作者:L. S. Skogareva、N. A. Minaeva、T. V. Filippova
DOI:10.1134/s0036023609090010
日期:2009.9
Simple strontium peroxodisulfate SrS2O8 center dot 4H(2)O was synthesized by the reaction of solid Sr(OH)(2) center dot 8H(2)O taken in 30% excess with an aqueous solution of (NH4)(2)S2O8; simple magnesium peroxodisulfate MgS2O8 center dot 6H(2)O was synthesized by the reaction of an aqueous solution of BaS2O8 with a stoichiometric amount of MgSO4 center dot 7H(2)O. Persulfate ammine complexes [M(NH3)(4)]S2O8 (M = Zn, Cu) were prepared in concentrated aqueous ammonia from [Zn(NH3)(4)](OH)(2), [Cu(NH3)(4)](OH)(2), and an ammoniac solution of (NH4)(2)S2O8. The compounds were characterized by X-ray powder diffraction (pRSA) and vibrational (IR and Raman) spectroscopy. Their stability was studied during storage and in DTA experiments. The [Zn(NH3)(4)]S2O8 structure was solved. Its crystals are orthorhombic, a = 10.5512(8) , b = 12.8039(12) , c = 8.0448(5) , V = 1086(15) (3), Z = 4, space group Pna2(1). The compound is built of [Zn(NH3)(4)](2+) complex cations and S2O (8) (2-) persulfate anions. In a cation, Zn-N bond lengths are within 2.04(2)-2.056(14) . In an anion, the lengths of S(1)-O(4), S(2)-O(5), and O(4)-O(5) bridging bonds are, respectively, 1.676(14), 1.672(16), and 1.465(16) ; the other S-O bond lengths are within 1.409(14)-1.443(12) ; the S(1)O(4)O(5)S(2) torsion angle is 140.8(7)A degrees.