Using the Rapid Injection NMR (RINMR) system, we have been able to observe the formation of the Cu(III) species in THF-d₈ at _¯100 °C from the injection of 2-cyclohexenone into a mixture of TMSCl and Me₂CuLi●LiCN.  The reaction proceeds almost exclusively to the Cu(III) intermediate, 1.   The intermediate is stable for hours at _¯100 °C allowing extensive characterization by multiple NMR techniques.  Compound 1 has been characterized by ¹H & ¹³C NMR, NOESY, HMQC and HMBC.   The two bond coupling constants (¹³C-Cu-¹³C) around ligands of the ¹³C enriched 1 reveal the Cu(III)  intermediate to have a square planar geometry.  Upon warming to _¯80 °C, the reductive elimination product, 2, can be observed to form as 1 disappears.