a, b, Experimental versus simulated powder diffraction pattern of LiInP 2 Se 6 scaled to the largest peak (a) and scaled by a factor of 20 (b). The simulated pattern has a March–Dollase parameter of 0.3. The X-ray powder diffraction pattern of LiInP 2 Se 6 in a shows a considerable preference to orientation along \(\langle 0\,0\,1\rangle \), that is, the peaks with the largest intensity correspond to the (0 0 2), (0 0 4) and (0 0 8) planes. This preferred orientation stems from the layered nature of this compound, which causes the layers to lie parallel to the sample holder. The simulated pattern with a March–Dollase parameter of 0.3 was the reference pattern used to compare with the experimental pattern, and accurately accounts for the sample’s preferred orientation. When the patterns are zoomed-in closer to the baseline, the reflections with contributions from the h and k directions can be seen and match well with the simulated pattern (b). c, Experimental versus simulated powder diffraction pattern of LiInP 2 Se 6 obtained using a stoichiometric amount of reagents. The unknown secondary phases are marked by asterisks. d, Sink side of the reaction tube used for CVT with no iodine charged into the tube. e, Sink side of the reaction tube used for CVT with iodine as the transporting agent. This reaction did not employ an initial reverse transport step. f, Experimental versus simulated powder diffraction pattern of LiInP 2 Se 6 grown using CVT. The simulated pattern has a March–Dollase coefficient of 0.3. g, Experimental powder diffraction pattern of bulk LiInP 2 Se 6 before (red) and after (black) DTA up to 760 °C. h, Experimental diffraction pattern of LiInP 2 Se 6 grown by CVT before (red) and after (black) DTA up to 760 °C.