SmC20Sb2H24(NO4)4 crystallizes in the monoclinic Pc space group. Sm(1) is bonded in a distorted rectangular see-saw-like geometry to one O(10), one O(16), one O(4), and one O(6) atom. The Sm(1)-O(10) bond length is 2.36 Å. The Sm(1)-O(16) bond length is 2.38 Å. The Sm(1)-O(4) bond length is 2.36 Å. The Sm(1)-O(6) bond length is 2.36 Å. There are twenty inequivalent C sites. In the first C site, C(1) is bonded in a 3-coordinate geometry to one N(1) and two equivalent H(1,2) atoms. The C(1)-N(1) bond length is 1.49 Å. Both C(1)-H(1,2) bond lengths are 0.99 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 1.31 Å. The C(2)-O(2) bond length is 1.21 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 1.49 Å. Both C(3)-H(3,4) bond lengths are 0.99 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 1.24 Å. In the fifth C site, C(5) is bonded in a 4-coordinate geometry to one C(6), one N(1), one H(5), and one H(6) atom. The C(5)-C(6) bond length is 1.48 Å. The C(5)-N(1) bond length is 1.49 Å. The C(5)-H(5) bond length is 0.99 Å. The C(5)-H(6) bond length is 0.99 Å. In the sixth C site, C(6) is bonded in a 4-coordinate geometry to one C(5); one N(2); and two equivalent H(7,8) atoms. The C(6)-N(2) bond length is 1.51 Å. Both C(6)-H(7,8) bond lengths are 0.99 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 1.48 Å. Both C(7)-H(9,10) bond lengths are 0.99 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 1.26 Å. The C(8)-O(6) bond length is 1.26 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 0.99 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 1.31 Å. The C(10)-O(8) bond length is 1.22 Å. In the eleventh C site, C(11) is bonded in a 3-coordinate geometry to one N(3) and two equivalent H(13,14) atoms. The C(11)-N(3) bond length is 1.48 Å. Both C(11)-H(13,14) bond lengths are 0.99 Å. In the twelfth C site, C(12) is bonded in a distorted bent 120 degrees geometry to one O(10) and one O(9) atom. The C(12)-O(10) bond length is 1.26 Å. The C(12)-O(9) bond length is 1.25 Å. In the thirteenth C site, C(13) is bonded in a 3-coordinate geometry to one N(3) and two equivalent H(15,16) atoms. The C(13)-N(3) bond length is 1.50 Å. Both C(13)-H(15,16) bond lengths are 0.99 Å. In the fourteenth C site, C(14) is bonded in a distorted bent 120 degrees geometry to one O(11) and one O(12) atom. The C(14)-O(11) bond length is 1.28 Å. The C(14)-O(12) bond length is 1.23 Å. In the fifteenth C site, C(15) is bonded in a 3-coordinate geometry to one N(3) and two equivalent H(17,18) atoms. The C(15)-N(3) bond length is 1.50 Å. Both C(15)-H(17,18) bond lengths are 0.99 Å. In the sixteenth C site, C(16) is bonded in a 3-coordinate geometry to one N(4) and two equivalent H(19,20,23,24) atoms. The C(16)-N(4) bond length is 1.48 Å. Both C(16)-H(19,20,23,24) bond lengths are 0.99 Å. In the seventeenth C site, C(17) is bonded in a 3-coordinate geometry to one N(4) and two equivalent H(21,22) atoms. The C(17)-N(4) bond length is 1.50 Å. Both C(17)-H(21,22) bond lengths are 0.99 Å. In the eighteenth C site, C(18) is bonded in a distorted bent 120 degrees geometry to one O(13) and one O(14) atom. The C(18)-O(13) bond length is 1.30 Å. The C(18)-O(14) bond length is 1.21 Å. In the nineteenth C site, C(19) is bonded in a 3-coordinate geometry to one N(4) and two equivalent H(19,20,23,24) atoms. The C(19)-N(4) bond length is 1.48 Å. Both C(19)-H(19,20,23,24) bond lengths are 0.99 Å. In the twentieth C site, C(20) is bonded in a distorted bent 120 degrees geometry to one O(15) and one O(16) atom. The C(20)-O(15) bond length is 1.28 Å. The C(20)-O(16) bond length is 1.25 Å. There are two inequivalent Sb sites. In the first Sb site, 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 2.31 Å. The Sb(1)-N(2) bond length is 2.32 Å. The Sb(1)-O(1) bond length is 2.21 Å. The Sb(1)-O(3) bond length is 2.51 Å. The Sb(1)-O(5) bond length is 2.52 Å. The Sb(1)-O(7) bond length is 2.12 Å. In the second Sb site, Sb(2) is bonded in a distorted pentagonal pyramidal geometry to one N(3), one N(4), one O(11), one O(13), one O(15), and one O(9) atom. The Sb(2)-N(3) bond length is 2.31 Å. The Sb(2)-N(4) bond length is 2.32 Å. The Sb(2)-O(11) bond length is 2.13 Å. The Sb(2)-O(13) bond length is 2.22 Å. The Sb(2)-O(15) bond length is 2.47 Å. The Sb(2)-O(9) bond length is 2.52 Å. There are four 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. In the third N site, N(3) is bonded to one C(11), one C(13), one C(15), and one Sb(2) atom to form distorted corner-sharing NSbC3 tetrahedra. In the fourth N site, N(4) is bonded to one C(16), one C(17), one C(19), and one Sb(2) atom to form distorted corner-sharing NSbC3 tetrahedra. There are twelve inequivalent H sites. In the first H site, H(1,2) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(3,4) is bonded in a single-bond geometry to one C(3) atom. In the third H site, H(5) is bonded in a single-bond geometry to one C(5) atom. In the fourth H site, H(6) is bonded in a single-bond geometry to one C(5) atom. In the fifth H site, H(7,8) is bonded in a single-bond geometry to one C(6) atom. In the sixth H site, H(9,10) is bonded in a single-bond geometry to one C(7) atom. In the seventh H site, H(11,12) is bonded in a single-bond geometry to one C(9) atom. In the eighth H site, H(13,14) is bonded in a single-bond geometry to one C(11) atom. In the ninth H site, H(15,16) is bonded in a single-bond geometry to one C(13) atom. In the tenth H site, H(17,18) is bonded in a single-bond geometry to one C(15) atom. In the eleventh H site, H(19,20,23,24) is bonded in a single-bond geometry to one C(16) atom. In the twelfth H site, H(21,22) is bonded in a single-bond geometry to one C(17) atom. There are sixteen inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one C(2) and one Sb(1) atom. In the second O site, O(2) is bonded in a single-bond geometry to one C(2) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one C(4) and one Sb(1) atom. In the fourth O site, O(4) is bonded in a distorted bent 150 degrees geometry to one Sm(1) and one C(4) atom. In the fifth O site, O(5) is bonded in a distorted single-bond geometry to one C(8) and one Sb(1) atom. In the sixth O site, O(6) is bonded in a distorted bent 150 degrees geometry to one Sm(1) and one C(8) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one C(10) and one Sb(1) atom. In the eighth O site, O(8) is bonded in a single-bond geometry to one C(10) atom. In the ninth O site, O(9) is bonded in a distorted single-bond geometry to one C(12) and one Sb(2) atom. In the tenth O site, O(10) is bonded in a distorted bent 150 degrees geometry to one Sm(1) and one C(12) atom. In the eleventh O site, O(11) is bonded in a bent 120 degrees geometry to one C(14) and one Sb(2) atom. In the twelfth O site, O(12) is bonded in a single-bond geometry to one C(14) atom. In the thirteenth O site, O(13) is bonded in a distorted bent 120 degrees geometry to one C(18) and one Sb(2) atom. In the fourteenth O site, O(14) is bonded in a single-bond geometry to one C(18) atom. In the fifteenth O site, O(15) is bonded in a distorted single-bond geometry to one C(20) and one Sb(2) atom. In the sixteenth O site, O(16) is bonded in a distorted bent 150 degrees geometry to one Sm(1) and one C(20) 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=[C]O[Sm](O[C]=O)(O[C]=O)O[C]=O. RCSR code: dia. The MOF has largest included sphere 5.20 A, density 1.85 g/cm3, surface area 2863.17 m2/g, accessible volume 0.24 cm3/g