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K3Rh crystallizes in the hexagonal P6_3/mmc space group. The structure is three-dimensional. K is bonded in a 2-coordinate geometry to four equivalent Rh atoms. There are two shorter (3.45 Å) and two longer (3.95 Å) K–Rh bond lengths. Rh is bonded to twelve equivalent K atoms to form a mixture of distorted corner and face-sharing RhK12 cuboctahedra.
K(K(NO2)3)2Rh crystallizes in the cubic Fm-3m space group. The structure is three-dimensional and consists of four potassium molecules, four rhodium molecules, and one K(NO2)3 framework. In the K(NO2)3 framework, K1+ is bonded in a distorted q4 geometry to twelve equivalent O2- atoms. All K–O bond lengths are 2.68 Å. N3+ is bonded in a rectangular see-saw-like geometry to four equivalent O2- atoms. All N–O bond lengths are 2.12 Å. O2- is bonded to two equivalent K1+, two equivalent N3+, and one O2- atom to form a mixture of distorted edge and corner-sharing OK2N2O square pyramids. The O–O bond length is 1.34 Å.