Zn3H20(C2O)24 crystallizes in the tetragonal I-42d space group. There are two inequivalent Zn sites. In the first Zn site, Zn(1) is bonded in a distorted tetrahedral geometry to four equivalent O(1) atoms. All Zn(1)-O(1) bond lengths are 1.96 Å. In the second Zn site, Zn(2) is bonded in a 6-coordinate geometry to two equivalent O(3), two equivalent O(4), and two equivalent O(5) atoms. Both Zn(2)-O(3) bond lengths are 2.03 Å. Both Zn(2)-O(4) bond lengths are 2.40 Å. Both Zn(2)-O(5) bond lengths are 2.00 Å. There are twelve inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(1), and one O(2) atom. The C(1)-C(3) bond length is 1.52 Å. The C(1)-O(1) bond length is 1.25 Å. The C(1)-O(2) bond length is 1.23 Å. In the second C site, C(2) is bonded in a bent 120 degrees geometry to one C(5), one O(3), and one O(4) atom. The C(2)-C(5) bond length is 1.50 Å. The C(2)-O(3) bond length is 1.26 Å. The C(2)-O(4) bond length is 1.23 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(1), one C(4), and one C(8) atom. The C(3)-C(4) bond length is 1.34 Å. The C(3)-C(8) bond length is 1.42 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(3), one C(5), and one H(1) atom. The C(4)-C(5) bond length is 1.41 Å. The C(4)-H(1) bond length is 0.93 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(2), one C(4), and one C(6) atom. The C(5)-C(6) bond length is 1.38 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(5), one C(7), and one H(2) atom. The C(6)-C(7) bond length is 1.39 Å. The C(6)-H(2) bond length is 0.93 Å. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(12), one C(6), and one C(8) atom. The C(7)-C(12) bond length is 1.52 Å. The C(7)-C(8) bond length is 1.38 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one C(3), one C(7), and one H(3) atom. The C(8)-H(3) bond length is 0.93 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one C(10), one O(5), and one O(6) atom. The C(9)-C(10) bond length is 1.49 Å. The C(9)-O(5) bond length is 1.24 Å. The C(9)-O(6) bond length is 1.27 Å. In the tenth C site, C(10) is bonded in a trigonal planar geometry to one C(10), one C(11), and one C(9) atom. The C(10)-C(10) bond length is 1.45 Å. The C(10)-C(11) bond length is 1.36 Å. In the eleventh C site, C(11) is bonded in a distorted single-bond geometry to one C(10), one C(12), and one H(4) atom. The C(11)-C(12) bond length is 1.39 Å. The C(11)-H(4) bond length is 0.93 Å. In the twelfth C site, C(12) is bonded in a trigonal planar geometry to one C(11), one C(12), and one C(7) atom. The C(12)-C(12) bond length is 1.37 Å. There are five inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(4) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(6) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(8) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(11) atom. In the fifth H site, H(5) is bonded in a distorted single-bond geometry to one O(6) atom. The H(5)-O(6) bond length is 0.82 Å. There are six inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Zn(1) and one C(1) atom. In the second O site, O(2) is bonded in a single-bond geometry to one C(1) atom. In the third O site, O(3) is bonded in a water-like geometry to one Zn(2) and one C(2) atom. In the fourth O site, O(4) is bonded in a distorted L-shaped geometry to one Zn(2) and one C(2) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Zn(2) and one C(9) atom. In the sixth O site, O(6) is bonded in a water-like geometry to one C(9) and one H(5) atom. Linkers: 8 [O]C(=O)c1cc(C([O])=O)cc(-c2cc(C(=O)O)c(C(=O)O)cc2-c2cc(C([O])=O)cc(C([O])=O)c2)c1. Metal clusters: 4 O=[C]O[Zn](O[C]=O)(O[C]=O)O[C]=O ,8 O=[C]O[Zn](O[C]O)(O[C]O)O[C]=O. The MOF has largest included sphere 5.64 A, density 1.01 g/cm3, surface area 4179.08 m2/g, accessible volume 0.67 cm3/g