WFe2Ni3P6O24 crystallizes in the trigonal R3 space group. W(1) is bonded to three equivalent O(3) and three equivalent O(6) atoms to form WO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra, and  a faceface with one Fe(1)O6 octahedra. There are two inequivalent Fe sites. In the first Fe site, Fe(1) is bonded to three equivalent O(2) and three equivalent O(6) atoms to form distorted FeO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra,  a faceface with one W(1)O6 octahedra, and  a faceface with one Ni(2)O6 octahedra. In the second Fe site, Fe(2) is bonded to three equivalent O(4) and three equivalent O(7) atoms to form FeO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra,  a faceface with one Ni(1)O6 octahedra, and  a faceface with one Ni(3)O6 octahedra. There are three inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to three equivalent O(4) and three equivalent O(8) atoms to form distorted NiO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra, and  a faceface with one Fe(2)O6 octahedra. In the second Ni site, Ni(2) is bonded to three equivalent O(2) and three equivalent O(5) atoms to form distorted NiO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra, and  a faceface with one Fe(1)O6 octahedra. In the third Ni site, Ni(3) is bonded to three equivalent O(1) and three equivalent O(7) atoms to form NiO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra, and  a faceface with one Fe(2)O6 octahedra. There are two inequivalent P sites. In the first P site, P(1) is bonded to one O(1), one O(2), one O(3), and one O(4) atom to form PO4 tetrahedra that share  a cornercorner with one W(1)O6 octahedra,  a cornercorner with one Fe(1)O6 octahedra,  a cornercorner with one Fe(2)O6 octahedra,  a cornercorner with one Ni(1)O6 octahedra,  a cornercorner with one Ni(2)O6 octahedra, and  a cornercorner with one Ni(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 22-60°. In the second P site, P(2) is bonded to one O(5), one O(6), one O(7), and one O(8) atom to form PO4 tetrahedra that share  a cornercorner with one W(1)O6 octahedra,  a cornercorner with one Fe(1)O6 octahedra,  a cornercorner with one Fe(2)O6 octahedra,  a cornercorner with one Ni(1)O6 octahedra,  a cornercorner with one Ni(2)O6 octahedra, and  a cornercorner with one Ni(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 33-53°. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a bent 150 degrees geometry to one Ni(3) and one P(1) atom. In the second O site, O(2) is bonded in a 3-coordinate geometry to one Fe(1), one Ni(2), and one P(1) atom. In the third O site, O(3) is bonded in a bent 150 degrees geometry to one W(1) and one P(1) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Fe(2), one Ni(1), and one P(1) atom. In the fifth O site, O(5) is bonded in a bent 150 degrees geometry to one Ni(2) and one P(2) atom. In the sixth O site, O(6) is bonded in a 3-coordinate geometry to one W(1), one Fe(1), and one P(2) atom. In the seventh O site, O(7) is bonded in a 3-coordinate geometry to one Fe(2), one Ni(3), and one P(2) atom. In the eighth O site, O(8) is bonded in a bent 150 degrees geometry to one Ni(1) and one P(2) atom.
WFe2Ni3P6O24 crystallizes in the trigonal R3 space group. W(1) is bonded to three equivalent O(3) and three equivalent O(6) atoms to form WO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra, and  a faceface with one Fe(1)O6 octahedra. All W(1)-O(3) bond lengths are 1.89 Å. All W(1)-O(6) bond lengths are 1.99 Å. There are two inequivalent Fe sites. In the first Fe site, Fe(1) is bonded to three equivalent O(2) and three equivalent O(6) atoms to form distorted FeO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra,  a faceface with one W(1)O6 octahedra, and  a faceface with one Ni(2)O6 octahedra. All Fe(1)-O(2) bond lengths are 1.98 Å. All Fe(1)-O(6) bond lengths are 2.32 Å. In the second Fe site, Fe(2) is bonded to three equivalent O(4) and three equivalent O(7) atoms to form FeO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra,  a faceface with one Ni(1)O6 octahedra, and  a faceface with one Ni(3)O6 octahedra. All Fe(2)-O(4) bond lengths are 2.10 Å. All Fe(2)-O(7) bond lengths are 2.05 Å. There are three inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to three equivalent O(4) and three equivalent O(8) atoms to form distorted NiO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra, and  a faceface with one Fe(2)O6 octahedra. All Ni(1)-O(4) bond lengths are 2.19 Å. All Ni(1)-O(8) bond lengths are 2.00 Å. In the second Ni site, Ni(2) is bonded to three equivalent O(2) and three equivalent O(5) atoms to form distorted NiO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra, and  a faceface with one Fe(1)O6 octahedra. All Ni(2)-O(2) bond lengths are 2.17 Å. All Ni(2)-O(5) bond lengths are 1.94 Å. In the third Ni site, Ni(3) is bonded to three equivalent O(1) and three equivalent O(7) atoms to form NiO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra, corners with three equivalent P(2)O4 tetrahedra, and  a faceface with one Fe(2)O6 octahedra. All Ni(3)-O(1) bond lengths are 1.97 Å. All Ni(3)-O(7) bond lengths are 2.10 Å. There are two inequivalent P sites. In the first P site, P(1) is bonded to one O(1), one O(2), one O(3), and one O(4) atom to form PO4 tetrahedra that share  a cornercorner with one W(1)O6 octahedra,  a cornercorner with one Fe(1)O6 octahedra,  a cornercorner with one Fe(2)O6 octahedra,  a cornercorner with one Ni(1)O6 octahedra,  a cornercorner with one Ni(2)O6 octahedra, and  a cornercorner with one Ni(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 22-60°. The P(1)-O(1) bond length is 1.48 Å. The P(1)-O(2) bond length is 1.56 Å. The P(1)-O(3) bond length is 1.62 Å. The P(1)-O(4) bond length is 1.54 Å. In the second P site, P(2) is bonded to one O(5), one O(6), one O(7), and one O(8) atom to form PO4 tetrahedra that share  a cornercorner with one W(1)O6 octahedra,  a cornercorner with one Fe(1)O6 octahedra,  a cornercorner with one Fe(2)O6 octahedra,  a cornercorner with one Ni(1)O6 octahedra,  a cornercorner with one Ni(2)O6 octahedra, and  a cornercorner with one Ni(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 33-53°. The P(2)-O(5) bond length is 1.50 Å. The P(2)-O(6) bond length is 1.67 Å. The P(2)-O(7) bond length is 1.56 Å. The P(2)-O(8) bond length is 1.50 Å. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a bent 150 degrees geometry to one Ni(3) and one P(1) atom. In the second O site, O(2) is bonded in a 3-coordinate geometry to one Fe(1), one Ni(2), and one P(1) atom. In the third O site, O(3) is bonded in a bent 150 degrees geometry to one W(1) and one P(1) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Fe(2), one Ni(1), and one P(1) atom. In the fifth O site, O(5) is bonded in a bent 150 degrees geometry to one Ni(2) and one P(2) atom. In the sixth O site, O(6) is bonded in a 3-coordinate geometry to one W(1), one Fe(1), and one P(2) atom. In the seventh O site, O(7) is bonded in a 3-coordinate geometry to one Fe(2), one Ni(3), and one P(2) atom. In the eighth O site, O(8) is bonded in a bent 150 degrees geometry to one Ni(1) and one P(2) atom.