Yb2C10H8S(N2O7)2 crystallizes in the monoclinic C2/c space group. Yb(1) is bonded in a 8-coordinate geometry to one N(1), one O(1), one O(2), one O(3), one O(4), one O(5), one O(6), and one O(7) atom. The Yb(1)-N(1) bond length is 2.55 Å. The Yb(1)-O(1) bond length is 2.31 Å. The Yb(1)-O(2) bond length is 2.43 Å. The Yb(1)-O(3) bond length is 2.34 Å. The Yb(1)-O(4) bond length is 2.26 Å. The Yb(1)-O(5) bond length is 2.25 Å. The Yb(1)-O(6) bond length is 2.25 Å. The Yb(1)-O(7) bond length is 2.26 Å. There are five inequivalent C sites. In the first C site, C(1) is bonded in a distorted single-bond geometry to one C(2), one C(5), and one N(1) atom. The C(1)-C(2) bond length is 1.47 Å. The C(1)-C(5) bond length is 1.39 Å. The C(1)-N(1) bond length is 1.38 Å. In the second C site, C(2) is bonded in a bent 120 degrees geometry to one C(1), one O(1), and one O(4) atom. The C(2)-O(1) bond length is 1.29 Å. The C(2)-O(4) bond length is 1.26 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one N(1), one N(2), and one H(1) atom. The C(3)-N(1) bond length is 1.33 Å. The C(3)-N(2) bond length is 1.35 Å. The C(3)-H(1) bond length is 1.09 Å. In the fourth C site, C(4) is bonded in a bent 120 degrees geometry to one O(5) and one O(6) atom. The C(4)-O(5) bond length is 1.27 Å. The C(4)-O(6) bond length is 1.27 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(1) and one N(2) atom. The C(5)-N(2) bond length is 1.38 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a 3-coordinate geometry to one Yb(1), one C(1), and one C(3) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one C(3), one C(5), and one H(2) atom. The N(2)-H(2) bond length is 1.03 Å. There are four inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(2) is bonded in a single-bond geometry to one N(2) atom. In the third H site, H(3) is bonded in a distorted linear geometry to one O(1) and one O(7) atom. The H(3)-O(1) bond length is 1.64 Å. The H(3)-O(7) bond length is 1.01 Å. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(7) atom. The H(4)-O(7) bond length is 0.98 Å. S(1) is bonded in a tetrahedral geometry to two equivalent O(2) and two equivalent O(3) atoms. Both S(1)-O(2) bond lengths are 1.49 Å. Both S(1)-O(3) bond lengths are 1.50 Å. There are seven inequivalent O sites. In the first O site, O(1) is bonded in a distorted trigonal planar geometry to one Yb(1), one C(2), and one H(3) atom. In the second O site, O(2) is bonded in a distorted L-shaped geometry to one Yb(1) and one S(1) atom. In the third O site, O(3) is bonded in a distorted water-like geometry to one Yb(1) and one S(1) atom. In the fourth O site, O(4) is bonded in a distorted bent 150 degrees geometry to one Yb(1) and one C(2) atom. In the fifth O site, O(5) is bonded in a distorted linear geometry to one Yb(1) and one C(4) atom. In the sixth O site, O(6) is bonded in a bent 150 degrees geometry to one Yb(1) and one C(4) atom. In the seventh O site, O(7) is bonded in a distorted water-like geometry to one Yb(1), one H(3), and one H(4) atom. Linkers: 4 [O]C(=O)c1nc[nH]c1C([O])=O. Metal clusters: 4 [Yb]. The MOF has largest included sphere 2.20 A, density 3.08 g/cm3, surface area 1996.50 m2/g, accessible volume 0.05 cm3/g