Yb2NiSb2 crystallizes in the trigonal R3m space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded in a 9-coordinate geometry to three equivalent Ni(1), three equivalent Sb(1), and three equivalent Sb(2) atoms. In the second Yb site, Yb(2) is bonded to one Ni(1), three equivalent Sb(1), and three equivalent Sb(2) atoms to form distorted YbNiSb6 pentagonal bipyramids that share  a cornercorner with one Sb(2)Yb6Ni pentagonal bipyramid and edges with six equivalent Yb(2)NiSb6 pentagonal bipyramids. Ni(1) is bonded in a body-centered cubic geometry to one Yb(2), three equivalent Yb(1), one Sb(2), and three equivalent Sb(1) atoms. There are two inequivalent Sb sites. In the first Sb site, Sb(1) is bonded in a distorted q6 geometry to three equivalent Yb(1), three equivalent Yb(2), and three equivalent Ni(1) atoms. In the second Sb site, Sb(2) is bonded to three equivalent Yb(1), three equivalent Yb(2), and one Ni(1) atom to form distorted SbYb6Ni pentagonal bipyramids that share  a cornercorner with one Yb(2)NiSb6 pentagonal bipyramid and edges with six equivalent Sb(2)Yb6Ni pentagonal bipyramids.
Yb2NiSb2 crystallizes in the trigonal R3m space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded in a 9-coordinate geometry to three equivalent Ni(1), three equivalent Sb(1), and three equivalent Sb(2) atoms. All Yb(1)-Ni(1) bond lengths are 2.80 Å. All Yb(1)-Sb(1) bond lengths are 3.22 Å. All Yb(1)-Sb(2) bond lengths are 3.11 Å. In the second Yb site, Yb(2) is bonded to one Ni(1), three equivalent Sb(1), and three equivalent Sb(2) atoms to form distorted YbNiSb6 pentagonal bipyramids that share  a cornercorner with one Sb(2)Yb6Ni pentagonal bipyramid and edges with six equivalent Yb(2)NiSb6 pentagonal bipyramids. The Yb(2)-Ni(1) bond length is 2.94 Å. All Yb(2)-Sb(1) bond lengths are 3.34 Å. All Yb(2)-Sb(2) bond lengths are 3.22 Å. Ni(1) is bonded in a body-centered cubic geometry to one Yb(2), three equivalent Yb(1), one Sb(2), and three equivalent Sb(1) atoms. The Ni(1)-Sb(2) bond length is 2.60 Å. All Ni(1)-Sb(1) bond lengths are 2.78 Å. There are two inequivalent Sb sites. In the first Sb site, Sb(1) is bonded in a distorted q6 geometry to three equivalent Yb(1), three equivalent Yb(2), and three equivalent Ni(1) atoms. In the second Sb site, Sb(2) is bonded to three equivalent Yb(1), three equivalent Yb(2), and one Ni(1) atom to form distorted SbYb6Ni pentagonal bipyramids that share  a cornercorner with one Yb(2)NiSb6 pentagonal bipyramid and edges with six equivalent Sb(2)Yb6Ni pentagonal bipyramids.