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(5), one O(6), one O(7), and one O(8) atom. The Gd(1)-O(1) bond length is 2.51 Å. The Gd(1)-O(10) bond length is 2.44 Å. The Gd(1)-O(11) bond length is 2.42 Å. The Gd(1)-O(2) bond length is 2.44 Å. The Gd(1)-O(5) bond length is 2.37 Å. The Gd(1)-O(6) bond length is 2.40 Å. The Gd(1)-O(7) bond length is 2.36 Å. The Gd(1)-O(8) bond length is 2.28 Å. Cu(1) is bonded to two equivalent N(1), two equivalent O(3), and two equivalent O(4) 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(3) bond lengths are 2.39 Å. Both Cu(1)-O(4) bond lengths are 2.03 Å. There are seven inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(6), one N(1), and one H(1) atom. The C(1)-C(6) bond length is 1.39 Å. The C(1)-N(1) bond length is 1.34 Å. The C(1)-H(1) bond length is 1.09 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one C(5), one N(1), and one H(2) atom. The C(2)-C(5) bond length is 1.40 Å. The C(2)-N(1) bond length is 1.35 Å. The C(2)-H(2) bond length is 1.09 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(6), and one O(9) atom. The C(3)-C(5) bond length is 1.50 Å. The C(3)-O(6) bond length is 1.29 Å. The C(3)-O(9) bond length is 1.26 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(6), one O(7), and one O(8) atom. The C(4)-C(6) bond length is 1.50 Å. The C(4)-O(7) bond length is 1.27 Å. The C(4)-O(8) bond length is 1.27 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(2), one C(3), and one C(7) atom. The C(5)-C(7) bond length is 1.40 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one C(1), one C(4), and one C(7) atom. The C(6)-C(7) bond length is 1.39 Å. In the seventh C site, C(7) is bonded in a distorted single-bond geometry to one C(5), one C(6), and one H(3) atom. The C(7)-H(3) bond length is 1.09 Å. N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(2) atom. There are nine inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(2) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(7) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(10) atom. The H(4)-O(10) bond length is 0.99 Å. In the fifth H site, H(5) is bonded in a linear geometry to one O(10) and one O(9) atom. The H(5)-O(10) bond length is 1.02 Å. The H(5)-O(9) bond length is 1.56 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 1.00 Å. In the seventh H site, H(7) is bonded in a single-bond geometry to one O(11) atom. The H(7)-O(11) bond length is 0.98 Å. In the eighth H site, H(8) is bonded in a single-bond geometry to one O(4) atom. The H(8)-O(4) bond length is 0.98 Å. In the ninth H site, H(9) is bonded in a distorted single-bond geometry to one O(2) and one O(4) atom. The H(9)-O(2) bond length is 1.68 Å. The H(9)-O(4) bond length is 1.00 Å. S(1) is bonded to one O(1), one O(2), one O(3), and one O(5) atom to form SO4 tetrahedra that share  a cornercorner with one Cu(1)N2O4 octahedra. The corner-sharing octahedral tilt angles are 43°. The S(1)-O(1) bond length is 1.50 Å. The S(1)-O(2) bond length is 1.52 Å. The S(1)-O(3) bond length is 1.47 Å. The S(1)-O(5) bond length is 1.48 Å. There are eleven inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one Gd(1) and one S(1) atom. In the second O site, O(2) is bonded in a distorted T-shaped geometry to one Gd(1), one H(9), and one S(1) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one Cu(1) and one S(1) atom. In the fourth O site, O(4) is bonded in a distorted water-like geometry to one Cu(1), one H(8), and one H(9) atom. In the fifth O site, O(5) is bonded in a distorted bent 150 degrees geometry to one Gd(1) and one S(1) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Gd(1) and one C(3) atom. In the seventh O site, O(7) is bonded in a distorted bent 120 degrees geometry to one Gd(1) and one C(4) atom. In the eighth O site, O(8) is bonded in a distorted linear geometry to one Gd(1) and one C(4) atom. In the ninth O site, O(9) is bonded in a bent 120 degrees geometry to one C(3) and one H(5) atom. In the tenth O site, O(10) is bonded in a water-like geometry to one Gd(1), one H(4), and one H(5) atom. In the eleventh O site, O(11) is bonded in a distorted water-like geometry to one Gd(1), one H(6), and one H(7) atom. Linkers: 2 [O]C(=O)c1cncc(C([O])=O)c1. Metal clusters: 2 [Gd] ,1 [Cu]. The MOF has largest included sphere 2.05 A, density 2.75 g/cm3, surface area 2177.56 m2/g, accessible volume 0.07 cm3/g