Fe3P3H2(CO5)4 crystallizes in the triclinic P-1 space group. There are three inequivalent Fe sites. In the first Fe site, Fe(1) is bonded to one O(11), one O(13), one O(15), one O(2), one O(5), and one O(6) atom to form FeO6 octahedra that share  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(3)O4 tetrahedra, and corners with two equivalent P(2)O4 tetrahedra. The Fe(1)-O(11) bond length is 1.99 Å. The Fe(1)-O(13) bond length is 2.09 Å. The Fe(1)-O(15) bond length is 2.07 Å. The Fe(1)-O(2) bond length is 1.93 Å. The Fe(1)-O(5) bond length is 1.95 Å. The Fe(1)-O(6) bond length is 1.98 Å. In the second Fe site, Fe(2) is bonded to one O(1), one O(10), one O(17), one O(19), one O(7), and one O(9) atom to form FeO6 octahedra that share  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(2)O4 tetrahedra, and corners with two equivalent P(3)O4 tetrahedra. The Fe(2)-O(1) bond length is 1.95 Å. The Fe(2)-O(10) bond length is 1.96 Å. The Fe(2)-O(17) bond length is 2.07 Å. The Fe(2)-O(19) bond length is 2.05 Å. The Fe(2)-O(7) bond length is 2.07 Å. The Fe(2)-O(9) bond length is 1.94 Å. In the third Fe site, Fe(3) is bonded in a 5-coordinate geometry to one O(14), one O(16), one O(3), one O(4), and one O(7) atom. The Fe(3)-O(14) bond length is 2.10 Å. The Fe(3)-O(16) bond length is 2.20 Å. The Fe(3)-O(3) bond length is 2.02 Å. The Fe(3)-O(4) bond length is 2.02 Å. The Fe(3)-O(7) bond length is 2.10 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 O(13) and one O(14) atom. The C(1)-O(13) bond length is 1.25 Å. The C(1)-O(14) bond length is 1.25 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one O(15) and one O(16) atom. The C(2)-O(15) bond length is 1.26 Å. The C(2)-O(16) bond length is 1.24 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one O(17) and one O(18) atom. The C(3)-O(17) bond length is 1.26 Å. The C(3)-O(18) bond length is 1.23 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one O(19) and one O(20) atom. The C(4)-O(19) bond length is 1.27 Å. The C(4)-O(20) bond length is 1.23 Å. There are three inequivalent P sites. In the first P site, P(1) is bonded to one O(1), one O(2), one O(3), and one O(4) atom to form PO4 tetrahedra that share  a cornercorner with one Fe(1)O6 octahedra and  a cornercorner with one Fe(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 47-49°. The P(1)-O(1) bond length is 1.54 Å. The P(1)-O(2) bond length is 1.55 Å. The P(1)-O(3) bond length is 1.52 Å. The P(1)-O(4) bond length is 1.53 Å. In the second P site, P(2) is bonded to one O(5), one O(6), one O(7), and one O(8) atom to form PO4 tetrahedra that share  a cornercorner with one Fe(2)O6 octahedra and corners with two equivalent Fe(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 43-46°. The P(2)-O(5) bond length is 1.51 Å. The P(2)-O(6) bond length is 1.52 Å. The P(2)-O(7) bond length is 1.54 Å. The P(2)-O(8) bond length is 1.57 Å. In the third P site, P(3) is bonded to one O(10), one O(11), one O(12), and one O(9) atom to form PO4 tetrahedra that share  a cornercorner with one Fe(1)O6 octahedra and corners with two equivalent Fe(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 35-45°. The P(3)-O(10) bond length is 1.53 Å. The P(3)-O(11) bond length is 1.53 Å. The P(3)-O(12) bond length is 1.58 Å. The P(3)-O(9) bond length is 1.51 Å. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(8) atom. The H(1)-O(8) bond length is 0.90 Å. In the second H site, H(2) is bonded in a distorted single-bond geometry to one O(12) and one O(18) atom. The H(2)-O(12) bond length is 0.97 Å. The H(2)-O(18) bond length is 1.68 Å. There are twenty inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Fe(2) and one P(1) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Fe(1) and one P(1) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one Fe(3) and one P(1) atom. In the fourth O site, O(4) is bonded in a 2-coordinate geometry to one Fe(3) and one P(1) atom. In the fifth O site, O(5) is bonded in a distorted bent 150 degrees geometry to one Fe(1) and one P(2) atom. In the sixth O site, O(6) is bonded in a distorted bent 150 degrees geometry to one Fe(1) and one P(2) atom. In the seventh O site, O(7) is bonded in a distorted trigonal planar geometry to one Fe(2), one Fe(3), and one P(2) atom. In the eighth O site, O(8) is bonded in a bent 120 degrees geometry to one P(2) and one H(1) atom. In the ninth O site, O(9) is bonded in a bent 150 degrees geometry to one Fe(2) and one P(3) atom. In the tenth O site, O(10) is bonded in a distorted bent 150 degrees geometry to one Fe(2) and one P(3) atom. In the eleventh O site, O(11) is bonded in a distorted bent 150 degrees geometry to one Fe(1) and one P(3) atom. In the twelfth O site, O(12) is bonded in a bent 120 degrees geometry to one P(3) and one H(2) atom. In the thirteenth O site, O(13) is bonded in a bent 120 degrees geometry to one Fe(1) and one C(1) atom. In the fourteenth O site, O(14) is bonded in a bent 120 degrees geometry to one Fe(3) and one C(1) atom. In the fifteenth O site, O(15) is bonded in a bent 120 degrees geometry to one Fe(1) and one C(2) atom. In the sixteenth O site, O(16) is bonded in a water-like geometry to one Fe(3) and one C(2) atom. In the seventeenth O site, O(17) is bonded in a bent 120 degrees geometry to one Fe(2) and one C(3) atom. In the eighteenth O site, O(18) is bonded in a distorted bent 120 degrees geometry to one C(3) and one H(2) atom. In the nineteenth O site, O(19) is bonded in a bent 120 degrees geometry to one Fe(2) and one C(4) atom. In the twentieth O site, O(20) is bonded in a single-bond geometry to one C(4) atom. Linkers: 4 [O]C(=O)C([O])=O. Metal clusters: 6 [Fe]. The MOF has largest included sphere 3.96 A, density 2.08 g/cm3, surface area 2422.46 m2/g, accessible volume 0.16 cm3/g