Ni(WB)3 crystallizes in the orthorhombic Cmcm space group. There are two inequivalent W sites. In the first W site, W(1) is bonded in a 9-coordinate geometry to three equivalent Ni(1), two equivalent B(2), and four equivalent B(1) atoms. In the second W site, W(2) is bonded in a 7-coordinate geometry to two equivalent Ni(1), three equivalent B(2), and four equivalent B(1) atoms. Ni(1) is bonded to two equivalent W(2), six equivalent W(1), and four equivalent B(1) atoms to form a mixture of distorted corner, face, and edge-sharing NiB4W8 cuboctahedra. There are two inequivalent B sites. In the first B site, B(1) is bonded in a 9-coordinate geometry to two equivalent W(2), four equivalent W(1), two equivalent Ni(1), and one B(2) atom. In the second B site, B(2) is bonded in a 9-coordinate geometry to three equivalent W(2), four equivalent W(1), and two equivalent B(1) atoms.
Ni(WB)3 crystallizes in the orthorhombic Cmcm space group. There are two inequivalent W sites. In the first W site, W(1) is bonded in a 9-coordinate geometry to three equivalent Ni(1), two equivalent B(2), and four equivalent B(1) atoms. There are two shorter (2.66 Å) and one longer (2.69 Å) W(1)-Ni(1) bond length. Both W(1)-B(2) bond lengths are 2.31 Å. There are a spread of W(1)-B(1) bond distances ranging from 2.32-2.52 Å. In the second W site, W(2) is bonded in a 7-coordinate geometry to two equivalent Ni(1), three equivalent B(2), and four equivalent B(1) atoms. Both W(2)-Ni(1) bond lengths are 2.68 Å. There are two shorter (2.36 Å) and one longer (2.46 Å) W(2)-B(2) bond length. All W(2)-B(1) bond lengths are 2.35 Å. Ni(1) is bonded to two equivalent W(2), six equivalent W(1), and four equivalent B(1) atoms to form a mixture of distorted corner, face, and edge-sharing NiB4W8 cuboctahedra. All Ni(1)-B(1) bond lengths are 2.08 Å. There are two inequivalent B sites. In the first B site, B(1) is bonded in a 9-coordinate geometry to two equivalent W(2), four equivalent W(1), two equivalent Ni(1), and one B(2) atom. The B(1)-B(2) bond length is 1.87 Å. In the second B site, B(2) is bonded in a 9-coordinate geometry to three equivalent W(2), four equivalent W(1), and two equivalent B(1) atoms.