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Abstract
Here we describe the formation of a trigonal prismatic cage, utilizing 2-formyl-1,8-naphthyridine subcomponents to bind pairs of silver(I) ions in close proximity. This cage is the first example of a new class of subcomponent self-assembled polyhedral structures having bimetallic vertices, as opposed to the single metal centers that typically serve as structural elements within such cages. Our new cage self-assembles around a pair of anionic templates, which are shown by crystallographic and solution-phase data to bind within the central cavity of the structure. Many different anions serve as competent templates and guests. Elongated dianions, such as the strong oxidizing agent peroxysulfate, also serve to template and bind within the cavity of the prism. The principle of using subcomponents that have more than one spatially close, but nonchelating, binding site may thus allow access to other higher-order structures with multimetallic vertices.
Highlights
We describe the formation of a trigonal prismatic cage, utilizing 2-formyl-1,8-naphthyridine subcomponents to bind pairs of silver(I) ions in close proximity
Imine arms of each ligand connect vertices belonging to the same triangular face, while the third arm bridges to a vertex of the opposing triangular face, through the interior of the structure
Cl distance was found to be 4.88(2) Å (Figure 3b). These results suggest that hydrogen bonding between the two HSO4− anions within the cage cavity,[41] coupled with interactions between the internally directed protons of the cage and the HSO4−, facilitates close proximity between bisulfate anions
Summary
Disorder, nonincluded anions, and solvent molecules have been omitted for clarity. imine arms of each ligand connect vertices belonging to the same triangular face, while the third arm bridges to a vertex of the opposing triangular face, through the interior of the structure. The crystal structure revealed that the triangular prism bound a pair of ClO4− anions within its elongated cavity Both encapsulated anions benefit from nonclassical hydrogen bonding interactions with internally directed protons of the cage, with CH···anion distances in the range 2.4−2.7 Å. Imide (AgNTf2) was used as the silver(I) source in all cases Following treatment of this salt with subcomponents A and B, it was found that no well-defined structure formed in the absence of a competent template ion (Figure S58), even after heating the mixture to 60 °C in an inert atmosphere for 3 days. These changes in the structure of 1 are attributed to two factors: structural tuning of 1 to maximize favorable interactions with the internalized anions and crystal packing effects. Detailed descriptions of synthetic procedures; characterization of new compounds; spectroscopic data (PDF)
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