PrC20Sb2H24(NO5)4 crystallizes in the orthorhombic Pnn2 space group. Pr(1) is bonded in a 8-coordinate geometry to two equivalent O(10), two equivalent O(2), two equivalent O(8), and two equivalent O(9) atoms. Both Pr(1)-O(10) bond lengths are 2.49 Å. Both Pr(1)-O(2) bond lengths are 2.48 Å. Both Pr(1)-O(8) bond lengths are 2.46 Å. Both Pr(1)-O(9) bond lengths are 2.59 Å. There are ten inequivalent C sites. In the first C site, C(1) is bonded in a 3-coordinate geometry to one N(1), one H(1), and one H(2) atom. The C(1)-N(1) bond length is 1.48 Å. The C(1)-H(1) bond length is 0.97 Å. The C(1)-H(2) bond length is 0.97 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(2)-O(1) bond length is 1.25 Å. The C(2)-O(2) bond length is 1.25 Å. In the third C site, C(3) is bonded in a 3-coordinate geometry to one N(1) and two equivalent H(3,4) atoms. The C(3)-N(1) bond length is 1.50 Å. Both C(3)-H(3,4) 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 1.30 Å. The C(4)-O(4) bond length is 1.22 Å. In the fifth C site, C(5) is bonded in a 3-coordinate geometry to one N(1) and two equivalent H(5,6) atoms. The C(5)-N(1) bond length is 1.49 Å. Both C(5)-H(5,6) bond lengths are 0.97 Å. In the sixth C site, C(6) is bonded in a 3-coordinate geometry to one N(2), one H(7), and one H(8) atom. The C(6)-N(2) bond length is 1.49 Å. The C(6)-H(7) bond length is 0.97 Å. The C(6)-H(8) bond length is 0.97 Å. In the seventh C site, C(7) is bonded in a 3-coordinate geometry to one N(2) and two equivalent H(9,10) atoms. The C(7)-N(2) bond length is 1.49 Å. Both C(7)-H(9,10) bond lengths are 0.97 Å. In the eighth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one O(5) and one O(6) atom. The C(8)-O(5) bond length is 1.28 Å. The C(8)-O(6) bond length is 1.23 Å. In the ninth C site, C(9) is bonded in a 3-coordinate geometry to one N(2) and two equivalent H(11,12) atoms. The C(9)-N(2) bond length is 1.49 Å. Both C(9)-H(11,12) bond lengths are 0.97 Å. In the tenth C site, C(10) is bonded in a distorted bent 120 degrees geometry to one O(7) and one O(8) atom. The C(10)-O(7) bond length is 1.26 Å. The C(10)-O(8) bond length is 1.24 Å. Sb(1) is bonded in a distorted pentagonal pyramidal geometry to one N(1), one N(2), one O(1), one O(3), one O(5), and one O(7) atom. The Sb(1)-N(1) bond length is 2.32 Å. The Sb(1)-N(2) bond length is 2.31 Å. The Sb(1)-O(1) bond length is 2.56 Å. The Sb(1)-O(3) bond length is 2.12 Å. The Sb(1)-O(5) bond length is 2.21 Å. The Sb(1)-O(7) bond length is 2.44 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded to one C(1), one C(3), one C(5), and one Sb(1) atom to form distorted corner-sharing NSbC3 tetrahedra. In the second N site, N(2) is bonded to one C(6), one C(7), one C(9), and one Sb(1) atom to form distorted corner-sharing NSbC3 tetrahedra. There are eight inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(1) atom. In the third H site, H(3,4) is bonded in a single-bond geometry to one C(3) atom. In the fourth H site, H(5,6) is bonded in a single-bond geometry to one C(5) atom. In the fifth H site, H(7) is bonded in a single-bond geometry to one C(6) atom. In the sixth H site, H(8) is bonded in a single-bond geometry to one C(6) atom. In the seventh H site, H(9,10) is bonded in a single-bond geometry to one C(7) atom. In the eighth H site, H(11,12) is bonded in a single-bond geometry to one C(9) atom. There are ten inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one C(2) and one Sb(1) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one Pr(1) and one C(2) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one C(4) and one Sb(1) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one C(4) atom. In the fifth O site, O(5) is bonded in a distorted bent 120 degrees geometry to one C(8) and one Sb(1) atom. In the sixth O site, O(6) is bonded in a single-bond geometry to one C(8) atom. In the seventh O site, O(7) is bonded in a distorted single-bond geometry to one C(10) and one Sb(1) atom. In the eighth O site, O(8) is bonded in a distorted bent 150 degrees geometry to one Pr(1) and one C(10) atom. In the ninth O site, O(9) is bonded in a 2-coordinate geometry to one Pr(1) and one O(10) atom. The O(9)-O(10) bond length is 0.93 Å. In the tenth O site, O(10) is bonded in an L-shaped geometry to one Pr(1) and one O(9) atom. Linkers: 2 [O]C(=O)CN1CC[N@]2(CC(=O)[O])CC(=O)O[Sb]2OC(=O)C1 ,2 [O]C(=O)CN1CC[N@@]2(CC(=O)[O])CC(=O)O[Sb]2OC(=O)C1. Metal clusters: 2 [O]O[Pr]([O])([O])(O[O])(O[C]=O)O[C]=O. RCSR code: dia. The MOF has largest included sphere 5.11 A, density 1.90 g/cm3, surface area 2996.51 m2/g, accessible volume 0.17 cm3/g