K3CuC10PH16(NO6)2 crystallizes in the orthorhombic P2_12_12 space group. There are two inequivalent K sites. In the first K site, K(1) is bonded in a distorted octahedral geometry to two equivalent O(2), two equivalent O(4), and two equivalent O(6) atoms. Both K(1)-O(2) bond lengths are 2.80 Å. Both K(1)-O(4) bond lengths are 2.61 Å. Both K(1)-O(6) bond lengths are 2.76 Å. In the second K site, K(2) is bonded in a 8-coordinate geometry to one H(7), one O(1), one O(3), one O(4), one O(5), one O(6), and two equivalent O(2) atoms. The K(2)-H(7) bond length is 2.97 Å. The K(2)-O(1) bond length is 2.87 Å. The K(2)-O(3) bond length is 2.74 Å. The K(2)-O(4) bond length is 3.15 Å. The K(2)-O(5) bond length is 2.78 Å. The K(2)-O(6) bond length is 2.80 Å. There is one shorter (2.73 Å) and one longer (3.01 Å) K(2)-O(2) bond length. Cu(1) is bonded to two equivalent N(1), two equivalent O(1), and two equivalent O(3) atoms to form CuN2O4 octahedra that share corners with two equivalent C(5)PH2N tetrahedra. Both Cu(1)-N(1) bond lengths are 2.09 Å. Both Cu(1)-O(1) bond lengths are 2.01 Å. Both Cu(1)-O(3) bond lengths are 2.29 Å. There are five inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal non-coplanar geometry to one N(1), one H(1), and one H(2) atom. The C(1)-N(1) bond length is 1.48 Å. The C(1)-H(1) bond length is 1.10 Å. The C(1)-H(2) bond length is 1.10 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(2)-O(1) bond length is 1.30 Å. The C(2)-O(2) bond length is 1.25 Å. In the third C site, C(3) is bonded in a distorted trigonal non-coplanar geometry to one N(1), one H(3), and one H(4) atom. The C(3)-N(1) bond length is 1.49 Å. The C(3)-H(3) bond length is 1.10 Å. The C(3)-H(4) bond length is 1.10 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one O(3) and one O(4) atom. The C(4)-O(3) bond length is 1.27 Å. The C(4)-O(4) bond length is 1.26 Å. In the fifth C site, C(5) is bonded to one P(1), one N(1), one H(5), and one H(6) atom to form distorted CPH2N tetrahedra that share  a cornercorner with one Cu(1)N2O4 octahedra and  a cornercorner with one C(5)PH2N tetrahedra. The corner-sharing octahedral tilt angles are 69°. The C(5)-P(1) bond length is 1.83 Å. The C(5)-N(1) bond length is 1.48 Å. The C(5)-H(5) bond length is 1.10 Å. The C(5)-H(6) bond length is 1.11 Å. P(1) is bonded to two equivalent C(5) and two equivalent O(5) atoms to form distorted PC2O2 tetrahedra that share corners with two equivalent N(1)CuC3 tetrahedra. Both P(1)-O(5) bond lengths are 1.53 Å. N(1) is bonded to one Cu(1), one C(1), one C(3), and one C(5) atom to form NCuC3 tetrahedra that share  a cornercorner with one P(1)C2O2 tetrahedra and  a cornercorner with one N(1)CuC3 tetrahedra. There are eight 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(1) 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 C(5) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(5) atom. In the seventh H site, H(7) is bonded in a distorted single-bond geometry to one K(2), one O(5), and one O(6) atom. The H(7)-O(5) bond length is 1.67 Å. The H(7)-O(6) 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. There are six inequivalent O sites. In the first O site, O(1) is bonded in a 2-coordinate geometry to one K(2), one Cu(1), and one C(2) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one K(1), two equivalent K(2), and one C(2) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one K(2), one Cu(1), and one C(4) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one K(1), one K(2), and one C(4) atom. In the fifth O site, O(5) is bonded in a 3-coordinate geometry to one K(2), one P(1), and one H(7) atom. In the sixth O site, O(6) is bonded in a water-like geometry to one K(1), one K(2), one H(7), and one H(8) atom. Linkers: 2 [O]C(=O)CN(CC([O])=O)CP([O])(=O)CN(CC([O])=O)CC([O])=O. Metal clusters: 6 [K] ,2 [Cu]. The MOF has largest included sphere 1.84 A, density 1.94 g/cm3, surface area 1779.20 m2/g, accessible volume 0.05 cm3/g