Mo2C2H3(NO2)3 crystallizes in the orthorhombic Pca2_1 space group. There are two inequivalent Mo sites. In the first Mo site, Mo(1) is bonded in a 6-coordinate geometry to one N(1); one O(3); one O(5); one O(6); and two equivalent O(1,2) atoms. The Mo(1)-N(1) bond length is 2.38 Å. The Mo(1)-O(3) bond length is 1.71 Å. The Mo(1)-O(5) bond length is 1.94 Å. The Mo(1)-O(6) bond length is 1.90 Å. There is one shorter (1.76 Å) and one longer (2.19 Å) Mo(1)-O(1,2) bond length. In the second Mo site, Mo(2) is bonded in a 6-coordinate geometry to one N(2); one O(4); one O(5); one O(6); and two equivalent O(1,2) atoms. The Mo(2)-N(2) bond length is 2.38 Å. The Mo(2)-O(4) bond length is 1.71 Å. The Mo(2)-O(5) bond length is 1.94 Å. The Mo(2)-O(6) bond length is 1.90 Å. There is one shorter (1.76 Å) and one longer (2.19 Å) Mo(2)-O(1,2) bond length. There are two inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one N(1); one N(3); and one H(1,2) atom. The C(1)-N(1) bond length is 1.32 Å. The C(1)-N(3) bond length is 1.36 Å. The C(1)-H(1,2) bond length is 1.09 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one N(2); one N(3); and one H(1,2) atom. The C(2)-N(2) bond length is 1.32 Å. The C(2)-N(3) bond length is 1.36 Å. The C(2)-H(1,2) bond length is 1.09 Å. There are three inequivalent N sites. In the first N site, N(3) is bonded in a trigonal planar geometry to one C(1), one C(2), and one H(3) atom. The N(3)-H(3) bond length is 1.04 Å. In the second N site, N(1) is bonded in a distorted single-bond geometry to one Mo(1), one C(1), and one N(2) atom. The N(1)-N(2) bond length is 1.37 Å. In the third N site, N(2) is bonded in a distorted single-bond geometry to one Mo(2), one C(2), and one N(1) atom. There are two inequivalent H sites. In the first H site, H(1,2) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(3) is bonded in a distorted single-bond geometry to one N(3) and one O(5) atom. The H(3)-O(5) bond length is 1.72 Å. There are five inequivalent O sites. In the first O site, O(1,2) is bonded in a distorted linear geometry to two equivalent Mo(1) atoms. In the second O site, O(6) is bonded in a linear geometry to one Mo(1) and one Mo(2) atom. In the third O site, O(3) is bonded in a single-bond geometry to one Mo(1) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one Mo(2) atom. In the fifth O site, O(5) is bonded in a 3-coordinate geometry to one Mo(1), one Mo(2), and one H(3) atom. Linkers: 4 c1nnc[nH]1. Metal clusters: 8 [Mo]. The MOF has largest included sphere 1.63 A, density 3.22 g/cm3, surface area 1932.41 m2/g, accessible volume 0.03 cm3/g