Single crystals of Bi1.9Cu4V4O16 have been prepared by quenching of CO2-LASER heated samples. They were investigated by X-ray techniques. The compound crystallizes with tetragonal symmetry, space group C54h-I4 /m , a = 9.945(2) Å , c = 2.915(3) Å, Z = 1, and is isotypic to the mineral Hollandite. Bi1.9Cu4V4O16 is the first Hollandite with a statistical distribution of vanadium and copper in the network of octahedra. Calculations of the Coulomb terms of lattice energy led to a distance of bismuth to the lone pair of 1.07 Å. Considering the lone pair as part of the coordination sphere of Bi3+ a square pyramidal polyhedron is obtained.
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