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The thermodynamically controlled syntheses of different di‐, tetra‐, and hexacavitand polyacylhydrazone nanocapsules are reported. [2+4]‐, [4+8]‐, and [6+12]‐nanocapsules assemble upon reacting a tetraformyl cavitand with two equivalents of isophthalic dihydrazide, or terephthalic dihydrazide in the presence of trifluoroacetic acid, whereby the building blocks are linked together through 8, 16, or...
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