Ho2Cu3C24H30(NO4)6 crystallizes in the trigonal P-3c1 space group. Ho(1) is bonded in a 9-coordinate geometry to three equivalent O(1), three equivalent O(2), and three equivalent O(4) atoms. All Ho(1)-O(1) bond lengths are 2.35 Å. All Ho(1)-O(2) bond lengths are 2.70 Å. All Ho(1)-O(4) bond lengths are 2.29 Å. Cu(1) is bonded in a distorted octahedral geometry to two equivalent N(1), two equivalent O(1), and two equivalent O(3) atoms. Both Cu(1)-N(1) bond lengths are 2.01 Å. Both Cu(1)-O(1) bond lengths are 2.43 Å. Both Cu(1)-O(3) 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 O(1) and one O(2) atom. The C(1)-O(1) bond length is 1.26 Å. The C(1)-O(2) bond length is 1.25 Å. In the second C site, C(2) is bonded in a 3-coordinate geometry to one N(1) and two equivalent H(2,3) atoms. The C(2)-N(1) bond length is 1.49 Å. Both C(2)-H(2,3) bond lengths are 0.97 Å. In the third C site, C(3) is bonded in a 3-coordinate geometry to one N(1) and two equivalent H(4,5) atoms. The C(3)-N(1) bond length is 1.48 Å. Both C(3)-H(4,5) bond lengths are 0.97 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one O(3) and one O(4) atom. The C(4)-O(3) bond length is 1.27 Å. The C(4)-O(4) bond length is 1.26 Å. N(1) is bonded to one Cu(1), one C(2), one C(3), and one H(1) atom to form distorted corner-sharing NCuHC2 tetrahedra. The N(1)-H(1) bond length is 0.91 Å. There are three inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one N(1) atom. In the second H site, H(2,3) is bonded in a single-bond geometry to one C(2) atom. In the third H site, H(4,5) is bonded in a single-bond geometry to one C(3) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one Ho(1), one Cu(1), and one C(1) atom. In the second O site, O(2) is bonded in a single-bond geometry to one Ho(1) and one C(1) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(4) atom. In the fourth O site, O(4) is bonded in a bent 150 degrees geometry to one Ho(1) and one C(4) atom. Linkers: 12 [O]C(=O)CNCC([O])=O. Metal clusters: 4 [Ho] ,6 [Cu]. The MOF has largest included sphere 7.17 A, density 1.95 g/cm3, surface area 2672.68 m2/g, accessible volume 0.21 cm3/g