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Abstract Structural DNA nanotechnology enables the self‐organization of matter at the nanometer scale, but approaches to expand the inorganic and electrical functionality of these scaffolds remain limited. Developments in nucleic acid metallics have enabled the incorporation of site‐specific metal ions in DNA duplexes and provide a means of functionalizing the double helix with atomistic precision. Here a class of 2D DNA nanostructures that incorporate the cytosine‐Ag⁺‐cytosine (dC:Ag⁺:dC) base pair as a chemical trigger for self‐assembly is described. It is demonstrated that Ag⁺‐functionalized DNA can undergo programmable assembly into large arrays and rings, and can be further coassembled with guanine tetraplexes (G4). It is shown that 2D DNA lattices can be assembled with a variety of embedded nanowires at tunable spacing. These results serve as a foundation for further development of self‐assembled, metalated DNA nanostructures, with potential for high‐precision DNA nanoelectronics with nanometer pitch. 

Abstract The DNA tensegrity triangle is known to reliably self‐assemble into a 3D rhombohedral crystalline lattice via sticky‐end cohesion. Here, the library of accessible motifs is expanded through covalent extensions of intertriangle regions and sticky‐end‐coordinated linkages of adjacent triangles with double helical segments using both geometrically symmetric and asymmetric configurations. The molecular structures of 18 self‐assembled architectures at resolutions of 3.32–9.32 Å are reported; the observed cell dimensions, cavity sizes, and cross‐sectional areas agree with theoretical expectations. These data demonstrate that fine control over triclinic and rhombohedral crystal parameters and the customizability of more complex 3D DNA lattices are attainable via rational design. It is anticipated that augmented DNA architectures may be fine‐tuned for the self‐assembly of designer nanocages, guest–host complexes, and proscriptive 3D nanomaterials, as originally envisioned. Finally, designer asymmetric crystalline building blocks can be seen as a first step toward controlling and encoding information in three dimensions.