“…According to previous research, the structure of ((CH 3 ) 4 N) 3 Bi 2 Cl 9 exhibits high symmetry (hexagonal, space group = P 6 3 / mmc ), which comprises two isolated face-sharing Bi 2 Cl 9 3– octahedral anionic clusters encompassed by tetramethylammonium cations . Besides, there was no appearance of BiOCl, BiONO 3 , and/or metallic bismuth crystalline phases, confirming the purity of the product. , Interestingly, based on the position of the diffraction peak on the XRD pattern, the ((CH 3 ) 4 N) 3 Bi 2 Cl 9 structure in this study differs from the polychloro-chlorobismuthate structure, (Me 4 N) 3 {[Bi 2 Cl 9 ](Cl 2 )}, in the previous study, where Cl 2 fragments were incorporated into a chlorobismuthate matrix via halogen bonding . Moreover, high-purity ((CH 3 ) 4 N) 3 Bi 2 Cl 9 can be obtained when the DCM/DMF volume ratios are 10/50, 20/40, 30/30, and 40/20 (Figure B).…”