NiSb2 is Marcasite structured and crystallizes in the orthorhombic Pnnm space group. Ni(1) is bonded to six equivalent Sb(1) atoms to form a mixture of corner and edge-sharing NiSb6 octahedra. The corner-sharing octahedral tilt angles are 56°. Sb(1) is bonded in a 4-coordinate geometry to three equivalent Ni(1) and one Sb(1) atom.
NiSb2 is Marcasite structured and crystallizes in the orthorhombic Pnnm space group. Ni(1) is bonded to six equivalent Sb(1) atoms to form a mixture of corner and edge-sharing NiSb6 octahedra. The corner-sharing octahedral tilt angles are 56°. There are two shorter (2.54 Å) and four longer (2.58 Å) Ni(1)-Sb(1) bond lengths. Sb(1) is bonded in a 4-coordinate geometry to three equivalent Ni(1) and one Sb(1) atom. The Sb(1)-Sb(1) bond length is 2.88 Å.