures to the study of borane and heteroborane derivatives are discussed. © 1999 Elsevier Science S.A.