Four-component intergrowth structures of the metal-ion cage complexes fac-(1,5,9,13,20-pentamethyl-3,7,11,15,18,22-hexaazabicyclo[7.7.7]tricosane) M^II diperchlorate hydrate, [M(C₂₂H₄₈N₆)](ClO₄) ₂xH₂O, M = Ni, Zn

The crystal structures of (1,5,9,13,20-pentamethyl-3,7,11,15,18,22-hexaazabicyclo[7.7.7]tricosane-K ⁶N,N′,N″,N‴,N″″,N‴″) nickel(II) diperchlorate-x(water) (x = 0.530), [Ni(C₂₂H₄₈N₆)](ClO₄) ₂.0.530H₂O, and (1,5,9,13,20-pentamethyl-3,7,11,15,18,22-hexaazabicyclo-[7.7.7]tricosane-K ⁶N,N′,N″,N‴,N″″,N‴″) zinc(II) diperchlorate-x(water) (x = 0.608), [Zn(C₂₂H₄₈N₆)](ClO₄) ₂.0.608H₂O, are isomorphic and each is described as an intergrowth of four substructures, consistent with different modulations of an idealized parent structure of space group C2/c. Two substructures correspond to alternative orientations of a C1 structure for which x = O in the general formula [M(C₂₂H₄₈N₆)](ClO₄) ₂.xH₂O, and two substructures correspond to alternative origins of a P2₁/n structure for which x = 1. Twinning also occurs. An analysis of the pseudosymmetry, a description of the refinement and a description of the refined structures are presented. The MN₆ coordination geometry is essentially octahedral, in contrast to the trigonal-prismatic geometry observed for the Cd^II and Hg^II complexes of the same ligand.