Hydrothermal synthesis and characterization of a new vanadyl sulfate compound:: crystal structure of [V(IV)OSO4(H2O)4]•SO4•[H2N(C2H4)2NH2]

The hydrothermal reaction of a mixture of vanadylacetylacetonate-VO(acac)(2), Na2SO4, piperazine, and diluted H2SO4 at 160 degrees C gives a blue colored solution which yields rectangular blue crystals of [V(IV)OSO4(H2O)(4)]. SO4.[H2N(C2H4)(2)NH2] (1) in a 60% yield. Complex 1 is a new organic-inorganic compound: a vanadyl sulfate cocrystallized with organic species. The structure of 1 consists of layers of [V(IV)OSO4(H2O)(4)] separated by SO42- and doubly protonated piperazine cations [H2N(C2H4)(2)NH2](2+) which are hydrogen bonded with each other. Crystal data for 1: monoclinic, space group P2(1)/c (no. 14), a = 17.1502(10), b = 7.2860(4), c = 12.4448(7) Angstrom, beta = 107.058(10)degrees, V = 1486.7(2) Angstrom(3), Z = 4. The structure was solved by direct methods and least-squares refinement converged at R = 0.0305. (C) 1999 Elsevier Science S.A. All rights reserved.