Abstract A new compound dicetyltrimethylammonium hexafluorotitanium dihydrate, [( n -C 16 H 33 )N(CH 3 ) 3 ] 2 [TiF 6 ]·2H 2 O (compound 1), was hydrothermally synthesized at 150 °C and characterized by single crystal X-ray diffraction, Fourier-transform infrared (FTIR) spectroscopy, elemental analysis, and thermogravimetric analysis. Compound 1 crystallizes in the monoclinic system, space group C 2/ c . It consists of hexafluorotitanium cations [TiF 6 ] 2− , water molecular (H 2 O), and cetyltrimethylammonium ions [( n -C 16 H 33 )N(CH 3 ) 3 ] + , which are connected together by extensive hydrogen bonding.