NbFeNi(O2F)2 is Hydrophilite-derived structured and crystallizes in the monoclinic Pm space group. There are two inequivalent Nb sites. In the first Nb site, Nb(1) is bonded to one O(5), one O(6), two equivalent O(1), and two equivalent O(2) atoms to form NbO6 octahedra that share corners with four equivalent Fe(1)O6 octahedra, corners with four equivalent Ni(1)O3F3 octahedra, and edges with two equivalent Nb(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 49-52°. In the second Nb site, Nb(2) is bonded to one O(7), one O(8), two equivalent O(3), and two equivalent O(4) atoms to form NbO6 octahedra that share corners with four equivalent Fe(2)O3F3 octahedra, corners with four equivalent Fe(1)O6 octahedra, and edges with two equivalent Nb(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 47-53°. There are two inequivalent Fe sites. In the first Fe site, Fe(1) is bonded to one O(2), one O(3), two equivalent O(5), and two equivalent O(8) atoms to form FeO6 octahedra that share corners with four equivalent Nb(1)O6 octahedra, corners with four equivalent Nb(2)O6 octahedra, and edges with two equivalent Fe(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 47-52°. In the second Fe site, Fe(2) is bonded to one O(4), two equivalent O(7), one F(1), and two equivalent F(4) atoms to form FeO3F3 octahedra that share corners with four equivalent Nb(2)O6 octahedra, corners with four equivalent Ni(2)F6 octahedra, and edges with two equivalent Fe(2)O3F3 octahedra. The corner-sharing octahedral tilt angles range from 47-53°. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(1), two equivalent O(6), one F(2), and two equivalent F(3) atoms to form NiO3F3 octahedra that share corners with four equivalent Nb(1)O6 octahedra, corners with four equivalent Ni(2)F6 octahedra, and edges with two equivalent Ni(1)O3F3 octahedra. The corner-sharing octahedral tilt angles range from 48-51°. In the second Ni site, Ni(2) is bonded to one F(3), one F(4), two equivalent F(1), and two equivalent F(2) atoms to form NiF6 octahedra that share corners with four equivalent Fe(2)O3F3 octahedra, corners with four equivalent Ni(1)O3F3 octahedra, and edges with two equivalent Ni(2)F6 octahedra. The corner-sharing octahedral tilt angles range from 47-51°. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a trigonal planar geometry to two equivalent Nb(1) and one Ni(1) atom. In the second O site, O(2) is bonded in a distorted trigonal planar geometry to two equivalent Nb(1) and one Fe(1) atom. In the third O site, O(3) is bonded in a trigonal planar geometry to two equivalent Nb(2) and one Fe(1) atom. In the fourth O site, O(4) is bonded in a distorted trigonal planar geometry to two equivalent Nb(2) and one Fe(2) atom. In the fifth O site, O(5) is bonded in a trigonal planar geometry to one Nb(1) and two equivalent Fe(1) atoms. In the sixth O site, O(6) is bonded in a distorted trigonal planar geometry to one Nb(1) and two equivalent Ni(1) atoms. In the seventh O site, O(7) is bonded in a trigonal planar geometry to one Nb(2) and two equivalent Fe(2) atoms. In the eighth O site, O(8) is bonded in a distorted T-shaped geometry to one Nb(2) and two equivalent Fe(1) atoms. There are four inequivalent F sites. In the first F site, F(1) is bonded in a distorted trigonal planar geometry to one Fe(2) and two equivalent Ni(2) atoms. In the second F site, F(2) is bonded in a trigonal planar geometry to one Ni(1) and two equivalent Ni(2) atoms. In the third F site, F(3) is bonded in a distorted trigonal planar geometry to one Ni(2) and two equivalent Ni(1) atoms. In the fourth F site, F(4) is bonded in a distorted T-shaped geometry to two equivalent Fe(2) and one Ni(2) atom.
NbFeNi(O2F)2 is Hydrophilite-derived structured and crystallizes in the monoclinic Pm space group. There are two inequivalent Nb sites. In the first Nb site, Nb(1) is bonded to one O(5), one O(6), two equivalent O(1), and two equivalent O(2) atoms to form NbO6 octahedra that share corners with four equivalent Fe(1)O6 octahedra, corners with four equivalent Ni(1)O3F3 octahedra, and edges with two equivalent Nb(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 49-52°. The Nb(1)-O(5) bond length is 2.13 Å. The Nb(1)-O(6) bond length is 1.89 Å. Both Nb(1)-O(1) bond lengths are 2.00 Å. Both Nb(1)-O(2) bond lengths are 2.06 Å. In the second Nb site, Nb(2) is bonded to one O(7), one O(8), two equivalent O(3), and two equivalent O(4) atoms to form NbO6 octahedra that share corners with four equivalent Fe(2)O3F3 octahedra, corners with four equivalent Fe(1)O6 octahedra, and edges with two equivalent Nb(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 47-53°. The Nb(2)-O(7) bond length is 2.13 Å. The Nb(2)-O(8) bond length is 1.90 Å. Both Nb(2)-O(3) bond lengths are 2.00 Å. Both Nb(2)-O(4) bond lengths are 2.06 Å. There are two inequivalent Fe sites. In the first Fe site, Fe(1) is bonded to one O(2), one O(3), two equivalent O(5), and two equivalent O(8) atoms to form FeO6 octahedra that share corners with four equivalent Nb(1)O6 octahedra, corners with four equivalent Nb(2)O6 octahedra, and edges with two equivalent Fe(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 47-52°. The Fe(1)-O(2) bond length is 1.99 Å. The Fe(1)-O(3) bond length is 2.15 Å. Both Fe(1)-O(5) bond lengths are 1.96 Å. Both Fe(1)-O(8) bond lengths are 2.14 Å. In the second Fe site, Fe(2) is bonded to one O(4), two equivalent O(7), one F(1), and two equivalent F(4) atoms to form FeO3F3 octahedra that share corners with four equivalent Nb(2)O6 octahedra, corners with four equivalent Ni(2)F6 octahedra, and edges with two equivalent Fe(2)O3F3 octahedra. The corner-sharing octahedral tilt angles range from 47-53°. The Fe(2)-O(4) bond length is 2.01 Å. Both Fe(2)-O(7) bond lengths are 1.94 Å. The Fe(2)-F(1) bond length is 2.08 Å. Both Fe(2)-F(4) bond lengths are 2.12 Å. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(1), two equivalent O(6), one F(2), and two equivalent F(3) atoms to form NiO3F3 octahedra that share corners with four equivalent Nb(1)O6 octahedra, corners with four equivalent Ni(2)F6 octahedra, and edges with two equivalent Ni(1)O3F3 octahedra. The corner-sharing octahedral tilt angles range from 48-51°. The Ni(1)-O(1) bond length is 2.07 Å. Both Ni(1)-O(6) bond lengths are 2.02 Å. The Ni(1)-F(2) bond length is 2.12 Å. Both Ni(1)-F(3) bond lengths are 2.08 Å. In the second Ni site, Ni(2) is bonded to one F(3), one F(4), two equivalent F(1), and two equivalent F(2) atoms to form NiF6 octahedra that share corners with four equivalent Fe(2)O3F3 octahedra, corners with four equivalent Ni(1)O3F3 octahedra, and edges with two equivalent Ni(2)F6 octahedra. The corner-sharing octahedral tilt angles range from 47-51°. The Ni(2)-F(3) bond length is 1.99 Å. The Ni(2)-F(4) bond length is 2.07 Å. Both Ni(2)-F(1) bond lengths are 2.09 Å. Both Ni(2)-F(2) bond lengths are 2.02 Å. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a trigonal planar geometry to two equivalent Nb(1) and one Ni(1) atom. In the second O site, O(2) is bonded in a distorted trigonal planar geometry to two equivalent Nb(1) and one Fe(1) atom. In the third O site, O(3) is bonded in a trigonal planar geometry to two equivalent Nb(2) and one Fe(1) atom. In the fourth O site, O(4) is bonded in a distorted trigonal planar geometry to two equivalent Nb(2) and one Fe(2) atom. In the fifth O site, O(5) is bonded in a trigonal planar geometry to one Nb(1) and two equivalent Fe(1) atoms. In the sixth O site, O(6) is bonded in a distorted trigonal planar geometry to one Nb(1) and two equivalent Ni(1) atoms. In the seventh O site, O(7) is bonded in a trigonal planar geometry to one Nb(2) and two equivalent Fe(2) atoms. In the eighth O site, O(8) is bonded in a distorted T-shaped geometry to one Nb(2) and two equivalent Fe(1) atoms. There are four inequivalent F sites. In the first F site, F(1) is bonded in a distorted trigonal planar geometry to one Fe(2) and two equivalent Ni(2) atoms. In the second F site, F(2) is bonded in a trigonal planar geometry to one Ni(1) and two equivalent Ni(2) atoms. In the third F site, F(3) is bonded in a distorted trigonal planar geometry to one Ni(2) and two equivalent Ni(1) atoms. In the fourth F site, F(4) is bonded in a distorted T-shaped geometry to two equivalent Fe(2) and one Ni(2) atom.