FeC6N4H5O crystallizes in the triclinic P-1 space group. There are two inequivalent Fe sites. In the first Fe site, Fe(1) is bonded to four equivalent N(1,2) and two equivalent O(1) atoms to form corner-sharing FeN4O2 octahedra. The corner-sharing octahedral tilt angles are 68°. All Fe(1)-N(1,2) bond lengths are 1.94 Å. Both Fe(1)-O(1) bond lengths are 1.90 Å. In the second Fe site, Fe(2) is bonded to two equivalent N(3), two equivalent N(4), and two equivalent O(1) atoms to form corner-sharing FeN4O2 octahedra. The corner-sharing octahedral tilt angles are 68°. Both Fe(2)-N(3) bond lengths are 2.12 Å. Both Fe(2)-N(4) bond lengths are 2.12 Å. Both Fe(2)-O(1) bond lengths are 2.04 Å. There are three inequivalent C sites. In the first C site, C(1,2) is bonded in a bent 120 degrees geometry to one C(5,6); one N(1,2); and one H(1,2) atom. The C(1,2)-C(5,6) bond length is 1.41 Å. The C(1,2)-N(1,2) bond length is 1.35 Å. The C(1,2)-H(1,2) bond length is 1.08 Å. In the second C site, C(3,4) is bonded in a distorted bent 120 degrees geometry to one C(5,6); one N(3); and one H(3,4) atom. The C(3,4)-C(5,6) bond length is 1.41 Å. The C(3,4)-N(3) bond length is 1.34 Å. The C(3,4)-H(3,4) bond length is 1.09 Å. In the third C site, C(5,6) is bonded in a trigonal planar geometry to one C(1,2); one C(3,4); and one C(5,6) atom. The C(5,6)-C(5,6) bond length is 1.45 Å. There are three inequivalent N sites. In the first N site, N(1,2) is bonded in a distorted trigonal planar geometry to one Fe(1); one C(1,2); and one N(3) atom. The N(1,2)-N(3) bond length is 1.36 Å. In the second N site, N(3) is bonded in a distorted trigonal planar geometry to one Fe(2); one C(3,4); and one N(1,2) atom. In the third N site, N(4) is bonded in a distorted trigonal planar geometry to one Fe(2); one C(3,4); and one N(1,2) atom. The N(4)-C(3,4) bond length is 1.35 Å. The N(4)-N(1,2) bond length is 1.36 Å. There are three inequivalent H sites. In the first H site, H(1,2) is bonded in a single-bond geometry to one C(1,2) atom. In the second H site, H(3,4) is bonded in a single-bond geometry to one C(3,4) atom. In the third H site, H(5) is bonded in a single-bond geometry to one O(1) atom. The H(5)-O(1) bond length is 0.97 Å. O(1) is bonded in a distorted trigonal planar geometry to one Fe(1), one Fe(2), and one H(5) atom. Linkers: 2 C1=N[N]C=C1[C]1C=NN=C1. Metal clusters: 2 [Fe]. The MOF has largest included sphere 5.62 A, density 1.26 g/cm3, surface area 3615.11 m2/g, accessible volume 0.42 cm3/g