Gd2CuC14H18S2(NO11)2 crystallizes in the triclinic P-1 space group. Gd(1) is bonded in a 8-coordinate geometry to one O(1), one O(10), one O(11), one O(2), one O(3), one O(6), one O(7), and one O(8) atom. The Gd(1)-O(1) bond length is 2.28 Å. The Gd(1)-O(10) bond length is 2.47 Å. The Gd(1)-O(11) bond length is 2.39 Å. The Gd(1)-O(2) bond length is 2.35 Å. The Gd(1)-O(3) bond length is 2.43 Å. The Gd(1)-O(6) bond length is 2.47 Å. The Gd(1)-O(7) bond length is 2.46 Å. The Gd(1)-O(8) bond length is 2.39 Å. Cu(1) is bonded to two equivalent N(1), two equivalent O(5), and two equivalent O(9) atoms to form CuN2O4 octahedra that share corners with two equivalent S(1)O4 tetrahedra. Both Cu(1)-N(1) bond lengths are 2.00 Å. Both Cu(1)-O(5) bond lengths are 2.38 Å. Both Cu(1)-O(9) bond lengths are 2.03 Å. There are seven inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one N(1), and one H(7) atom. The C(1)-C(2) bond length is 1.39 Å. The C(1)-N(1) bond length is 1.34 Å. The C(1)-H(7) bond length is 1.08 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(6) atom. The C(2)-C(3) bond length is 1.39 Å. The C(2)-C(6) bond length is 1.50 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2), one C(4), and one H(8) atom. The C(3)-C(4) bond length is 1.40 Å. The C(3)-H(8) bond length is 1.09 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(3), one C(5), and one C(7) atom. The C(4)-C(5) bond length is 1.40 Å. The C(4)-C(7) bond length is 1.50 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(4), one N(1), and one H(9) atom. The C(5)-N(1) bond length is 1.35 Å. The C(5)-H(9) bond length is 1.09 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(6)-O(1) bond length is 1.27 Å. The C(6)-O(2) bond length is 1.27 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(7)-O(3) bond length is 1.29 Å. The C(7)-O(4) bond length is 1.26 Å. N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(5) atom. There are nine inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(9) atom. The H(1)-O(9) bond length is 0.98 Å. In the second H site, H(2) is bonded in a distorted single-bond geometry to one O(7) and one O(9) atom. The H(2)-O(7) bond length is 1.64 Å. The H(2)-O(9) bond length is 1.01 Å. In the third H site, H(3) is bonded in a single-bond geometry to one O(10) atom. The H(3)-O(10) bond length is 0.98 Å. In the fourth H site, H(4) is bonded in a linear geometry to one O(10) and one O(4) atom. The H(4)-O(10) bond length is 1.02 Å. The H(4)-O(4) bond length is 1.56 Å. In the fifth H site, H(5) is bonded in a single-bond geometry to one O(11) atom. The H(5)-O(11) bond length is 1.00 Å. In the sixth H site, H(6) is bonded in a single-bond geometry to one O(11) atom. The H(6)-O(11) bond length is 0.98 Å. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(1) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(3) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(5) atom. S(1) is bonded to one O(5), one O(6), one O(7), and one O(8) atom to form SO4 tetrahedra that share  a cornercorner with one Cu(1)N2O4 octahedra. The corner-sharing octahedral tilt angles are 38°. The S(1)-O(5) bond length is 1.46 Å. The S(1)-O(6) bond length is 1.50 Å. The S(1)-O(7) bond length is 1.52 Å. The S(1)-O(8) bond length is 1.49 Å. There are eleven inequivalent O sites. In the first O site, O(1) is bonded in a distorted linear geometry to one Gd(1) and one C(6) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Gd(1) and one C(6) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one Gd(1) and one C(7) atom. In the fourth O site, O(4) is bonded in a water-like geometry to one C(7) and one H(4) atom. In the fifth O site, O(5) is bonded in a distorted bent 150 degrees geometry to one Cu(1) and one S(1) atom. In the sixth O site, O(6) is bonded in a distorted water-like geometry to one Gd(1) and one S(1) atom. In the seventh O site, O(7) is bonded in a 3-coordinate geometry to one Gd(1), one H(2), and one S(1) atom. In the eighth O site, O(8) is bonded in a 2-coordinate geometry to one Gd(1) and one S(1) atom. In the ninth O site, O(9) is bonded in a distorted water-like geometry to one Cu(1), one H(1), and one H(2) atom. In the tenth O site, O(10) is bonded in a water-like geometry to one Gd(1), one H(3), and one H(4) atom. In the eleventh O site, O(11) is bonded in a distorted water-like geometry to one Gd(1), one H(5), and one H(6) atom. Linkers: 2 [O]C(=O)c1cncc(C([O])=O)c1. Metal clusters: 2 [Gd] ,1 [Cu]. The MOF has largest included sphere 2.01 A, density 2.76 g/cm3, surface area 2117.72 m2/g, accessible volume 0.03 cm3/g