Mo3ZnC3HO8 crystallizes in the orthorhombic I222 space group. There are nine inequivalent Mo sites. In the first Mo site, Mo(1) is bonded in a 3-coordinate geometry to one O(1), one O(2), and two equivalent O(3) atoms. The Mo(1)-O(1) bond length is 1.86 Å. The Mo(1)-O(2) bond length is 1.84 Å. There is one shorter (1.96 Å) and one longer (2.12 Å) Mo(1)-O(3) bond length. In the second Mo site, Mo(2) is bonded in a 4-coordinate geometry to one O(2), one O(4), one O(5), and one O(6) atom. The Mo(2)-O(2) bond length is 2.01 Å. The Mo(2)-O(4) bond length is 1.96 Å. The Mo(2)-O(5) bond length is 1.93 Å. The Mo(2)-O(6) bond length is 2.07 Å. In the third Mo site, Mo(3) is bonded in a 4-coordinate geometry to one O(1), one O(6), one O(7), and one O(8) atom. The Mo(3)-O(1) bond length is 2.01 Å. The Mo(3)-O(6) bond length is 2.09 Å. The Mo(3)-O(7) bond length is 1.97 Å. The Mo(3)-O(8) bond length is 2.01 Å. In the fourth Mo site, Mo(4) is bonded in a 4-coordinate geometry to one O(10), one O(7), one O(8), and one O(9) atom. The Mo(4)-O(10) bond length is 2.13 Å. The Mo(4)-O(7) bond length is 1.95 Å. The Mo(4)-O(8) bond length is 1.95 Å. The Mo(4)-O(9) bond length is 1.98 Å. In the fifth Mo site, Mo(5) is bonded in a 3-coordinate geometry to one O(11), one O(9), and two equivalent O(12) atoms. The Mo(5)-O(11) bond length is 1.86 Å. The Mo(5)-O(9) bond length is 1.90 Å. There is one shorter (2.01 Å) and one longer (2.06 Å) Mo(5)-O(12) bond length. In the sixth Mo site, Mo(6) is bonded in a distorted square co-planar geometry to one O(10), one O(11), one O(4), and one O(5) atom. The Mo(6)-O(10) bond length is 2.05 Å. The Mo(6)-O(11) bond length is 1.96 Å. The Mo(6)-O(4) bond length is 1.96 Å. The Mo(6)-O(5) bond length is 1.90 Å. In the seventh Mo site, Mo(7) is bonded in a distorted square co-planar geometry to one O(16), one O(17), and two equivalent O(15) atoms. The Mo(7)-O(16) bond length is 1.99 Å. The Mo(7)-O(17) bond length is 1.99 Å. There is one shorter (1.86 Å) and one longer (1.89 Å) Mo(7)-O(15) bond length. In the eighth Mo site, Mo(8) is bonded in a distorted T-shaped geometry to one O(16), one O(22), and two equivalent O(18) atoms. The Mo(8)-O(16) bond length is 1.96 Å. The Mo(8)-O(22) bond length is 2.08 Å. There is one shorter (1.94 Å) and one longer (1.98 Å) Mo(8)-O(18) bond length. In the ninth Mo site, Mo(9) is bonded in a 3-coordinate geometry to one O(17), one O(22), and two equivalent O(19) atoms. The Mo(9)-O(17) bond length is 1.88 Å. The Mo(9)-O(22) bond length is 1.85 Å. There is one shorter (1.98 Å) and one longer (2.01 Å) Mo(9)-O(19) bond length. There are three inequivalent Zn sites. In the first Zn site, Zn(1) is bonded in a tetrahedral geometry to one O(13), one O(3), one O(4), and one O(7) atom. The Zn(1)-O(13) bond length is 1.98 Å. The Zn(1)-O(3) bond length is 1.91 Å. The Zn(1)-O(4) bond length is 1.99 Å. The Zn(1)-O(7) bond length is 1.97 Å. In the second Zn site, Zn(2) is bonded in a tetrahedral geometry to one O(12), one O(14), one O(5), and one O(8) atom. The Zn(2)-O(12) bond length is 1.90 Å. The Zn(2)-O(14) bond length is 1.94 Å. The Zn(2)-O(5) bond length is 2.02 Å. The Zn(2)-O(8) bond length is 1.95 Å. In the third Zn site, Zn(3) is bonded in a 5-coordinate geometry to one O(15), one O(18), one O(19), one O(20), and one O(21) atom. The Zn(3)-O(15) bond length is 2.04 Å. The Zn(3)-O(18) bond length is 1.98 Å. The Zn(3)-O(19) bond length is 1.97 Å. The Zn(3)-O(20) bond length is 2.00 Å. The Zn(3)-O(21) bond length is 2.37 Å. There are nine inequivalent C sites. In the first C site, C(9) is bonded in a bent 120 degrees geometry to one C(5), one O(20), and one O(21) atom. The C(9)-C(5) bond length is 1.42 Å. The C(9)-O(20) bond length is 1.33 Å. The C(9)-O(21) bond length is 1.24 Å. In the second C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(6), and one C(7) atom. The C(1)-C(2) bond length is 1.41 Å. The C(1)-C(6) bond length is 1.43 Å. The C(1)-C(7) bond length is 1.48 Å. In the third C site, C(2) is bonded in a distorted trigonal planar geometry to one C(1), one C(3), and one H(1) atom. The C(2)-C(3) bond length is 1.33 Å. The C(2)-H(1) bond length is 0.93 Å. In the fourth C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(4), and one C(8) atom. The C(3)-C(4) bond length is 1.33 Å. The C(3)-C(8) bond length is 1.52 Å. In the fifth C site, C(4) is bonded in a distorted single-bond geometry to one C(3), one C(5), and one H(2) atom. The C(4)-C(5) bond length is 1.36 Å. The C(4)-H(2) bond length is 0.93 Å. In the sixth C site, C(5) is bonded in a trigonal planar geometry to one C(4), one C(6), and one C(9) atom. The C(5)-C(6) bond length is 1.35 Å. In the seventh C site, C(6) is bonded in a distorted single-bond geometry to one C(1), one C(5), and one H(3) atom. The C(6)-H(3) bond length is 0.93 Å. In the eighth C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(13), and one O(23) atom. The C(7)-O(13) bond length is 1.30 Å. The C(7)-O(23) bond length is 1.11 Å. In the ninth C site, C(8) is bonded in a bent 120 degrees geometry to one C(3), one O(14), and one O(24) atom. The C(8)-O(14) bond length is 1.25 Å. The C(8)-O(24) bond length is 1.13 Å. There are three 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(4) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(6) atom. There are twenty-four inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Mo(1) and one Mo(3) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Mo(1) and one Mo(2) atom. In the third O site, O(3) is bonded in a single-bond geometry to two equivalent Mo(1) and one Zn(1) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Mo(2), one Mo(6), and one Zn(1) atom. In the fifth O site, O(5) is bonded in a 3-coordinate geometry to one Mo(2), one Mo(6), and one Zn(2) atom. In the sixth O site, O(6) is bonded in a bent 120 degrees geometry to one Mo(2) and one Mo(3) atom. In the seventh O site, O(7) is bonded in a 3-coordinate geometry to one Mo(3), one Mo(4), and one Zn(1) atom. In the eighth O site, O(8) is bonded in a 3-coordinate geometry to one Mo(3), one Mo(4), and one Zn(2) atom. In the ninth O site, O(9) is bonded in a bent 120 degrees geometry to one Mo(4) and one Mo(5) atom. In the tenth O site, O(10) is bonded in a bent 120 degrees geometry to one Mo(4) and one Mo(6) atom. In the eleventh O site, O(11) is bonded in a distorted bent 120 degrees geometry to one Mo(5) and one Mo(6) atom. In the twelfth O site, O(12) is bonded in a single-bond geometry to two equivalent Mo(5) and one Zn(2) atom. In the thirteenth O site, O(13) is bonded in a water-like geometry to one Zn(1) and one C(7) atom. In the fourteenth O site, O(14) is bonded in a bent 120 degrees geometry to one Zn(2) and one C(8) atom. In the fifteenth O site, O(15) is bonded in a 3-coordinate geometry to two equivalent Mo(7) and one Zn(3) atom. In the sixteenth O site, O(16) is bonded in a bent 120 degrees geometry to one Mo(7) and one Mo(8) atom. In the seventeenth O site, O(17) is bonded in a bent 120 degrees geometry to one Mo(7) and one Mo(9) atom. In the eighteenth O site, O(18) is bonded in a 3-coordinate geometry to two equivalent Mo(8) and one Zn(3) atom. In the nineteenth O site, O(19) is bonded in a distorted single-bond geometry to two equivalent Mo(9) and one Zn(3) atom. In the twentieth O site, O(20) is bonded in a water-like geometry to one Zn(3) and one C(9) atom. In the twenty-first O site, O(21) is bonded in an L-shaped geometry to one Zn(3) and one C(9) atom. In the twenty-second O site, O(22) is bonded in a bent 120 degrees geometry to one Mo(8) and one Mo(9) atom. In the twenty-third O site, O(23) is bonded in a single-bond geometry to one C(7) atom. In the twenty-fourth O site, O(24) is bonded in a single-bond geometry to one C(8) atom. Linkers: 4 [O]C(=O)c1cc(C([O])=O)cc(C([O])=O)c1. Metal clusters: 2 O=[C]O[Zn]1O[Mo]2O[Mo]3O[Mo]45(O2)O[Mo]42(O[Mo]4O[Zn](O[C]=O)O[Mo]6(O[Zn](O[C]=O)O[Mo]7O[Mo]6O[Mo]68(O7)O[Mo]67(O[Mo]6O[Zn](O[C]=O)O[Mo]3(O1)(O6)O7)O8)(O4)O2)O5 ,1 O=[C]O[Zn]1O[Mo]2O[Mo@]34O[Zn](O[C]=O)O[Mo]5O[Mo@@]3(O1)O[Mo@]1(O5)O[Mo@@]3(O[Mo]5O[Zn](O[C]=O)O[Mo@@]67O[Mo](O[Zn](O[C]=O)O[Mo@]6(O5)O3)O[Mo@@]3(O7)O[Mo@](O2)(O4)O3)O1. RCSR code: ofp. The MOF has largest included sphere 18.95 A, density 1.01 g/cm3, surface area 1931.39 m2/g, accessible volume 0.83 cm3/g