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NiFe crystallizes in the orthorhombic Cmmm space group. The structure is three-dimensional. Fe is bonded in a 8-coordinate geometry to four equivalent Fe and four equivalent Ni atoms. All Fe–Fe bond lengths are 2.45 Å. All Fe–Ni bond lengths are 2.44 Å. Ni is bonded in a 8-coordinate geometry to four equivalent Fe and four equivalent Ni atoms. All Ni–Ni bond lengths are 2.45 Å.
NiFe2 crystallizes in the trigonal P-3m1 space group. The structure is three-dimensional. Fe is bonded to nine equivalent Fe and three equivalent Ni atoms to form FeFe9Ni3 cuboctahedra that share corners with three equivalent NiFe6Ni6 cuboctahedra, corners with nine equivalent FeFe9Ni3 cuboctahedra, edges with nine equivalent NiFe6Ni6 cuboctahedra, edges with fifteen equivalent FeFe9Ni3 cuboctahedra, faces with six equivalent NiFe6Ni6 cuboctahedra, and faces with twelve equivalent FeFe9Ni3 cuboctahedra. There are six shorter (2.52 Å) and three longer (2.59 Å) Fe–Fe bond lengths. All Fe–Ni bond lengths are 2.52 Å. Ni is bonded to six equivalent Fe and six equivalent Ni atoms to form NiFe6Ni6 cuboctahedra that share corners with six equivalent FeFe9Ni3 cuboctahedra, corners with six equivalent NiFe6Ni6 cuboctahedra, edges with six equivalent NiFe6Ni6 cuboctahedra, edges with eighteen equivalent FeFe9Ni3 cuboctahedra, faces with six equivalent NiFe6Ni6 cuboctahedra, and faces with twelve equivalent FeFe9Ni3 cuboctahedra. All Ni–Ni bond lengths are 2.52 Å.