PbNi2V2O8 crystallizes in the tetragonal I4_1cd space group. V(1) is bonded to one O(1), one O(2), one O(3), and one O(4) atom to form VO4 tetrahedra that share corners with six equivalent Ni(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 46-56°. Ni(1) is bonded to one O(3), one O(4), two equivalent O(1), and two equivalent O(2) atoms to form NiO6 octahedra that share corners with six equivalent V(1)O4 tetrahedra and edges with two equivalent Ni(1)O6 octahedra. Pb(1) is bonded in a 4-coordinate geometry to two equivalent O(3) and two equivalent O(4) atoms. There are four inequivalent O sites. In the first O site, O(4) is bonded in a 3-coordinate geometry to one V(1), one Ni(1), and one Pb(1) atom. In the second O site, O(1) is bonded in a distorted trigonal planar geometry to one V(1) and two equivalent Ni(1) atoms. In the third O site, O(2) is bonded in a 3-coordinate geometry to one V(1) and two equivalent Ni(1) atoms. In the fourth O site, O(3) is bonded in a 3-coordinate geometry to one V(1), one Ni(1), and one Pb(1) atom.
PbNi2V2O8 crystallizes in the tetragonal I4_1cd space group. V(1) is bonded to one O(1), one O(2), one O(3), and one O(4) atom to form VO4 tetrahedra that share corners with six equivalent Ni(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 46-56°. The V(1)-O(1) bond length is 1.76 Å. The V(1)-O(2) bond length is 1.76 Å. The V(1)-O(3) bond length is 1.75 Å. The V(1)-O(4) bond length is 1.73 Å. Ni(1) is bonded to one O(3), one O(4), two equivalent O(1), and two equivalent O(2) atoms to form NiO6 octahedra that share corners with six equivalent V(1)O4 tetrahedra and edges with two equivalent Ni(1)O6 octahedra. The Ni(1)-O(3) bond length is 2.09 Å. The Ni(1)-O(4) bond length is 2.06 Å. There is one shorter (2.04 Å) and one longer (2.14 Å) Ni(1)-O(1) bond length. There is one shorter (2.07 Å) and one longer (2.12 Å) Ni(1)-O(2) bond length. Pb(1) is bonded in a 4-coordinate geometry to two equivalent O(3) and two equivalent O(4) atoms. Both Pb(1)-O(3) bond lengths are 2.48 Å. Both Pb(1)-O(4) bond lengths are 2.49 Å. There are four inequivalent O sites. In the first O site, O(4) is bonded in a 3-coordinate geometry to one V(1), one Ni(1), and one Pb(1) atom. In the second O site, O(1) is bonded in a distorted trigonal planar geometry to one V(1) and two equivalent Ni(1) atoms. In the third O site, O(2) is bonded in a 3-coordinate geometry to one V(1) and two equivalent Ni(1) atoms. In the fourth O site, O(3) is bonded in a 3-coordinate geometry to one V(1), one Ni(1), and one Pb(1) atom.