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New quaternary niobium cluster chlorides corresponding to the general formula ATi[Nb 6 Cl 18 ] (A = K, Rb, Cs, In, Tl) have been synthesized in sealed quartz tubes at 720 °C, starting from stoichiometric amounts of NbCl 5 , niobium metal, TiCl 3 , and ACl (A = K, Rb, Cs), or In or Tl metals. The structures of RbTi[Nb 6 Cl 18 ] and CsTi[Nb 6 Cl 18 ] were determined using single­ crystal X-ray diffraction. RbTi[Nb 6 Cl 18 ] crystallizes in the rhombohedral crystal system, space group R3̄ (no. 148), Z = 3, with lattice parameters: a = 9.163(4), c = 25.014(14) Å (hexagonal setting). The structure refinement converged to R 1  = 0.044 and wR 2  = 0.058 for all data. In this structure, discrete [Nb 6 Cl 18 ] 4- cluster units are linked by Rb +  and Ti 3+  cations, located in a 12-coordinated anticubeoctahedral and octahedral chloride coordination environment, respectively. In contrast, CsTi[Nb 6 Cl 18 ] crystallizes in the trigonal crystal system, space group P3̄1c (no. 163), Z = 2. The lattice parameters were determined to be a = 9.1075(6), c = 17.0017(8) Å. The structure refinement gives the reliability factors R 1  = 0.029 and wR 2  = 0.063 for all data. The structure is built up of discrete octahedral [Nb 6 Cl 18 ] 4-  cluster units, linked by Cs +  and Ti 3+  cations which are located in a distorted hexagonal antiprismatic and octahedral chloride coordination environment, respectively. The structures of the compounds ATi[Nb 6 Cl 18 ] (A = K, In, Tl) were found to be isotypic with RbTi[Nb 6 Cl 18 ], and their unit cell parameters were refined using X-ray powder diffraction analysis.

Synthesis and Crystal Structures of ATi[Nb 6 Cl 18 ] Compounds (A = K, Rb, Cs, In, Tl)