Mo6Cu2C27P2N6H24O17(CH)8 crystallizes in the orthorhombic Pnma space group. The structure consists of thirty-two 02329_fluka molecules inside a Mo6Cu2C27P2N6H24O17 framework. In the Mo6Cu2C27P2N6H24O17 framework, there are three inequivalent Mo sites. In the first Mo site, Mo(1) is bonded in a 5-coordinate geometry to one O(1), one O(2), one O(4), one O(5), and one O(6) atom. The Mo(1)-O(1) bond length is 1.74 Å. The Mo(1)-O(2) bond length is 1.92 Å. The Mo(1)-O(4) bond length is 2.35 Å. The Mo(1)-O(5) bond length is 1.87 Å. The Mo(1)-O(6) bond length is 2.18 Å. In the second Mo site, Mo(2) is bonded in a 4-coordinate geometry to one O(2), one O(4), one O(8), and one O(9) atom. The Mo(2)-O(2) bond length is 1.88 Å. The Mo(2)-O(4) bond length is 2.38 Å. The Mo(2)-O(8) bond length is 2.33 Å. The Mo(2)-O(9) bond length is 1.92 Å. In the third Mo site, Mo(3) is bonded in a 5-coordinate geometry to one O(10), one O(11), one O(3), one O(5), and one O(7) atom. The Mo(3)-O(10) bond length is 1.91 Å. The Mo(3)-O(11) bond length is 2.33 Å. The Mo(3)-O(3) bond length is 1.71 Å. The Mo(3)-O(5) bond length is 1.88 Å. The Mo(3)-O(7) bond length is 2.47 Å. Cu(1) is bonded in a square pyramidal geometry to one N(1), one N(2), one N(3), one O(1), and one O(3) atom. The Cu(1)-N(1) bond length is 1.96 Å. The Cu(1)-N(2) bond length is 1.95 Å. The Cu(1)-N(3) bond length is 2.04 Å. The Cu(1)-O(1) bond length is 1.96 Å. The Cu(1)-O(3) bond length is 2.26 Å. There are fifteen inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(1) atom. The C(1)-N(1) bond length is 1.33 Å. The C(1)-H(1) bond length is 0.95 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(3), one C(4), and one N(1) atom. The C(2)-C(3) bond length is 1.40 Å. The C(2)-C(4) bond length is 1.50 Å. The C(2)-N(1) bond length is 1.34 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2) and one H(2) atom. The C(3)-H(2) bond length is 0.95 Å. In the fourth C site, C(4) is bonded in a 3-coordinate geometry to one C(2); one N(3); and two equivalent H(3,4) atoms. The C(4)-N(3) bond length is 1.50 Å. Both C(4)-H(3,4) bond lengths are 0.99 Å. In the fifth C site, C(5) is bonded in a 4-coordinate geometry to one C(6), one N(3), one H(5), and one H(6) atom. The C(5)-C(6) bond length is 1.48 Å. The C(5)-N(3) bond length is 1.49 Å. The C(5)-H(5) bond length is 0.99 Å. The C(5)-H(6) bond length is 0.99 Å. In the sixth C site, C(7) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(9) atom. The C(7)-N(2) bond length is 1.34 Å. The C(7)-H(9) bond length is 0.95 Å. In the seventh C site, C(11) is bonded in a distorted trigonal planar geometry to one C(12), one C(13), and one N(2) atom. The C(11)-C(12) bond length is 1.49 Å. The C(11)-C(13) bond length is 1.37 Å. The C(11)-N(2) bond length is 1.35 Å. In the eighth C site, C(12) is bonded in a 3-coordinate geometry to one C(11), one N(3), one H(13), and one H(14) atom. The C(12)-N(3) bond length is 1.48 Å. The C(12)-H(13) bond length is 0.99 Å. The C(12)-H(14) bond length is 0.99 Å. In the ninth C site, C(13) is bonded in a distorted single-bond geometry to one C(11) and one H(15) atom. The C(13)-H(15) bond length is 0.95 Å. In the tenth C site, C(15) is bonded in a distorted trigonal non-coplanar geometry to one C(15), one C(16), and one C(18) atom. The C(15)-C(15) bond length is 1.25 Å. The C(15)-C(16) bond length is 1.65 Å. The C(15)-C(18) bond length is 1.43 Å. In the eleventh C site, C(16) is bonded in a distorted bent 120 degrees geometry to one C(15) and one C(17) atom. The C(16)-C(17) bond length is 1.20 Å. In the twelfth C site, C(17) is bonded in a 3-coordinate geometry to two equivalent C(16) and one P(1) atom. The C(17)-P(1) bond length is 1.75 Å. In the thirteenth C site, C(18) is bonded in a 3-coordinate geometry to two equivalent C(15) and one P(2) atom. The C(18)-P(2) bond length is 1.79 Å. In the fourteenth C site, C(6) is bonded in a water-like geometry to one C(19); one C(5); and two equivalent H(7,8) atoms. The C(6)-C(19) bond length is 1.56 Å. Both C(6)-H(7,8) bond lengths are 0.99 Å. In the fifteenth C site, C(19) is bonded in a water-like geometry to two equivalent C(6) atoms. There are two inequivalent P sites. In the first P site, P(1) is bonded in a tetrahedral geometry to one C(17), one O(11), and two equivalent O(4) atoms. The P(1)-O(11) bond length is 1.54 Å. Both P(1)-O(4) bond lengths are 1.52 Å. In the second P site, P(2) is bonded in a tetrahedral geometry to one C(18), one O(8), and two equivalent O(6) atoms. The P(2)-O(8) bond length is 1.55 Å. Both P(2)-O(6) bond lengths are 1.51 Å. There are three inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(2) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Cu(1), one C(11), and one C(7) atom. In the third N site, N(3) is bonded in a tetrahedral geometry to one Cu(1), one C(12), one C(4), and one C(5) atom. There are ten inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(3) atom. In the third H site, H(3,4) is bonded in a single-bond geometry to one C(4) atom. In the fourth H site, H(5) is bonded in a single-bond geometry to one C(5) atom. In the fifth H site, H(6) is bonded in a single-bond geometry to one C(5) atom. In the sixth H site, H(7,8) is bonded in a single-bond geometry to one C(6) atom. In the seventh H site, H(9) is bonded in a single-bond geometry to one C(7) atom. In the eighth H site, H(13) is bonded in a single-bond geometry to one C(12) atom. In the ninth H site, H(14) is bonded in a single-bond geometry to one C(12) atom. In the tenth H site, H(15) is bonded in a single-bond geometry to one C(13) atom. There are eleven inequivalent O sites. In the first O site, O(11) is bonded in a distorted single-bond geometry to two equivalent Mo(3) and one P(1) atom. In the second O site, O(1) is bonded in a bent 150 degrees geometry to one Mo(1) and one Cu(1) atom. In the third O site, O(2) is bonded in a bent 120 degrees geometry to one Mo(1) and one Mo(2) atom. In the fourth O site, O(3) is bonded in a bent 150 degrees geometry to one Mo(3) and one Cu(1) atom. In the fifth O site, O(4) is bonded in a distorted single-bond geometry to one Mo(1), one Mo(2), and one P(1) atom. In the sixth O site, O(5) is bonded in a bent 150 degrees geometry to one Mo(1) and one Mo(3) atom. In the seventh O site, O(6) is bonded in a distorted single-bond geometry to one Mo(1) and one P(2) atom. In the eighth O site, O(7) is bonded in an L-shaped geometry to two equivalent Mo(3) atoms. In the ninth O site, O(8) is bonded in a distorted single-bond geometry to two equivalent Mo(2) and one P(2) atom. In the tenth O site, O(9) is bonded in a bent 120 degrees geometry to two equivalent Mo(2) atoms. In the eleventh O site, O(10) is bonded in a bent 120 degrees geometry to two equivalent Mo(3) atoms. Linkers: 4 [O]P([O])(=O)[C]1[C]2[C]C(P([O])([O])=O)=[C][C]21 ,4 [C](CCN(Cc1ccccn1)Cc1ccccn1)CCN(Cc1ccccn1)Cc1ccccn1. Metal clusters: 8 [Cu] ,24 [Mo]. The MOF has largest included sphere 4.22 A, density 1.84 g/cm3, surface area 3011.58 m2/g, accessible volume 0.21 cm3/g