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FeBr3 is Bismuth triodide structured and crystallizes in the trigonal R-3 space group. The structure is two-dimensional and consists of three FeBr3 sheets oriented in the (0, 0, 1) direction. Fe3+ is bonded to six equivalent Br1- atoms to form edge-sharing FeBr6 octahedra. All Fe–Br bond lengths are 2.43 Å. Br1- is bonded in a water-like geometry to two equivalent Fe3+ atoms.
FeBr3NH4 crystallizes in the monoclinic P2_1 space group. The structure is one-dimensional and consists of two ammonium molecules and one FeBr3 ribbon oriented in the (0, 1, 0) direction. In the FeBr3 ribbon, Fe2+ is bonded to six Br1- atoms to form face-sharing FeBr6 octahedra. There are a spread of Fe–Br bond distances ranging from 2.61–2.65 Å. There are three inequivalent Br1- sites. In the first Br1- site, Br1- is bonded in a 2-coordinate geometry to two equivalent Fe2+ atoms. In the second Br1- site, Br1- is bonded in a 2-coordinate geometry to two equivalent Fe2+ atoms. In the third Br1- site, Br1- is bonded in a 2-coordinate geometry to two equivalent Fe2+ atoms.