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The new inorganic misfit layer compound (LaSe) 1.20 (TiSe 2 ) 2  was prepared by high-temperature reaction of the elements. It can be regarded as an intercalate of TiSe 2  with LaSe double layers inserted into every second van der Waals gap of the TiSe 2  sandwiches (stage-2 intercalate). The structure, determined by single crystal X-ray diffraction on the basis of (3 + 1)-dimensional superspace, is described by two interpenetrating, incommensurately modulated subsystems. The first subsystem comprises of paired TiSe 2  sandwiches. Its basic space group is  C [unk](0.5957(4), −0.0004(10), −0.189(4)) and the lattice parameters are  a  11  = 3.556(2) Å,  a  12  = 6.120(2) Å,  a  13  = 17.876(10) Å,  α  1  = 86.71(3)°,  β  1  = 92.93(3)°, and  γ  1  = 90.03(3)°. The second subsystem comprises of LaSe double layers with basic space group  C [unk](1.679(1), 0.001(2), 0.317(6)) and unit cell dimensions  a  21  = 5.969(2) Å,  a  22  = 6.118(2) Å,  a  23  = 17.859(9) Å,  α  2  = 86.69(3)°,  β  2  = 89.33(4)°, and  γ  2  = 90.01(3)°. The two subsystems have the common ([unk],[unk]) plane. Refinement on 1602 reflections with  I  &gt; 2.5 σ ( I ) converged to  R  = 0.126 ( wR  = 0.155) for the average structure. Stacking disorder of TiSe 2  is found corresponding to displacements of the sandwiches along the [unk] 21  axis; in the final structure model 9.9(4)% of TiSe 2  is rigidly shifted by ½ [unk] 11 .

Crystal structure determination of the TiSe 2 -based misfit layer compound (LaSe) 1.20 (TiSe 2 ) 2