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A new oxofluoride Co 15 F 2 (TeO 3 ) 14 has been prepared by optimized hydrothermal synthesis involving a complex mineralization process. The crystal structure consists of a three-dimensional network of CoO 5 (O,F) octahedra, distorted CoO 5 square pyramids, TeO 3 rigonal pyramids and grossly distorted TeO 3+3 octahedra, which are linked by sharing corners and edges. The Te(iv) lone pairs are accommodated within novel pyritohedron-shaped [(TeO 3 ) 14 ] 28- units. This special framework provides a much larger free space that allows Te atoms to vibrate with a large amplitude, which leads to extremely low lattice thermal conductivity. Magnetic susceptibility data for Co 15 F 2 (TeO 3 ) 14 show antiferromagnetic ordering below 9.6 K with a substantial orbital component to the effective magnetic moment. An S = 3/2 honeycomb-like spin network was carefully analyzed by experimental techniques and first principles calculations.

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Lone-pair self-containment in pyritohedron-shaped closed cavities: optimized hydrothermal synthesis, structure, magnetism and lattice thermal conductivity of Co15F2(TeO3)14