Abstract Single crystals of the new oxochlorotantalate Nd7.33Ta8O28Cl6, could be obtained only by chemical transport reactions (T2 → T1; T2 - 1000 °C, T, = 900 °C) with mixtures of Cl2/TaCl5 as transport agent. NdTaO4 was chosen as the starting material. A direct preparative route to Nd7.33Ta8O28Cl6 from binary and ternary components, however, was not successful. Nd7.33Ta8O28Cl6 , crystallizes in the space group Cmmm with a = 10.3381(8) Å, b = 18.865(1) Å, c - 3.9152(3) A; Z = 1. The structure was refined to R - 4.42%, R w = 2.76%. Main building units are pairs of edge-sharing TaO6 -octahedra which are connected with threefold capped trigonal prisms around Nd. Especially remarkable is one Nd position with an occupation factor of 0.833. The relationship of this new structure type with Nd2Ta2O7Cl2 is considered. Furthermore, we have measured the magnetic susceptibilities of both Nd-compounds in a temperature range from 3,6 to 251,3 K. The results are compared with calculated data.