MoCuC2NH2O4 crystallizes in the monoclinic P2_1/c space group. Mo(1) is bonded to one O(1), one O(2), one O(3), and one O(4) atom to form MoO4 tetrahedra that share corners with four equivalent Cu(1)NO4 square pyramids. The Mo(1)-O(1) bond length is 1.75 Å. The Mo(1)-O(2) bond length is 1.81 Å. The Mo(1)-O(3) bond length is 1.80 Å. The Mo(1)-O(4) bond length is 1.78 Å. Cu(1) is bonded to one N(1), one O(1), one O(2), one O(3), and one O(4) atom to form CuNO4 square pyramids that share corners with four equivalent Mo(1)O4 tetrahedra. The Cu(1)-N(1) bond length is 1.98 Å. The Cu(1)-O(1) bond length is 2.29 Å. The Cu(1)-O(2) bond length is 1.94 Å. The Cu(1)-O(3) bond length is 1.96 Å. The Cu(1)-O(4) bond length is 1.99 Å. There are two inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one N(1), and one H(1) atom. The C(1)-C(2) 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 trigonal planar geometry to one C(1), one N(1), and one H(2) atom. The C(2)-N(1) bond length is 1.34 Å. The C(2)-H(2) 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 two 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. There are four inequivalent O sites. In the first O site, O(2) is bonded in a bent 150 degrees geometry to one Mo(1) and one Cu(1) atom. In the second O site, O(3) is bonded in a bent 120 degrees geometry to one Mo(1) and one Cu(1) atom. In the third O site, O(4) is bonded in a bent 120 degrees geometry to one Mo(1) and one Cu(1) atom. In the fourth O site, O(1) is bonded in a distorted linear geometry to one Mo(1) and one Cu(1) atom. Linkers: 2 c1cnccn1. Metal clusters: 4 [Cu] ,4 [Mo]. The MOF has largest included sphere 1.41 A, density 3.52 g/cm3, surface area 1654.44 m2/g, accessible volume 0.02 cm3/g