Yb4NiB13 crystallizes in the tetragonal P4/mnc space group. Yb(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 Yb(1) and eight equivalent B(3) atoms to form NiYb4B8 cuboctahedra that share corners with four equivalent B(1)Yb4B8 cuboctahedra and faces with two equivalent B(1)Yb4B8 cuboctahedra. There are three inequivalent B sites. In the first B site, B(1) is bonded to four equivalent Yb(1) and eight equivalent B(3) atoms to form BYb4B8 cuboctahedra that share corners with four equivalent Ni(1)Yb4B8 cuboctahedra and faces with two equivalent Ni(1)Yb4B8 cuboctahedra. In the second B site, B(2) is bonded in a 9-coordinate geometry to six equivalent Yb(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 Yb(1), one Ni(1), one B(1), one B(2), and two equivalent B(3) atoms.
Yb4NiB13 crystallizes in the tetragonal P4/mnc space group. Yb(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 Yb(1)-Ni(1) bond length is 2.65 Å. The Yb(1)-B(1) bond length is 2.74 Å. There are a spread of Yb(1)-B(2) bond distances ranging from 2.72-2.88 Å. There are a spread of Yb(1)-B(3) bond distances ranging from 2.57-2.69 Å. Ni(1) is bonded to four equivalent Yb(1) and eight equivalent B(3) atoms to form NiYb4B8 cuboctahedra that share corners with four equivalent B(1)Yb4B8 cuboctahedra and faces with two equivalent B(1)Yb4B8 cuboctahedra. All Ni(1)-B(3) bond lengths are 2.19 Å. There are three inequivalent B sites. In the first B site, B(1) is bonded to four equivalent Yb(1) and eight equivalent B(3) atoms to form BYb4B8 cuboctahedra that share corners with four equivalent Ni(1)Yb4B8 cuboctahedra and faces with two equivalent Ni(1)Yb4B8 cuboctahedra. All B(1)-B(3) bond lengths are 2.03 Å. In the second B site, B(2) is bonded in a 9-coordinate geometry to six equivalent Yb(1), one B(2), and two equivalent B(3) atoms. The B(2)-B(2) bond length is 1.91 Å. Both B(2)-B(3) bond lengths are 1.82 Å. In the third B site, B(3) is bonded in a 9-coordinate geometry to four equivalent Yb(1), one Ni(1), one B(1), one B(2), and two equivalent B(3) atoms. Both B(3)-B(3) bond lengths are 1.79 Å.