Pr2Cu3C24(NO4)6 crystallizes in the trigonal P-3c1 space group. Pr(1) is bonded in a 9-coordinate geometry to three equivalent O(1), three equivalent O(2), and three equivalent O(3) atoms. All Pr(1)-O(1) bond lengths are 2.69 Å. All Pr(1)-O(2) bond lengths are 2.42 Å. All Pr(1)-O(3) bond lengths are 2.40 Å. Cu(1) is bonded in a distorted octahedral geometry to two equivalent N(1), two equivalent O(2), and two equivalent O(4) atoms. Both Cu(1)-N(1) bond lengths are 2.02 Å. Both Cu(1)-O(2) bond lengths are 2.43 Å. Both Cu(1)-O(4) bond lengths are 1.95 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 O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.51 Å. The C(1)-O(1) bond length is 1.26 Å. The C(1)-O(2) bond length is 1.29 Å. In the second C site, C(2) is bonded in a bent 120 degrees geometry to one C(1) and one N(1) atom. The C(2)-N(1) bond length is 1.44 Å. In the third C site, C(3) is bonded in a bent 120 degrees geometry to one C(4) and one N(1) atom. The C(3)-C(4) bond length is 1.43 Å. The C(3)-N(1) bond length is 1.51 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(3), and one O(4) atom. The C(4)-O(3) bond length is 1.25 Å. The C(4)-O(4) bond length is 1.34 Å. N(1) is bonded in a trigonal non-coplanar geometry to one Cu(1), one C(2), and one C(3) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a single-bond geometry to one Pr(1) and one C(1) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one Pr(1), one Cu(1), and one C(1) atom. In the third O site, O(3) is bonded in a bent 150 degrees geometry to one Pr(1) and one C(4) atom. In the fourth O site, O(4) is bonded in a water-like geometry to one Cu(1) and one C(4) atom. Linkers: 12 [O]C(=O)[C][N][C]C([O])=O. Metal clusters: 4 [Pr] ,6 [Cu]. The MOF has largest included sphere 7.71 A, density 1.77 g/cm3, surface area 3024.56 m2/g, accessible volume 0.23 cm3/g