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Reddish-brown crystals of [Na (12-crown-4) 2] I 3 (1) and [Rb (12-crown-4) 2] I 3 (2) were formed through the reaction of NaI or RbI, I 2 and 12-crown-4 in ethanol. Both structures are triclinic, space group P1̅ with Z= 2. The lattice parameters are a= 8.505 (2), b= 14.280 (3), c= 10.695 (2) Å and α= 89.86 (2)○, β= 80.00 (2)○ and γ= 85.90 (2)○; and a= 10.694 (2), b= 11.598 (2), c= 12.718 (2) Å and α= 71.00 (2)○, β= 86.97 (2)○ and γ= 67.710 (10)○ for 1 and 2, respectively. Both crystal structures contain one independent complex cation without crystallographic symmetry. The anionic parts of both structures consist of two crystallographically independent, isolated, triiodide anions I 3− with crystallographic inversion symmetry. The cations are distorted sandwich-like complexes with two 12-crown-4 molecules surrounding the alkali metal atom in the center.