The reaction of oleum (65% SO(3)) with the tetrachlorides of silicon, germanium, and titanium, respectively, led to the complex disulfates Sr(2)[M(S(2)O(7))(4)] (M = Si, Ge), Ba[M(S(2)O(7))(3)] (M = Si, Ge, Ti) and Pb[M(S(2)O(7))(3)] (M = Ge, Ti) if strontium, barium, and lead were used as divalent counter cations. The strontium compounds exhibit the unique tetrakis-(disulfato)-metallate anions [M(S(2)O(7))(4)](4-) with the silicon and germanium atoms in octahedral coordination of two chelating and two monodentate disulfate groups. All of the other compounds display tris-(disulfato)-metallate anions [M(S(2)O(7))(3)](2-) with three chelating disulfate groups surrounding the M atoms. Thermoanalytical investigations on the germanium compounds Sr(2)[Ge(S(2)O(7))(4)] and Ba[Ge(S(2)O(7))(3)] revealed their decomposition in multi-step processes leading to a mixture of BSO(4) and BGe(4)O(9) (B = Sr, Ba), while the thermal degradation of Pb[Ti(S(2)O(7))(3)] yields PbTiO(3). For selected examples, IR data are additionally presented.

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The oxidation of copper, zinc and nickel by N 2 O 5 led, respectively, to turquoise-coloured single crystals of (NO)Cu (NO 3 ) ion is coordinated by six oxygen atoms of monodentate nitrate groups in the form of a tetragonal distorted octahedron. The nitrate groups are connected to further copper

N2O5 is prepared by reaction of fuming HNO3 with P4O10 and directly condensed on the metal powders.

The Unprecedented Tetrakis-(disulfato)-silicate Anion [Si(S 2 O 7 ) 4 ] 4-, Its Germanium Congener [Ge(S2O7)4] 4-, and the Tris-(disulfato)-metallates [M(S2O7)3] 2-(M: Si, Ge, Ti), Stabilized by Divalent Counter Cations B 2+ (B: Sr, Ba, Pb). -The compounds Sr2[M(S2O7)4] (M: Si, Ge), Ba[M(S2O7)3] (M: Si, Ge, Ti), and Pb[M(S2O7)3] (M: Ge, Ti) are prepared by reaction of MCl4 (M: Si, Ge, Ti) and BX (B: Sr, Ba, Pb; X: CO 3 , SO 4 ) with oleum (sealed glass ampules, 100-250°C, 12-14 h). The products are characterized by powder and single crystal XRD, thermal analysis, and IR spectroscopy. Sr2[M(S2O7)4] (M: Si, Ge) crystallize in the monoclinic space group P21/n with Z = 2. Ba[Si(S2O7)3] crystallizes in the orthorhombic space group Pbca with Z = 8, Ba[Ge(S2O7)3] in the orthorhombic space group P212121 with Z = 4, and Pb[Ge(S 2 O 7 ) 3 ] in the triclinic space group P1 with Z = 2. Ba[Ti(S 2 O 7 ) 3 ] and Pb[Ti(S2O7)3] crystallize in the monoclinic space group P21/c with Z = 4. The Sr compounds exhibit [M(S 2 O 7 ) 4 ] 4-(M: Si, Ge) anions with the Si and Ge atoms in octahedral coordination of two chelating and two monodentate disulfate groups. All the other compounds display [M(S2O7)3] 2anions with three chelating disulfate groups. -(LOGEMANN, C.; RIESS, K.; WICKLEDER*, M. S.; Chem. Asian J. 7 (2012) 12, 2912-2920, http://dx.