Gd4Ni13C4 crystallizes in the orthorhombic Cmmm space group. There are two inequivalent Gd sites. In the first Gd site, Gd(1) is bonded in a 14-coordinate geometry to two equivalent Ni(1), two equivalent Ni(3), two equivalent Ni(5), four equivalent Ni(2), and four equivalent Ni(4) atoms. In the second Gd site, Gd(2) is bonded in a 15-coordinate geometry to one Ni(5), two equivalent Ni(3), four equivalent Ni(2), four equivalent Ni(4), and four equivalent C(2) atoms. There are five inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to four equivalent Gd(1), four equivalent Ni(4), and four equivalent Ni(5) atoms to form NiGd4Ni8 cuboctahedra that share corners with four equivalent C(1)Ni6 octahedra and faces with two equivalent Ni(1)Gd4Ni8 cuboctahedra. The corner-sharing octahedral tilt angles are 33°. In the second Ni site, Ni(2) is bonded in a distorted bent 150 degrees geometry to two equivalent Gd(1), two equivalent Gd(2), one C(1), and one C(2) atom. In the third Ni site, Ni(3) is bonded in a linear geometry to two equivalent Gd(1), two equivalent Gd(2), and two equivalent C(1) atoms. In the fourth Ni site, Ni(4) is bonded in a single-bond geometry to two equivalent Gd(1), two equivalent Gd(2), one Ni(1), two equivalent Ni(5), and one C(1) atom. In the fifth Ni site, Ni(5) is bonded in a 9-coordinate geometry to one Gd(2), two equivalent Gd(1), two equivalent Ni(1), and four equivalent Ni(4) atoms. There are two inequivalent C sites. In the first C site, C(1) is bonded to two equivalent Ni(2), two equivalent Ni(3), and two equivalent Ni(4) atoms to form CNi6 octahedra that share corners with two equivalent Ni(1)Gd4Ni8 cuboctahedra and corners with two equivalent C(1)Ni6 octahedra. The corner-sharing octahedra are not tilted. In the second C site, C(2) is bonded in a 7-coordinate geometry to four equivalent Gd(2), two equivalent Ni(2), and one C(2) atom.
Gd4Ni13C4 crystallizes in the orthorhombic Cmmm space group. There are two inequivalent Gd sites. In the first Gd site, Gd(1) is bonded in a 14-coordinate geometry to two equivalent Ni(1), two equivalent Ni(3), two equivalent Ni(5), four equivalent Ni(2), and four equivalent Ni(4) atoms. Both Gd(1)-Ni(1) bond lengths are 2.96 Å. Both Gd(1)-Ni(3) bond lengths are 3.02 Å. Both Gd(1)-Ni(5) bond lengths are 2.66 Å. All Gd(1)-Ni(2) bond lengths are 2.81 Å. All Gd(1)-Ni(4) bond lengths are 3.03 Å. In the second Gd site, Gd(2) is bonded in a 15-coordinate geometry to one Ni(5), two equivalent Ni(3), four equivalent Ni(2), four equivalent Ni(4), and four equivalent C(2) atoms. The Gd(2)-Ni(5) bond length is 2.63 Å. Both Gd(2)-Ni(3) bond lengths are 3.19 Å. All Gd(2)-Ni(2) bond lengths are 2.91 Å. All Gd(2)-Ni(4) bond lengths are 3.02 Å. All Gd(2)-C(2) bond lengths are 2.72 Å. There are five inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to four equivalent Gd(1), four equivalent Ni(4), and four equivalent Ni(5) atoms to form NiGd4Ni8 cuboctahedra that share corners with four equivalent C(1)Ni6 octahedra and faces with two equivalent Ni(1)Gd4Ni8 cuboctahedra. The corner-sharing octahedral tilt angles are 33°. All Ni(1)-Ni(4) bond lengths are 2.49 Å. All Ni(1)-Ni(5) bond lengths are 2.40 Å. In the second Ni site, Ni(2) is bonded in a distorted bent 150 degrees geometry to two equivalent Gd(1), two equivalent Gd(2), one C(1), and one C(2) atom. The Ni(2)-C(1) bond length is 1.88 Å. The Ni(2)-C(2) bond length is 1.91 Å. In the third Ni site, Ni(3) is bonded in a linear geometry to two equivalent Gd(1), two equivalent Gd(2), and two equivalent C(1) atoms. Both Ni(3)-C(1) bond lengths are 1.93 Å. In the fourth Ni site, Ni(4) is bonded in a single-bond geometry to two equivalent Gd(1), two equivalent Gd(2), one Ni(1), two equivalent Ni(5), and one C(1) atom. Both Ni(4)-Ni(5) bond lengths are 2.43 Å. The Ni(4)-C(1) bond length is 1.87 Å. In the fifth Ni site, Ni(5) is bonded in a 9-coordinate geometry to one Gd(2), two equivalent Gd(1), two equivalent Ni(1), and four equivalent Ni(4) atoms. There are two inequivalent C sites. In the first C site, C(1) is bonded to two equivalent Ni(2), two equivalent Ni(3), and two equivalent Ni(4) atoms to form CNi6 octahedra that share corners with two equivalent Ni(1)Gd4Ni8 cuboctahedra and corners with two equivalent C(1)Ni6 octahedra. The corner-sharing octahedra are not tilted. In the second C site, C(2) is bonded in a 7-coordinate geometry to four equivalent Gd(2), two equivalent Ni(2), and one C(2) atom. The C(2)-C(2) bond length is 1.36 Å.