Dy2CuC32H12(NO6)4 crystallizes in the triclinic P-1 space group. Dy(1) is bonded in a 6-coordinate geometry to one O(1), one O(10), one O(2), one O(3), one O(8), and one O(9) atom. The Dy(1)-O(1) bond length is 2.30 Å. The Dy(1)-O(10) bond length is 2.44 Å. The Dy(1)-O(2) bond length is 2.30 Å. The Dy(1)-O(3) bond length is 2.41 Å. The Dy(1)-O(8) bond length is 2.27 Å. The Dy(1)-O(9) bond length is 2.51 Å. Cu(1) is bonded in a square co-planar geometry to two equivalent O(4) and two equivalent O(7) atoms. Both Cu(1)-O(4) bond lengths are 1.90 Å. Both Cu(1)-O(7) bond lengths are 1.95 Å. There are sixteen inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(6), and one C(7) atom. The C(1)-C(2) bond length is 1.40 Å. The C(1)-C(6) bond length is 1.38 Å. The C(1)-C(7) bond length is 1.51 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(1), one C(3), and one H(1) atom. The C(2)-C(3) bond length is 1.39 Å. The C(2)-H(1) bond length is 0.93 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(4), and one C(8) atom. The C(3)-C(4) bond length is 1.39 Å. The C(3)-C(8) bond length is 1.50 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(3), one C(5), and one H(2) atom. The C(4)-C(5) bond length is 1.38 Å. The C(4)-H(2) bond length is 0.93 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(4), one C(6), and one N(1) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-N(1) bond length is 1.47 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(1), one C(5), and one H(3) atom. The C(6)-H(3) bond length is 0.93 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(1), and one O(2) atom. The C(7)-O(1) bond length is 1.25 Å. The C(7)-O(2) bond length is 1.25 Å. In the eighth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(3), and one O(4) atom. The C(8)-O(3) bond length is 1.25 Å. The C(8)-O(4) bond length is 1.25 Å. In the ninth C site, C(9) is bonded in a trigonal planar geometry to one C(10), one C(14), and one C(15) atom. The C(9)-C(10) bond length is 1.39 Å. The C(9)-C(14) bond length is 1.39 Å. The C(9)-C(15) bond length is 1.49 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to one C(11), one C(9), and one H(4) atom. The C(10)-C(11) bond length is 1.39 Å. The C(10)-H(4) bond length is 0.93 Å. In the eleventh C site, C(11) is bonded in a trigonal planar geometry to one C(10), one C(12), and one C(16) atom. The C(11)-C(12) bond length is 1.39 Å. The C(11)-C(16) bond length is 1.50 Å. In the twelfth C site, C(12) is bonded in a single-bond geometry to one C(11), one C(13), and one H(5) atom. The C(12)-C(13) bond length is 1.37 Å. The C(12)-H(5) bond length is 0.93 Å. In the thirteenth C site, C(13) is bonded in a trigonal planar geometry to one C(12), one C(14), and one N(2) atom. The C(13)-C(14) bond length is 1.37 Å. The C(13)-N(2) bond length is 1.49 Å. In the fourteenth C site, C(14) is bonded in a distorted single-bond geometry to one C(13), one C(9), and one H(6) atom. The C(14)-H(6) bond length is 0.93 Å. In the fifteenth C site, C(15) is bonded in a distorted bent 120 degrees geometry to one C(9), one O(7), and one O(8) atom. The C(15)-O(7) bond length is 1.26 Å. The C(15)-O(8) bond length is 1.25 Å. In the sixteenth C site, C(16) is bonded in a distorted bent 120 degrees geometry to one C(11), one O(10), and one O(9) atom. The C(16)-O(10) bond length is 1.26 Å. The C(16)-O(9) bond length is 1.26 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one C(5), one O(5), and one O(6) atom. The N(1)-O(5) bond length is 1.23 Å. The N(1)-O(6) bond length is 1.20 Å. In the second N site, N(2) is bonded in a trigonal planar geometry to one C(13), one O(11), and one O(12) atom. The N(2)-O(11) bond length is 1.22 Å. The N(2)-O(12) bond length is 1.20 Å. There are six inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(2) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(4) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(6) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(10) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(12) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(14) atom. There are twelve inequivalent O sites. In the first O site, O(1) is bonded in a linear geometry to one Dy(1) and one C(7) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Dy(1) and one C(7) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one Dy(1) and one C(8) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(8) atom. In the fifth O site, O(5) is bonded in a single-bond geometry to one N(1) atom. In the sixth O site, O(6) is bonded in a single-bond geometry to one N(1) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(15) atom. In the eighth O site, O(8) is bonded in a distorted linear geometry to one Dy(1) and one C(15) atom. In the ninth O site, O(9) is bonded in a distorted L-shaped geometry to one Dy(1) and one C(16) atom. In the tenth O site, O(10) is bonded in a distorted L-shaped geometry to one Dy(1) and one C(16) atom. In the eleventh O site, O(11) is bonded in a single-bond geometry to one N(2) atom. In the twelfth O site, O(12) is bonded in a single-bond geometry to one N(2) atom. Linkers: 4 [O]C(=O)c1cc(C([O])=O)cc([N+](=O)[O-])c1. Metal clusters: 2 [Dy] ,1 [Cu]. The MOF has largest included sphere 4.45 A, density 1.79 g/cm3, surface area 3044.18 m2/g, accessible volume 0.20 cm3/g