Mo3Cu2C4H4(NO5)2 crystallizes in the orthorhombic Pnma space group. There are two inequivalent Mo sites. In the first Mo site, Mo(1) is bonded in a 6-coordinate geometry to one O(1), one O(3), one O(4), one O(5), and two equivalent O(2) atoms. The Mo(1)-O(1) bond length is 2.22 Å. The Mo(1)-O(3) bond length is 2.22 Å. The Mo(1)-O(4) bond length is 1.75 Å. The Mo(1)-O(5) bond length is 1.76 Å. Both Mo(1)-O(2) bond lengths are 1.94 Å. In the second Mo site, Mo(2) is bonded in a 6-coordinate geometry to one O(1), one O(3), one O(6), one O(7), and two equivalent O(2) atoms. The Mo(2)-O(1) bond length is 1.97 Å. The Mo(2)-O(3) bond length is 1.96 Å. The Mo(2)-O(6) bond length is 1.75 Å. The Mo(2)-O(7) bond length is 1.76 Å. There is one shorter (2.20 Å) and one longer (2.21 Å) Mo(2)-O(2) bond length. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a tetrahedral geometry to one N(1), one O(4), and two equivalent O(6) atoms. The Cu(1)-N(1) bond length is 1.97 Å. The Cu(1)-O(4) bond length is 2.00 Å. Both Cu(1)-O(6) bond lengths are 1.99 Å. In the second Cu site, Cu(2) is bonded in a tetrahedral geometry to one N(2), one O(5), and two equivalent O(7) atoms. The Cu(2)-N(2) bond length is 2.04 Å. The Cu(2)-O(5) bond length is 1.95 Å. Both Cu(2)-O(7) bond lengths are 1.96 Å. There are four inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(2), one N(1), and one H(1) atom. The C(1)-C(2) bond length is 1.38 Å. The C(1)-N(1) bond length is 1.35 Å. The C(1)-H(1) bond length is 1.08 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(1), one N(2), and one H(2) atom. The C(2)-N(2) bond length is 1.35 Å. The C(2)-H(2) bond length is 1.09 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(4), one N(2), and one H(3) atom. The C(3)-C(4) bond length is 1.39 Å. The C(3)-N(2) bond length is 1.35 Å. The C(3)-H(3) bond length is 1.09 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(3), one N(1), and one H(4) atom. The C(4)-N(1) bond length is 1.35 Å. The C(4)-H(4) bond length is 1.09 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(4) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Cu(2), one C(2), and one C(3) 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(2) is bonded in a single-bond geometry to one C(2) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(3) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(4) atom. There are seven inequivalent O sites. In the first O site, O(1) is bonded in a 3-coordinate geometry to one Mo(1) and two equivalent Mo(2) atoms. In the second O site, O(2) is bonded in a trigonal non-coplanar geometry to one Mo(1) and two equivalent Mo(2) atoms. In the third O site, O(3) is bonded in a 3-coordinate geometry to one Mo(1) and two equivalent Mo(2) atoms. In the fourth O site, O(4) is bonded in a bent 150 degrees geometry to one Mo(1) and one Cu(1) atom. In the fifth O site, O(5) is bonded in a linear geometry to one Mo(1) and one Cu(2) atom. In the sixth O site, O(6) is bonded in a distorted bent 120 degrees geometry to one Mo(2) and one Cu(1) atom. In the seventh O site, O(7) is bonded in a distorted bent 150 degrees geometry to one Mo(2) and one Cu(2) atom. Linkers: 4 c1cnccn1. Metal clusters: 8 [Cu] ,12 [Mo]. The MOF has largest included sphere 1.55 A, density 3.61 g/cm3, surface area 1809.25 m2/g, accessible volume 0.04 cm3/g