A procedure for the formation of a nitrate-encapsulating tripalladium(II) cage self-assembly of Pd(NO) with 1,3-bis(dimethyl(pyridin-4-yl)silyl)propane (L) was developed. The self-assembly reaction initially produces spiro-type macrocycles, PdL, and finally results in transformation into a nitrate-encapsulated cage, [(NO)@PdL], in the mother liquor. The reaction of PdX (X = BF, ClO, PF, and CFSO instead of NO) with L gives rise to a spiro species, PdL, as the final product, and anion exchange of the spiro products, [PdL](X), with NO produces the tripalladium cage [(NO)@PdL].
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