DyH9(CO2)4 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 O(1), one O(2), one O(3), one O(4), one O(7), one O(8), and two equivalent O(6) atoms. The Dy(1)-O(1) bond length is 2.36 Å. The Dy(1)-O(2) bond length is 2.32 Å. The Dy(1)-O(3) bond length is 2.49 Å. The Dy(1)-O(4) bond length is 2.35 Å. The Dy(1)-O(7) bond length is 2.38 Å. The Dy(1)-O(8) bond length is 2.54 Å. There is one shorter (2.27 Å) and one longer (2.28 Å) Dy(1)-O(6) bond length. In the second Dy site, Dy(2) is bonded in a 8-coordinate geometry to one O(10), one O(11), one O(12), one O(15), one O(16), one O(9), and two equivalent O(14) atoms. The Dy(2)-O(10) bond length is 2.36 Å. The Dy(2)-O(11) bond length is 2.49 Å. The Dy(2)-O(12) bond length is 2.40 Å. The Dy(2)-O(15) bond length is 2.42 Å. The Dy(2)-O(16) bond length is 2.38 Å. The Dy(2)-O(9) bond length is 2.42 Å. There is one shorter (2.24 Å) and one longer (2.26 Å) Dy(2)-O(14) bond length. There are eight inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(1)-O(1) bond length is 1.28 Å. The C(1)-O(2) bond length is 1.26 Å. In the second C site, C(2) is bonded in a distorted trigonal non-coplanar geometry to one H(1), one H(2), and one O(3) atom. The C(2)-H(1) bond length is 1.10 Å. The C(2)-H(2) bond length is 1.10 Å. The C(2)-O(3) bond length is 1.43 Å. In the third C site, C(3) is bonded in a distorted trigonal non-coplanar geometry to one H(3), one H(4), and one O(3) atom. The C(3)-H(3) bond length is 1.10 Å. The C(3)-H(4) bond length is 1.10 Å. The C(3)-O(3) bond length is 1.43 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one O(4) and one O(5) atom. The C(4)-O(4) bond length is 1.26 Å. The C(4)-O(5) bond length is 1.27 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one O(12) and one O(13) atom. The C(5)-O(12) bond length is 1.27 Å. The C(5)-O(13) bond length is 1.27 Å. In the sixth C site, C(6) is bonded in a distorted trigonal non-coplanar geometry to one H(10), one H(11), and one O(11) atom. The C(6)-H(10) bond length is 1.10 Å. The C(6)-H(11) bond length is 1.10 Å. The C(6)-O(11) bond length is 1.42 Å. In the seventh C site, C(7) is bonded in a distorted trigonal non-coplanar geometry to one H(12), one H(13), and one O(11) atom. The C(7)-H(12) bond length is 1.10 Å. The C(7)-H(13) bond length is 1.10 Å. The C(7)-O(11) bond length is 1.43 Å. In the eighth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one O(10) and one O(9) atom. The C(8)-O(10) bond length is 1.25 Å. The C(8)-O(9) bond length is 1.29 Å. There are eighteen 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(2) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(3) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(3) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one O(8) atom. The H(5)-O(8) bond length is 0.99 Å. In the sixth H site, H(6) is bonded in a single-bond geometry to one O(8) atom. The H(6)-O(8) bond length is 0.99 Å. In the seventh H site, H(7) is bonded in a distorted single-bond geometry to one O(5) and one O(7) atom. The H(7)-O(5) bond length is 1.66 Å. The H(7)-O(7) bond length is 1.00 Å. In the eighth H site, H(8) is bonded in a single-bond geometry to one O(6) atom. The H(8)-O(6) bond length is 0.98 Å. In the ninth H site, H(9) is bonded in a distorted linear geometry to one O(13) and one O(7) atom. The H(9)-O(13) bond length is 1.62 Å. The H(9)-O(7) bond length is 1.01 Å. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(6) atom. In the eleventh H site, H(11) is bonded in a single-bond geometry to one C(6) atom. In the twelfth H site, H(12) is bonded in a single-bond geometry to one C(7) atom. In the thirteenth H site, H(13) is bonded in a single-bond geometry to one C(7) atom. In the fourteenth H site, H(14) is bonded in a single-bond geometry to one O(16) atom. The H(14)-O(16) bond length is 0.99 Å. In the fifteenth H site, H(15) is bonded in a single-bond geometry to one O(13) and one O(15) atom. The H(15)-O(13) bond length is 1.72 Å. The H(15)-O(15) bond length is 1.00 Å. In the sixteenth H site, H(16) is bonded in a single-bond geometry to one O(14) atom. The H(16)-O(14) bond length is 0.97 Å. In the seventeenth H site, H(17) is bonded in a single-bond geometry to one O(15) and one O(5) atom. The H(17)-O(15) bond length is 1.00 Å. The H(17)-O(5) bond length is 1.71 Å. In the eighteenth H site, H(18) is bonded in a single-bond geometry to one O(16) atom. The H(18)-O(16) bond length is 1.00 Å. There are sixteen inequivalent O sites. In the first O site, O(1) is bonded in a 1-coordinate geometry to one Dy(1) and one C(1) atom. In the second O site, O(2) is bonded in a distorted bent 150 degrees geometry to one Dy(1) and one C(1) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Dy(1), one C(2), and one C(3) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one Dy(1) and one C(4) atom. In the fifth O site, O(5) is bonded in a distorted trigonal planar geometry to one C(4), one H(17), and one H(7) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to two equivalent Dy(1) and one H(8) atom. In the seventh O site, O(7) is bonded in a water-like geometry to one Dy(1), one H(7), and one H(9) atom. In the eighth O site, O(8) is bonded in a water-like geometry to one Dy(1), one H(5), and one H(6) atom. In the ninth O site, O(9) is bonded in a distorted single-bond geometry to one Dy(2) and one C(8) atom. In the tenth O site, O(10) is bonded in a distorted bent 150 degrees geometry to one Dy(2) and one C(8) atom. In the eleventh O site, O(11) is bonded in a distorted bent 120 degrees geometry to one Dy(2), one C(6), and one C(7) atom. In the twelfth O site, O(12) is bonded in a distorted bent 120 degrees geometry to one Dy(2) and one C(5) atom. In the thirteenth O site, O(13) is bonded in a distorted trigonal planar geometry to one C(5), one H(15), and one H(9) atom. In the fourteenth O site, O(14) is bonded in a distorted single-bond geometry to two equivalent Dy(2) and one H(16) atom. In the fifteenth O site, O(15) is bonded in a water-like geometry to one Dy(2), one H(15), and one H(17) atom. In the sixteenth O site, O(16) is bonded in a distorted water-like geometry to one Dy(2), one H(14), and one H(18) atom. Linkers: 2 [O]C(=O)COCC([O])=O ,4 [OH]. Metal clusters: 4 [Dy]. The MOF has largest included sphere 1.68 A, density 2.91 g/cm3, surface area 2262.79 m2/g, accessible volume 0.04 cm3/g