DyCuC16N5H10O9 crystallizes in the triclinic P-1 space group. Dy(1) is bonded in a 9-coordinate geometry to one O(2), one O(4), one O(5), one O(6), one O(7), one O(8), one O(9), and two equivalent O(3) atoms. The Dy(1)-O(2) bond length is 2.28 Å. The Dy(1)-O(4) bond length is 2.49 Å. The Dy(1)-O(5) bond length is 2.48 Å. The Dy(1)-O(6) bond length is 2.40 Å. The Dy(1)-O(7) bond length is 2.40 Å. The Dy(1)-O(8) bond length is 2.44 Å. The Dy(1)-O(9) bond length is 2.41 Å. There is one shorter (2.31 Å) and one longer (2.81 Å) Dy(1)-O(3) bond length. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in an octahedral geometry to two equivalent N(3), two equivalent N(5), and two equivalent O(4) atoms. Both Cu(1)-N(3) bond lengths are 1.93 Å. Both Cu(1)-N(5) bond lengths are 2.06 Å. Both Cu(1)-O(4) bond lengths are 2.42 Å. In the second Cu site, Cu(2) is bonded in a distorted octahedral geometry to two equivalent N(1), two equivalent N(4), and two equivalent O(1) atoms. Both Cu(2)-N(1) bond lengths are 1.94 Å. Both Cu(2)-N(4) bond lengths are 2.05 Å. Both Cu(2)-O(1) bond lengths are 2.54 Å. There are sixteen inequivalent C sites. In the first C site, C(1) is bonded in a distorted single-bond geometry to one C(2), one C(3), and one N(1) atom. The C(1)-C(2) bond length is 1.40 Å. The C(1)-C(3) bond length is 1.51 Å. The C(1)-N(1) bond length is 1.36 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(1) and one N(3) atom. The C(2)-N(3) bond length is 1.36 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(1), and one O(2) atom. The C(3)-O(1) bond length is 1.27 Å. The C(3)-O(2) bond length is 1.27 Å. In the fourth C site, C(4) is bonded in a bent 120 degrees geometry to one O(3) and one O(4) atom. The C(4)-O(3) bond length is 1.26 Å. The C(4)-O(4) bond length is 1.28 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(6), one N(4), and one H(1) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-N(4) bond length is 1.35 Å. The C(5)-H(1) bond length is 1.09 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(5), one C(7), and one H(2) atom. The C(6)-C(7) bond length is 1.40 Å. The C(6)-H(2) bond length is 1.09 Å. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(10), one C(6), and one C(8) atom. The C(7)-C(10) bond length is 1.50 Å. The C(7)-C(8) bond length is 1.40 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one C(7) and one H(3) atom. The C(8)-H(3) bond length is 1.09 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one N(4) and one H(4) atom. The C(9)-N(4) bond length is 1.35 Å. The C(9)-H(4) bond length is 1.09 Å. In the tenth C site, C(10) is bonded in a bent 120 degrees geometry to one C(7), one O(5), and one O(6) atom. The C(10)-O(5) bond length is 1.28 Å. The C(10)-O(6) bond length is 1.27 Å. In the eleventh C site, C(11) is bonded in a distorted bent 120 degrees geometry to one C(12), one N(5), and one H(5) atom. The C(11)-C(12) bond length is 1.39 Å. The C(11)-N(5) bond length is 1.35 Å. The C(11)-H(5) bond length is 1.09 Å. In the twelfth C site, C(12) is bonded in a distorted trigonal planar geometry to one C(11), one C(13), and one H(6) atom. The C(12)-C(13) bond length is 1.40 Å. The C(12)-H(6) bond length is 1.09 Å. In the thirteenth C site, C(13) is bonded in a trigonal planar geometry to one C(12), one C(14), and one C(16) atom. The C(13)-C(14) bond length is 1.40 Å. The C(13)-C(16) bond length is 1.50 Å. In the fourteenth C site, C(14) is bonded in a single-bond geometry to one C(13), one C(15), and one H(7) atom. The C(14)-C(15) bond length is 1.39 Å. The C(14)-H(7) bond length is 1.09 Å. In the fifteenth C site, C(15) is bonded in a distorted trigonal planar geometry to one C(14), one N(5), and one H(8) atom. The C(15)-N(5) bond length is 1.34 Å. The C(15)-H(8) bond length is 1.09 Å. In the sixteenth C site, C(16) is bonded in a distorted bent 120 degrees geometry to one C(13), one O(7), and one O(8) atom. The C(16)-O(7) bond length is 1.28 Å. The C(16)-O(8) bond length is 1.27 Å. There are five inequivalent N sites. In the first N site, N(1) is bonded in a distorted trigonal planar geometry to one Cu(2), one C(1), and one N(2) atom. The N(1)-N(2) bond length is 1.33 Å. In the second N site, N(2) is bonded in a distorted water-like geometry to one N(1) and one N(3) atom. The N(2)-N(3) bond length is 1.32 Å. In the third N site, N(3) is bonded in a distorted trigonal planar geometry to one Cu(1), one C(2), and one N(2) atom. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one Cu(2), one C(5), and one C(9) atom. In the fifth N site, N(5) is bonded in a trigonal planar geometry to one Cu(1), one C(11), and one C(15) atom. There are ten inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(5) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(6) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(8) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(9) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(11) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(12) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(14) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(15) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one O(9) atom. The H(9)-O(9) bond length is 0.99 Å. In the tenth H site, H(10) is bonded in a single-bond geometry to one O(9) atom. The H(10)-O(9) bond length is 1.00 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one Cu(2) and one C(3) atom. In the second O site, O(2) is bonded in a bent 150 degrees geometry to one Dy(1) and one C(3) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to two equivalent Dy(1) and one C(4) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one Dy(1), one Cu(1), and one C(4) atom. In the fifth O site, O(5) is bonded in a distorted single-bond geometry to one Dy(1) and one C(10) atom. In the sixth O site, O(6) is bonded in a distorted L-shaped geometry to one Dy(1) and one C(10) atom. In the seventh O site, O(7) is bonded in a distorted L-shaped geometry to one Dy(1) and one C(16) atom. In the eighth O site, O(8) is bonded in a distorted L-shaped geometry to one Dy(1) and one C(16) atom. In the ninth O site, O(9) is bonded in a distorted water-like geometry to one Dy(1), one H(10), and one H(9) atom. Linkers: 2 [O]C(=O)[C]1N=NN=C1C([O])=O ,4 [O]C(=O)c1ccncc1. Metal clusters: 2 [Dy] ,2 [Cu]. The MOF has largest included sphere 3.95 A, density 1.97 g/cm3, surface area 2892.79 m2/g, accessible volume 0.19 cm3/g