(a) [2 + 8 + 4] assembly of 5, 6 and 7 to furnish cage 1; 5, 6 and 8 to furnish cage 2; 5, 6 and 9 to furnish cage 3; and 5, 6 and 10 to furnish cage 4 via heteroligation-directed self-assembly of 90° Pt(II) acceptors and pyridyl and carboxylate ligands. (b−k) Partial 31P{1H} (b−f) and 1H NMR (g−k) spectra (CD2Cl2) of building blocks 5 (g) and 6 (b) and tetragonal cage 1 (c, h), cage 2 (d, i), cage 3 (e, j), and cage 4 (f, k) highlighting the changes associated with the transformation from diverse building blocks into discrete metallacages.