Table . Hits identified from the automated analysis that were taken forward for further H NMR interpretation to identify whether a single assembly or a mixture of species had been formed as the major product(s), and if single, the structural outcome. In the case of all three scale-ups, the tetrahedra could not be fully isolated from the minor component of the mixtures, which was assumed to be a mixture of M2X3 helicate and/or mesocate species as observed by HRMS. By finding the ratio of the imine N=CH signal integrations for the tetrahedron and the M2X2 species in each mixture, the molar composition of the tetrahedron in the mixtures could be calculatedthe signal at 8.5-8.6 ppm corresponds to the 9H resonance of the helicate and the signal at 8.7-8.8 ppm corresponds to the 12H resonance in the tetrahedron, similar to the related structures found by Bilbeisi et al. For the samples, this gives approximate tetrahedron:helicate molar ratios of 1:0.04 in cage 1, 1:0.19 for cage 2 and 1:0.17 for cage 3.