Figure shows an 1 H NMR spectrum obtained after extracting 9 from 9ÌC using ethyl acetate (see Figures for further NMR characterization). In contrast to the relatively complex spectrum of T, cage C's spectrum features only four aromatic peaks (which integrate to 12, 12, 12, and 12, i.e., four TImB molecules) and two aliphatic peaks (whose integration gives 72 and 24, corresponding to six TMEDA molecules). We made extensive efforts to confirm the proposed structure of C by single-crystal X-ray crystallography. First, we worked with aqueous solutions obtained by extracting the 9 from 9ÌC using ethyl acetate. However, slow evaporation of water and acetone vapor diffusion at various temperatures resulted in single crystals of pure T. Attempts to crystallize C in the presence of various salts afforded the same result.