Summary.Crystals of (NH3OH)2TiF62H2O have been isolated. The compound crystallizes in the monoclinic system (P21/c, No. 15) with cell parameters of a=6.203(1) , b=10.057(1) , c=7.464(1) , and =110.653(6). Reactions in the system In (OH)3 NH3OHF HF have been investigated. Crystals of (NH3OH)3InF6 were isolated from aqueous solution. The compound crystallizes in the trigonal system (R3c) with a=b=c=7.764(2) , ===97.21(4). The thermal decomposition of both compounds was studied by TG and DSC analysis; the decomposition products were characterized by X-ray powder diffraction.