Dy4H11(CO)24 crystallizes in the triclinic P1 space group. There are four inequivalent Dy sites. In the first Dy site, Dy(1) is bonded in a distorted pentagonal pyramidal geometry to one O(1), one O(2), one O(22), one O(23), one O(3), and one O(6) atom. The Dy(1)-O(1) bond length is 2.42 Å. The Dy(1)-O(2) bond length is 2.47 Å. The Dy(1)-O(22) bond length is 2.27 Å. The Dy(1)-O(23) bond length is 2.26 Å. The Dy(1)-O(3) bond length is 2.34 Å. The Dy(1)-O(6) bond length is 2.37 Å. In the second Dy site, Dy(2) is bonded in a distorted pentagonal pyramidal geometry to one O(12), one O(16), one O(17), one O(7), one O(8), and one O(9) atom. The Dy(2)-O(12) bond length is 2.37 Å. The Dy(2)-O(16) bond length is 2.27 Å. The Dy(2)-O(17) bond length is 2.26 Å. The Dy(2)-O(7) bond length is 2.42 Å. The Dy(2)-O(8) bond length is 2.47 Å. The Dy(2)-O(9) bond length is 2.34 Å. In the third Dy site, Dy(3) is bonded in a distorted pentagonal pyramidal geometry to one O(10), one O(11), one O(13), one O(14), one O(15), and one O(18) atom. The Dy(3)-O(10) bond length is 2.27 Å. The Dy(3)-O(11) bond length is 2.26 Å. The Dy(3)-O(13) bond length is 2.42 Å. The Dy(3)-O(14) bond length is 2.47 Å. The Dy(3)-O(15) bond length is 2.34 Å. The Dy(3)-O(18) bond length is 2.37 Å. In the fourth Dy site, Dy(4) is bonded in a distorted pentagonal pyramidal geometry to one O(19), one O(20), one O(21), one O(24), one O(4), and one O(5) atom. The Dy(4)-O(19) bond length is 2.42 Å. The Dy(4)-O(20) bond length is 2.47 Å. The Dy(4)-O(21) bond length is 2.34 Å. The Dy(4)-O(24) bond length is 2.37 Å. The Dy(4)-O(4) bond length is 2.27 Å. The Dy(4)-O(5) bond length is 2.26 Å. There are twenty inequivalent C sites. In the first C site, C(1,13) is bonded in a bent 120 degrees geometry to one C(2,14); one O(1); and one O(2) atom. The C(1,13)-C(2,14) bond length is 1.49 Å. The C(1,13)-O(1) bond length is 1.27 Å. The C(1,13)-O(2) bond length is 1.26 Å. In the second C site, C(2,14) is bonded in a distorted trigonal planar geometry to one C(1,13); one C(2,14); and one H(1,7) atom. The C(2,14)-C(2,14) bond length is 1.36 Å. The C(2,14)-H(1,7) bond length is 1.14 Å. In the third C site, C(3,9) is bonded in a bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(3,9)-C(4) bond length is 1.48 Å. The C(3,9)-O(3) bond length is 1.26 Å. The C(3,9)-O(4) bond length is 1.25 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(3,9); one C(5); and one H(2,5) atom. The C(4)-C(5) bond length is 1.32 Å. The C(4)-H(2,5) bond length is 1.14 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(4); one C(6,12); and one H(3,6) atom. The C(5)-C(6,12) bond length is 1.50 Å. The C(5)-H(3,6) bond length is 1.14 Å. In the sixth C site, C(6,12) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(5), and one O(6) atom. The C(6,12)-O(5) bond length is 1.24 Å. The C(6,12)-O(6) bond length is 1.25 Å. In the seventh C site, C(7) is bonded in a bent 120 degrees geometry to one C(8), one O(7), and one O(8) atom. The C(7)-C(8) bond length is 1.49 Å. The C(7)-O(7) bond length is 1.27 Å. The C(7)-O(8) bond length is 1.26 Å. In the eighth C site, C(8) is bonded in a distorted trigonal planar geometry to one C(20), one C(7), and one H(4) atom. The C(8)-C(20) bond length is 1.36 Å. The C(8)-H(4) bond length is 1.14 Å. In the ninth C site, C(10) is bonded in a distorted trigonal planar geometry to one C(11); one C(3,9); and one H(2,5) atom. The C(10)-C(11) bond length is 1.32 Å. The C(10)-C(3,9) bond length is 1.48 Å. The C(10)-H(2,5) bond length is 1.14 Å. In the tenth C site, C(11) is bonded in a distorted trigonal planar geometry to one C(10); one C(6,12); and one H(3,6) atom. The C(11)-C(6,12) bond length is 1.50 Å. The C(11)-H(3,6) bond length is 1.14 Å. In the eleventh C site, C(15) is bonded in a bent 120 degrees geometry to one C(16), one O(15), and one O(16) atom. The C(15)-C(16) bond length is 1.48 Å. The C(15)-O(15) bond length is 1.26 Å. The C(15)-O(16) bond length is 1.25 Å. In the twelfth C site, C(16) is bonded in a distorted trigonal planar geometry to one C(15), one C(17), and one H(8) atom. The C(16)-C(17) bond length is 1.32 Å. The C(16)-H(8) bond length is 1.14 Å. In the thirteenth C site, C(17) is bonded in a distorted trigonal planar geometry to one C(16), one C(18), and one H(9) atom. The C(17)-C(18) bond length is 1.50 Å. The C(17)-H(9) bond length is 1.14 Å. In the fourteenth C site, C(18) is bonded in a distorted bent 120 degrees geometry to one C(17), one O(17), and one O(18) atom. The C(18)-O(17) bond length is 1.24 Å. The C(18)-O(18) bond length is 1.25 Å. In the fifteenth C site, C(19) is bonded in a bent 120 degrees geometry to one C(20), one O(19), and one O(20) atom. The C(19)-C(20) bond length is 1.49 Å. The C(19)-O(19) bond length is 1.27 Å. The C(19)-O(20) bond length is 1.26 Å. In the sixteenth C site, C(20) is bonded in a bent 120 degrees geometry to one C(19) and one C(8) atom. In the seventeenth C site, C(21) is bonded in a bent 120 degrees geometry to one C(22), one O(21), and one O(22) atom. The C(21)-C(22) bond length is 1.48 Å. The C(21)-O(21) bond length is 1.26 Å. The C(21)-O(22) bond length is 1.25 Å. In the eighteenth C site, C(22) is bonded in a distorted trigonal planar geometry to one C(21), one C(23), and one H(10) atom. The C(22)-C(23) bond length is 1.32 Å. The C(22)-H(10) bond length is 1.14 Å. In the nineteenth C site, C(23) is bonded in a distorted trigonal planar geometry to one C(22), one C(24), and one H(11) atom. The C(23)-C(24) bond length is 1.50 Å. The C(23)-H(11) bond length is 1.14 Å. In the twentieth C site, C(24) is bonded in a distorted bent 120 degrees geometry to one C(23), one O(23), and one O(24) atom. The C(24)-O(23) bond length is 1.24 Å. The C(24)-O(24) bond length is 1.25 Å. There are eight inequivalent H sites. In the first H site, H(1,7) is bonded in a single-bond geometry to one C(2,14) atom. In the second H site, H(2,5) is bonded in a single-bond geometry to one C(4) atom. In the third H site, H(3,6) is bonded in a single-bond geometry to one C(5) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(8) atom. In the fifth H site, H(8) is bonded in a single-bond geometry to one C(16) atom. In the sixth H site, H(9) is bonded in a single-bond geometry to one C(17) atom. In the seventh H site, H(10) is bonded in a single-bond geometry to one C(22) atom. In the eighth H site, H(11) is bonded in a single-bond geometry to one C(23) atom. There are twenty-four inequivalent O sites. In the first O site, O(1) is bonded in a distorted L-shaped geometry to one Dy(1) and one C(1,13) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one Dy(1) and one C(1,13) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one Dy(1) and one C(3,9) atom. In the fourth O site, O(4) is bonded in a distorted bent 150 degrees geometry to one Dy(4) and one C(3,9) atom. In the fifth O site, O(5) is bonded in a linear geometry to one Dy(4) and one C(6,12) atom. In the sixth O site, O(6) is bonded in a bent 120 degrees geometry to one Dy(1) and one C(6,12) atom. In the seventh O site, O(7) is bonded in a distorted L-shaped geometry to one Dy(2) and one C(7) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to one Dy(2) and one C(7) atom. In the ninth O site, O(9) is bonded in a distorted bent 150 degrees geometry to one Dy(2) and one C(3,9) atom. The O(9)-C(3,9) bond length is 1.26 Å. In the tenth O site, O(10) is bonded in a distorted bent 150 degrees geometry to one Dy(3) and one C(3,9) atom. The O(10)-C(3,9) bond length is 1.25 Å. In the eleventh O site, O(11) is bonded in a linear geometry to one Dy(3) and one C(6,12) atom. The O(11)-C(6,12) bond length is 1.24 Å. In the twelfth O site, O(12) is bonded in a bent 120 degrees geometry to one Dy(2) and one C(6,12) atom. The O(12)-C(6,12) bond length is 1.25 Å. In the thirteenth O site, O(13) is bonded in a distorted L-shaped geometry to one Dy(3) and one C(1,13) atom. The O(13)-C(1,13) bond length is 1.27 Å. In the fourteenth O site, O(14) is bonded in a distorted single-bond geometry to one Dy(3) and one C(1,13) atom. The O(14)-C(1,13) bond length is 1.26 Å. In the fifteenth O site, O(15) is bonded in a distorted bent 150 degrees geometry to one Dy(3) and one C(15) atom. In the sixteenth O site, O(16) is bonded in a distorted bent 150 degrees geometry to one Dy(2) and one C(15) atom. In the seventeenth O site, O(17) is bonded in a linear geometry to one Dy(2) and one C(18) atom. In the eighteenth O site, O(18) is bonded in a bent 120 degrees geometry to one Dy(3) and one C(18) atom. In the nineteenth O site, O(19) is bonded in a distorted L-shaped geometry to one Dy(4) and one C(19) atom. In the twentieth O site, O(20) is bonded in a distorted L-shaped geometry to one Dy(4) and one C(19) atom. In the twenty-first O site, O(21) is bonded in a distorted bent 150 degrees geometry to one Dy(4) and one C(21) atom. In the twenty-second O site, O(22) is bonded in a distorted bent 150 degrees geometry to one Dy(1) and one C(21) atom. In the twenty-third O site, O(23) is bonded in a linear geometry to one Dy(1) and one C(24) atom. In the twenty-fourth O site, O(24) is bonded in a bent 120 degrees geometry to one Dy(4) and one C(24) atom. Linkers: 1 [O]C(=O)/[C]=C/C([O])=O ,5 [O]C(=O)/C=C/C([O])=O. Metal clusters: 4 [Dy]. The MOF has largest included sphere 4.98 A, density 1.68 g/cm3, surface area 2645.51 m2/g, accessible volume 0.31 cm3/g