CoCu3H3(CO2)9 crystallizes in the cubic P2_13 space group. Co(1) is bonded in an octahedral geometry to three equivalent O(2) and three equivalent O(5) atoms. All Co(1)-O(2) bond lengths are 2.10 Å. All Co(1)-O(5) bond lengths are 2.07 Å. Cu(1) is bonded in a distorted rectangular see-saw-like geometry to one O(1), one O(6), and two equivalent O(3) atoms. The Cu(1)-O(1) bond length is 1.93 Å. The Cu(1)-O(6) bond length is 1.96 Å. There is one shorter (1.91 Å) and one longer (2.00 Å) Cu(1)-O(3) bond length. There are three inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.44 Å. The C(1)-O(1) bond length is 1.33 Å. The C(1)-O(2) bond length is 1.20 Å. In the second C site, C(2) is bonded in a distorted water-like geometry to one C(1), one C(3), one O(3), and one O(4) atom. The C(2)-C(3) bond length is 1.46 Å. The C(2)-O(3) bond length is 1.35 Å. The C(2)-O(4) bond length is 1.44 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(2), one O(5), and one O(6) atom. The C(3)-O(5) bond length is 1.30 Å. The C(3)-O(6) bond length is 1.30 Å. H(1) is bonded in a single-bond geometry to one O(4) atom. The H(1)-O(4) bond length is 0.82 Å. There are six inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one Cu(1) and one C(1) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Co(1) and one C(1) atom. In the third O site, O(3) is bonded in a distorted trigonal non-coplanar geometry to two equivalent Cu(1) and one C(2) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one C(2) and one H(1) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Co(1) and one C(3) atom. In the sixth O site, O(6) is bonded in a water-like geometry to one Cu(1) and one C(3) atom. Linkers: 12 [O]C(=O)C([O])(O)C([O])=O. Metal clusters: 4 [Co] ,12 [Cu]. The MOF has largest included sphere 11.12 A, density 0.75 g/cm3, surface area 2706.22 m2/g, accessible volume 1.09 cm3/g