Synthesis and crystal structure of trans-[Ru(NO)(NH3)4SO4]ClO4 and [Ru(NO)(NH3)4SO4][Ru(NO)(NH3)3Cl(SO4)]HSO4•H2O

Abstract

After the addition of the saturated NaClO₄ solution to a solution of trans-[Ru(NO)(NH₃)₄SO₄]HSO₄•H₂O, trans-[Ru(NO)(NH₃)₄SO₄]ClO₄ perchlorate salt (I) is obtained with the yield of ~80%. The heating of trans-[Ru(NO)(NH₃)₄(H₂O)](HSO₄)SO₄ at a temperature of ~220 °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)₄SO₄][Ru(NO)(NH₃)₃Cl(SO₄)]HSO₄•H₂O crystals (II). The single crystal X-ray diffraction method is used to determine the structure of the compounds obtained. For I: space group P2₁/c, a = 6.6949(9) Å, b = 13.7049(19) Å, c = 12.8641(17) Å, β = 101.028(4)°; for II: space group Р2₁/c, a = 14.1304(4) Å, b = 12.4908(3) Å,, c = 11.6264(3) Å, β = 94.1980(10)°.