NiP2H22(CO)10 crystallizes in the triclinic P-1 space group. Ni(1) is bonded to two equivalent O(2), two equivalent O(4), and two equivalent O(5) atoms to form NiO6 octahedra that share corners with two equivalent P(1)CO3 tetrahedra. Both Ni(1)-O(2) bond lengths are 2.16 Å. Both Ni(1)-O(4) bond lengths are 2.05 Å. Both Ni(1)-O(5) bond lengths are 2.05 Å. There are five inequivalent C sites. In the first C site, C(1) is bonded in a distorted single-bond geometry to one C(2), one C(4), and one H(6) atom. The C(1)-C(2) bond length is 1.40 Å. The C(1)-C(4) bond length is 1.40 Å. The C(1)-H(6) bond length is 1.09 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(4), and one C(5) atom. The C(2)-C(4) bond length is 1.41 Å. The C(2)-C(5) bond length is 1.50 Å. In the third C site, C(3) is bonded in a distorted water-like geometry to one C(4), one P(1), one H(7), and one H(8) atom. The C(3)-C(4) bond length is 1.50 Å. The C(3)-P(1) bond length is 1.81 Å. The C(3)-H(7) bond length is 1.10 Å. The C(3)-H(8) bond length is 1.10 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(1), one C(2), and one C(3) atom. In the fifth C site, C(5) is bonded in a distorted trigonal non-coplanar geometry to one C(2), one H(10), one H(11), and one H(9) atom. The C(5)-H(10) bond length is 1.10 Å. The C(5)-H(11) bond length is 1.10 Å. The C(5)-H(9) bond length is 1.10 Å. P(1) is bonded to one C(3), one O(1), one O(2), and one O(3) atom to form PCO3 tetrahedra that share  a cornercorner with one Ni(1)O6 octahedra. The corner-sharing octahedral tilt angles are 23°. The P(1)-O(1) bond length is 1.55 Å. The P(1)-O(2) bond length is 1.50 Å. The P(1)-O(3) bond length is 1.61 Å. There are eleven inequivalent H sites. In the first H site, H(1) is bonded in a distorted single-bond geometry to one O(1) and one O(3) atom. The H(1)-O(1) bond length is 1.68 Å. The H(1)-O(3) bond length is 1.01 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(4) atom. The H(2)-O(4) bond length is 1.00 Å. In the third H site, H(3) is bonded in a single-bond geometry to one O(4) atom. The H(3)-O(4) bond length is 0.99 Å. In the fourth H site, H(4) is bonded in a distorted single-bond geometry to one O(1) and one O(5) atom. The H(4)-O(1) bond length is 1.63 Å. The H(4)-O(5) bond length is 1.01 Å. In the fifth H site, H(5) is bonded in a distorted single-bond geometry to one O(1) and one O(5) atom. The H(5)-O(1) bond length is 1.65 Å. The H(5)-O(5) bond length is 1.01 Å. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(1) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(3) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(3) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(5) atom. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(5) atom. In the eleventh H site, H(11) is bonded in a single-bond geometry to one C(5) atom. There are five inequivalent O sites. In the first O site, O(1) is bonded in a rectangular see-saw-like geometry to one P(1), one H(1), one H(4), and one H(5) atom. In the second O site, O(2) is bonded in a bent 150 degrees geometry to one Ni(1) and one P(1) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one P(1) and one H(1) atom. In the fourth O site, O(4) is bonded in a distorted water-like geometry to one Ni(1), one H(2), and one H(3) atom. In the fifth O site, O(5) is bonded in a distorted water-like geometry to one Ni(1), one H(4), and one H(5) atom. Linkers: 1 Cc1cc(CP([O])(=O)O)c(C)cc1CP([O])(=O)O. Metal clusters: 1 O.O.O.O.[O]P(O)O[Ni]OP([O])O. The MOF has largest included sphere 1.87 A, density 1.83 g/cm3, surface area 4069.62 m2/g, accessible volume 0.04 cm3/g