Fe3NiF6 crystallizes in the triclinic P-1 space group. There are three inequivalent Fe sites. In the first Fe site, Fe(1) is bonded in a linear geometry to two equivalent F(2) atoms. In the second Fe site, Fe(2) is bonded in a square co-planar geometry to two equivalent F(1) and two equivalent F(3) atoms. In the third Fe site, Fe(3) is bonded in a distorted square co-planar geometry to two equivalent F(1) and two equivalent F(2) atoms. Ni(1) is bonded in a distorted octahedral geometry to two equivalent F(1), two equivalent F(2), and two equivalent F(3) atoms. There are three inequivalent F sites. In the first F site, F(1) is bonded in a 3-coordinate geometry to one Fe(2), one Fe(3), and one Ni(1) atom. In the second F site, F(2) is bonded in a 3-coordinate geometry to one Fe(1), one Fe(3), and one Ni(1) atom. In the third F site, F(3) is bonded in an L-shaped geometry to one Fe(2) and one Ni(1) atom.
Fe3NiF6 crystallizes in the triclinic P-1 space group. There are three inequivalent Fe sites. In the first Fe site, Fe(1) is bonded in a linear geometry to two equivalent F(2) atoms. Both Fe(1)-F(2) bond lengths are 1.95 Å. In the second Fe site, Fe(2) is bonded in a square co-planar geometry to two equivalent F(1) and two equivalent F(3) atoms. Both Fe(2)-F(1) bond lengths are 2.08 Å. Both Fe(2)-F(3) bond lengths are 1.98 Å. In the third Fe site, Fe(3) is bonded in a distorted square co-planar geometry to two equivalent F(1) and two equivalent F(2) atoms. Both Fe(3)-F(1) bond lengths are 2.08 Å. Both Fe(3)-F(2) bond lengths are 2.06 Å. Ni(1) is bonded in a distorted octahedral geometry to two equivalent F(1), two equivalent F(2), and two equivalent F(3) atoms. Both Ni(1)-F(1) bond lengths are 2.24 Å. Both Ni(1)-F(2) bond lengths are 2.46 Å. Both Ni(1)-F(3) bond lengths are 2.06 Å. There are three inequivalent F sites. In the first F site, F(1) is bonded in a 3-coordinate geometry to one Fe(2), one Fe(3), and one Ni(1) atom. In the second F site, F(2) is bonded in a 3-coordinate geometry to one Fe(1), one Fe(3), and one Ni(1) atom. In the third F site, F(3) is bonded in an L-shaped geometry to one Fe(2) and one Ni(1) atom.