Single crystals of (NH4)2SnCl6 are obtained by thermal decomposition of SnCl 4·5NH3 in the gas phase under a stream of gaseous NH3 (quartz tube, 298 C, 6 h). The new precursor is formed in the reaction of liquid SnCl 4 with gaseous NH3 at 0 and 25 C. Orthorhombic crystals deposited on the inner wall of the tubular reactor are subjected to single crystal XRD and the lattice parameters are given. A phase transformation to the known cubic (NH 4)2SnCl6 phase (space group Fm3m, Z = 4, powder and single crystal XRD) is observed on the surface of the orthorhombic crystals. Raman spectra of both forms are also given. -(PODSIADLO*, S.; WEISBROD, G.; BIALOGLOWSKI, M.; JASTRZEBSKI, D.; FADAGHI, M.; OSTROWSKI, A.; Cryst. Res. Technol. 50 (2015) 9-10, 764-768, http://dx.doi.org/10.1002/crat.201500054 ; Fac. Chem., Warsaw Univ. Technol., PL-00-664 Warszawa, Pol.; Eng.) -J. Schramke 46-001