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

被引:34
作者
Khan, MI [1 ]
Cevik, S
Doedens, RJ
机构
[1] IIT, Dept Biol Chem & Phys Sci, Chicago, IL 60616 USA
[2] Univ Calif Irvine, Dept Chem, Irvine, CA 92697 USA
关键词
hydrothermal synthesis; crystal structures; vanadyl sulfate;
D O I
10.1016/S0020-1693(99)00153-X
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
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.
引用
收藏
页码:112 / 116
页数:5
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