GdCuC16N5H10O9 crystallizes in the triclinic P-1 space group. Gd(1) is bonded in a 9-coordinate geometry to one O(1), one O(2), one O(3), one O(4), one O(5), one O(8), one O(9), and two equivalent O(7) atoms. The Gd(1)-O(1) bond length is 2.50 Å. The Gd(1)-O(2) bond length is 2.45 Å. The Gd(1)-O(3) bond length is 2.41 Å. The Gd(1)-O(4) bond length is 2.49 Å. The Gd(1)-O(5) bond length is 2.32 Å. The Gd(1)-O(8) bond length is 2.51 Å. The Gd(1)-O(9) bond length is 2.46 Å. There is one shorter (2.35 Å) and one longer (2.70 Å) Gd(1)-O(7) bond length. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a distorted octahedral geometry to two equivalent N(3), two equivalent N(5), and two equivalent O(8) atoms. Both Cu(1)-N(3) bond lengths are 1.93 Å. Both Cu(1)-N(5) bond lengths are 2.04 Å. Both Cu(1)-O(8) bond lengths are 2.50 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(6) atoms. Both Cu(2)-N(1) bond lengths are 1.92 Å. Both Cu(2)-N(4) bond lengths are 2.05 Å. Both Cu(2)-O(6) bond lengths are 2.56 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 1.50 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(5), and one O(6) atom. The C(3)-O(5) bond length is 1.27 Å. The C(3)-O(6) bond length is 1.27 Å. In the fourth C site, C(4) is bonded in a bent 120 degrees geometry to one O(7) and one O(8) atom. The C(4)-O(7) bond length is 1.27 Å. The C(4)-O(8) bond length is 1.28 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one N(4) and one H(1,4) atom. The C(5)-N(4) bond length is 1.35 Å. The C(5)-H(1,4) bond length is 1.09 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to 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(1,4) atom. The C(9)-N(4) bond length is 1.35 Å. The C(9)-H(1,4) 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(3), and one O(4) atom. The C(10)-O(3) bond length is 1.27 Å. The C(10)-O(4) bond length is 1.28 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 1.39 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 bent 120 degrees geometry to one C(13), one O(1), and one O(2) atom. The C(16)-O(1) bond length is 1.28 Å. The C(16)-O(2) 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 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 nine inequivalent H sites. In the first H site, H(1,4) 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(5) is bonded in a single-bond geometry to one C(11) atom. In the fifth H site, H(6) is bonded in a single-bond geometry to one C(12) atom. In the sixth H site, H(7) is bonded in a single-bond geometry to one C(14) atom. In the seventh H site, H(8) is bonded in a single-bond geometry to one C(15) atom. In the eighth H site, H(9) is bonded in a single-bond geometry to one O(9) atom. The H(9)-O(9) bond length is 0.98 Å. In the ninth H site, H(10) is bonded in a single-bond geometry to one O(6) and one O(9) atom. The H(10)-O(6) bond length is 1.70 Å. The H(10)-O(9) bond length is 1.01 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one Gd(1) and one C(16) atom. In the second O site, O(2) is bonded in a distorted L-shaped geometry to one Gd(1) and one C(16) atom. In the third O site, O(3) is bonded in a distorted L-shaped geometry to one Gd(1) and one C(10) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one Gd(1) and one C(10) atom. In the fifth O site, O(5) is bonded in a bent 150 degrees geometry to one Gd(1) and one C(3) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Cu(2), one C(3), and one H(10) atom. In the seventh O site, O(7) is bonded in a 3-coordinate geometry to two equivalent Gd(1) and one C(4) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to one Gd(1), one Cu(1), and one C(4) atom. In the ninth O site, O(9) is bonded in a water-like geometry to one Gd(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 [Gd] ,2 [Cu]. The MOF has largest included sphere 3.93 A, density 1.93 g/cm3, surface area 3115.70 m2/g, accessible volume 0.18 cm3/g