After the addition of the saturated NaClO4 solution to a solution of trans-[Ru(NO)(NH3)(4)SO4]HSO(4)aEuro cent H2O, trans-[Ru(NO)(NH3)(4)SO4]ClO4 perchlorate salt (I) is obtained with the yield of similar to 80%. The heating of trans-[Ru(NO)(NH3)(4)(H2O)](HSO4)SO4 at a temperature of similar to 220 A degrees C results in a complete removal of coordination water and a partial removal of ammonia molecules. Successive treatment of the thermolysis product with sulfuric and hydrochloric acids yields [Ru(NO)(NH3)(4)SO4][Ru(NO)(NH3)(3)Cl(SO4)]HSO(4)aEuro cent H2O crystals (II). The single crystal X-ray diffraction method is used to determine the structure of the compounds obtained. For I: space group P2(1)/c, a = 6.6949(9) , b = 13.7049(19) , c = 12.8641(17) , beta = 101.028(4)A degrees; for II: space group D 2(1)/c, a = 14.1304(4) , b = 12.4908(3) ,, c = 11.6264(3) , beta = 94.1980(10)A degrees.