Dy2CuC10H14S(N2O9)2 crystallizes in the triclinic P-1 space group. There are two inequivalent Dy sites. In the first Dy site, Dy(1) is bonded in a 8-coordinate geometry to one N(1), one N(4), one O(10), one O(11), one O(12), one O(2), one O(8), and one O(9) atom. The Dy(1)-N(1) bond length is 2.47 Å. The Dy(1)-N(4) bond length is 2.53 Å. The Dy(1)-O(10) bond length is 2.33 Å. The Dy(1)-O(11) bond length is 2.46 Å. The Dy(1)-O(12) bond length is 2.31 Å. The Dy(1)-O(2) bond length is 2.36 Å. The Dy(1)-O(8) bond length is 2.36 Å. The Dy(1)-O(9) bond length is 2.32 Å. In the second Dy site, Dy(2) is bonded in a 8-coordinate geometry to one O(1), one O(13), one O(15), one O(16), one O(17), one O(18), one O(7), and one O(8) atom. The Dy(2)-O(1) bond length is 2.44 Å. The Dy(2)-O(13) bond length is 2.35 Å. The Dy(2)-O(15) bond length is 2.37 Å. The Dy(2)-O(16) bond length is 2.37 Å. The Dy(2)-O(17) bond length is 2.36 Å. The Dy(2)-O(18) bond length is 2.31 Å. The Dy(2)-O(7) bond length is 2.38 Å. The Dy(2)-O(8) bond length is 2.51 Å. Cu(1) is bonded in a square co-planar geometry to one N(2), one N(3), one O(4), and one O(5) atom. The Cu(1)-N(2) bond length is 1.93 Å. The Cu(1)-N(3) bond length is 1.92 Å. The Cu(1)-O(4) bond length is 2.00 Å. The Cu(1)-O(5) bond length is 2.01 Å. There are ten inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.47 Å. The C(1)-O(1) bond length is 1.26 Å. The C(1)-O(2) bond length is 1.29 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 N(1) atom. The C(2)-C(3) bond length is 1.40 Å. The C(2)-N(1) bond length is 1.37 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2), one C(4), and one H(1) atom. The C(3)-C(4) bond length is 1.39 Å. The C(3)-H(1) bond length is 1.08 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 N(2) atom. The C(4)-C(5) bond length is 1.46 Å. The C(4)-N(2) bond length is 1.36 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(5)-O(3) bond length is 1.25 Å. The C(5)-O(4) bond length is 1.31 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(7), one O(5), and one O(6) atom. The C(6)-C(7) bond length is 1.47 Å. The C(6)-O(5) bond length is 1.31 Å. The C(6)-O(6) bond length is 1.26 Å. In the seventh C site, C(7) is bonded in a distorted single-bond geometry to one C(6), one C(8), and one N(3) atom. The C(7)-C(8) bond length is 1.40 Å. The C(7)-N(3) bond length is 1.36 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one C(7), one C(9), and one H(2) atom. The C(8)-C(9) bond length is 1.41 Å. The C(8)-H(2) bond length is 1.09 Å. In the ninth C site, C(9) is bonded in a distorted single-bond geometry to one C(10), one C(8), and one N(4) atom. The C(9)-C(10) bond length is 1.46 Å. The C(9)-N(4) bond length is 1.37 Å. In the tenth C site, C(10) is bonded in a distorted bent 120 degrees geometry to one C(9), 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 1.30 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a distorted trigonal planar geometry to one Dy(1), one C(2), 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 3-coordinate geometry to one Cu(1), one C(4), and one N(1) atom. In the third N site, N(3) is bonded in a distorted trigonal planar geometry to one Cu(1), one C(7), and one N(4) atom. The N(3)-N(4) bond length is 1.32 Å. In the fourth N site, N(4) is bonded in a distorted single-bond geometry to one Dy(1), one C(9), and one N(3) atom. There are fourteen inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(8) atom. In the third H site, H(3) is bonded in a single-bond geometry to one O(9) atom. The H(3)-O(9) bond length is 0.99 Å. In the fourth H site, H(4) is bonded in a distorted single-bond geometry to one O(4) and one O(9) atom. The H(4)-O(4) bond length is 1.66 Å. The H(4)-O(9) bond length is 1.00 Å. In the fifth H site, H(5) is bonded in a distorted linear geometry to one O(10) and one O(3) atom. The H(5)-O(10) bond length is 1.01 Å. The H(5)-O(3) bond length is 1.58 Å. In the sixth H site, H(6) is bonded in a distorted single-bond geometry to one O(10) and one O(6) atom. The H(6)-O(10) bond length is 1.00 Å. The H(6)-O(6) bond length is 1.68 Å. In the seventh H site, H(7) is bonded in a distorted single-bond geometry to one O(11) and one O(14) atom. The H(7)-O(11) bond length is 1.01 Å. The H(7)-O(14) bond length is 1.61 Å. In the eighth H site, H(8) is bonded in a single-bond geometry to one O(11) atom. The H(8)-O(11) bond length is 0.99 Å. In the ninth H site, H(9) is bonded in a single-bond geometry to one O(16) atom. The H(9)-O(16) bond length is 1.00 Å. In the tenth H site, H(10) is bonded in a single-bond geometry to one O(16) atom. The H(10)-O(16) bond length is 0.98 Å. In the eleventh H site, H(11) is bonded in a distorted single-bond geometry to one O(17) and one O(6) atom. The H(11)-O(17) bond length is 1.00 Å. The H(11)-O(6) bond length is 1.67 Å. In the twelfth H site, H(12) is bonded in a single-bond geometry to one O(17) atom. The H(12)-O(17) bond length is 1.00 Å. In the thirteenth H site, H(13) is bonded in a linear geometry to one O(18) and one O(2) atom. The H(13)-O(18) bond length is 1.01 Å. The H(13)-O(2) bond length is 1.63 Å. In the fourteenth H site, H(14) is bonded in a single-bond geometry to one O(18) atom. The H(14)-O(18) bond length is 0.98 Å. S(1) is bonded in a tetrahedral geometry to one O(12), one O(13), one O(14), and one O(15) atom. The S(1)-O(12) bond length is 1.48 Å. The S(1)-O(13) bond length is 1.49 Å. The S(1)-O(14) bond length is 1.48 Å. The S(1)-O(15) bond length is 1.51 Å. There are eighteen inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one Dy(2) and one C(1) atom. In the second O site, O(2) is bonded in a distorted trigonal planar geometry to one Dy(1), one C(1), and one H(13) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one C(5) and one H(5) atom. In the fourth O site, O(4) is bonded in a distorted trigonal planar geometry to one Cu(1), one C(5), and one H(4) atom. In the fifth O site, O(5) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(6) atom. In the sixth O site, O(6) is bonded in a 3-coordinate geometry to one C(6), one H(11), and one H(6) atom. In the seventh O site, O(7) is bonded in a distorted single-bond geometry to one Dy(2) and one C(10) atom. In the eighth O site, O(8) is bonded in a 3-coordinate geometry to one Dy(1), one Dy(2), and one C(10) atom. In the ninth O site, O(9) is bonded in a distorted water-like geometry to one Dy(1), one H(3), and one H(4) atom. In the tenth O site, O(10) is bonded in a distorted water-like geometry to one Dy(1), one H(5), and one H(6) atom. In the eleventh O site, O(11) is bonded in a water-like geometry to one Dy(1), one H(7), and one H(8) atom. In the twelfth O site, O(12) is bonded in a bent 150 degrees geometry to one Dy(1) and one S(1) atom. In the thirteenth O site, O(13) is bonded in a distorted bent 120 degrees geometry to one Dy(2) and one S(1) atom. In the fourteenth O site, O(14) is bonded in a bent 120 degrees geometry to one H(7) and one S(1) atom. In the fifteenth O site, O(15) is bonded in a distorted bent 150 degrees geometry to one Dy(2) and one S(1) atom. In the sixteenth O site, O(16) is bonded in a distorted water-like geometry to one Dy(2), one H(10), and one H(9) atom. In the seventeenth O site, O(17) is bonded in a distorted water-like geometry to one Dy(2), one H(11), and one H(12) atom. In the eighteenth O site, O(18) is bonded in a distorted water-like geometry to one Dy(2), one H(13), and one H(14) atom. Linkers: 3 [O]C(=O)[C]1C=C(C([O])=O)N=N1 ,1 [O]C(=O)C1=CC(C([O])=O)=N[N]1. Metal clusters: 4 [Dy] ,2 [Cu]. The MOF has largest included sphere 3.48 A, density 2.83 g/cm3, surface area 2160.37 m2/g, accessible volume 0.06 cm3/g