Gd4NiB13 crystallizes in the tetragonal P4/mnc space group. Gd(1) is bonded in a 16-coordinate geometry to one Ni(1), one B(1), six equivalent B(2), and eight equivalent B(3) atoms. Ni(1) is bonded to four equivalent Gd(1) and eight equivalent B(3) atoms to form NiGd4B8 cuboctahedra that share corners with four equivalent B(1)Gd4B8 cuboctahedra and faces with two equivalent B(1)Gd4B8 cuboctahedra. There are three inequivalent B sites. In the first B site, B(1) is bonded to four equivalent Gd(1) and eight equivalent B(3) atoms to form BGd4B8 cuboctahedra that share corners with four equivalent Ni(1)Gd4B8 cuboctahedra and faces with two equivalent Ni(1)Gd4B8 cuboctahedra. In the second B site, B(2) is bonded in a 9-coordinate geometry to six equivalent Gd(1), one B(2), and two equivalent B(3) atoms. In the third B site, B(3) is bonded in a 9-coordinate geometry to four equivalent Gd(1), one Ni(1), one B(1), one B(2), and two equivalent B(3) atoms.
Gd4NiB13 crystallizes in the tetragonal P4/mnc space group. Gd(1) is bonded in a 16-coordinate geometry to one Ni(1), one B(1), six equivalent B(2), and eight equivalent B(3) atoms. The Gd(1)-Ni(1) bond length is 2.72 Å. The Gd(1)-B(1) bond length is 2.67 Å. There are a spread of Gd(1)-B(2) bond distances ranging from 2.75-2.91 Å. There are a spread of Gd(1)-B(3) bond distances ranging from 2.58-2.73 Å. Ni(1) is bonded to four equivalent Gd(1) and eight equivalent B(3) atoms to form NiGd4B8 cuboctahedra that share corners with four equivalent B(1)Gd4B8 cuboctahedra and faces with two equivalent B(1)Gd4B8 cuboctahedra. All Ni(1)-B(3) bond lengths are 2.20 Å. There are three inequivalent B sites. In the first B site, B(1) is bonded to four equivalent Gd(1) and eight equivalent B(3) atoms to form BGd4B8 cuboctahedra that share corners with four equivalent Ni(1)Gd4B8 cuboctahedra and faces with two equivalent Ni(1)Gd4B8 cuboctahedra. All B(1)-B(3) bond lengths are 2.13 Å. In the second B site, B(2) is bonded in a 9-coordinate geometry to six equivalent Gd(1), one B(2), and two equivalent B(3) atoms. The B(2)-B(2) bond length is 1.94 Å. Both B(2)-B(3) bond lengths are 1.79 Å. In the third B site, B(3) is bonded in a 9-coordinate geometry to four equivalent Gd(1), one Ni(1), one B(1), one B(2), and two equivalent B(3) atoms. Both B(3)-B(3) bond lengths are 1.82 Å.