GdC44H24S4(NO3)4 crystallizes in the tetragonal P4/mcc space group. Gd(1) is bonded in a 8-coordinate geometry to eight equivalent O(1) atoms. All Gd(1)-O(1) bond lengths are 2.35 Å. There are nine inequivalent C sites. In the first C site, C(1) is bonded in a distorted single-bond geometry to one C(2), one C(3), and one H(1) atom. The C(1)-C(2) bond length is 1.33 Å. The C(1)-C(3) bond length is 1.33 Å. The C(1)-H(1) bond length is 0.93 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(1), one C(4), and one H(2) atom. The C(2)-C(4) bond length is 1.36 Å. The C(2)-H(2) bond length is 0.93 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to two equivalent C(1) and one S(1) atom. The C(3)-S(1) bond length is 1.87 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(5) and two equivalent C(2) atoms. The C(4)-C(5) bond length is 1.54 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(4), one C(6), and one C(9) atom. The C(5)-C(6) bond length is 1.32 Å. The C(5)-C(9) bond length is 1.46 Å. In the sixth C site, C(6) is bonded in a distorted trigonal planar geometry to one C(5), one C(7), and one N(1) atom. The C(6)-C(7) bond length is 1.48 Å. The C(6)-N(1) bond length is 1.40 Å. In the seventh C site, C(7) is bonded in a single-bond geometry to one C(6) and one H(3) atom. The C(7)-H(3) bond length is 0.93 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one C(9) and one H(4) atom. The C(8)-C(9) bond length is 1.41 Å. The C(8)-H(4) bond length is 0.93 Å. In the ninth C site, C(9) is bonded in a distorted trigonal planar geometry to one C(5), one C(8), and one N(1) atom. The C(9)-N(1) bond length is 1.39 Å. N(1) is bonded in a water-like geometry to one C(6) and one C(9) atom. There are four 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(4) is bonded in a single-bond geometry to one C(8) atom. In the third H site, H(2) is bonded in a single-bond geometry to one C(2) atom. In the fourth H site, H(3) is bonded in a single-bond geometry to one C(7) atom. S(1) is bonded in a distorted trigonal non-coplanar geometry to one C(3), one O(2), and two equivalent O(1) atoms. The S(1)-O(2) bond length is 1.37 Å. Both S(1)-O(1) bond lengths are 1.47 Å. There are two inequivalent O sites. In the first O site, O(1) is bonded in a bent 150 degrees geometry to one Gd(1) and one S(1) atom. In the second O site, O(2) is bonded in a single-bond geometry to one S(1) atom. Linkers: 4 [O]S([O])([O])c1ccc(/C2=C3\C=C/C(=C(\c4ccc(S([O])([O])[O])cc4)C4=N/C(=C(/c5ccc(S([O])([O])[O])cc5)C5=CC=C([N]5)/C(c5ccc(S([O])([O])[O])cc5)=C5/C=CC2=N5)C=C4)[N]3)cc1. Metal clusters: 2 [Gd]. RCSR code: bcu. The MOF has largest included sphere 4.91 A, density 1.55 g/cm3, surface area 3808.85 m2/g, accessible volume 0.25 cm3/g