Solvothermal synthesis and crystal structures of two Thioantimonate(V) compounds with the [SbS4]3- anion acting as a monodentate ligand:: [Mn(C6H18N4)(C6H19N4)]SbS4 and [Mn(C6H14N2)3]2[Mn(C6H14N2)2(SbS4)2]•6H2O

被引:56
|
作者
Schaefer, M [1 ]
Engelke, L [1 ]
Bensch, W [1 ]
机构
[1] Univ Kiel, Inst Anorgan Chem, D-24098 Kiel, Germany
来源
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE | 2003年 / 629卷 / 11期
关键词
thioantimonate; solvothermal synthesis; thermal stability; Raman spectroscopy;
D O I
10.1002/zaac.200300158
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The two novel thioantimonate(V) compounds [Mn(C6H18N4)(C6H19N4)]SbS4 (I) and [Mn(C6H14N2)(3)](2)[Mn(C6H14N2)(2)(SbS4)(2)].6H(2)O (II) were synthesized under solvothermal conditions by reacting elemental Mn, Sb and S in the stoichiometric ratio in 5 ml tris(2-aminoethyl)amine (tren) at 140 degreesC or chxn (trans-1,2-diaminocyclohexane, aqueous solution 50 %) at 130 degreesC. Compound I crystallises in the triclinic space group P (1) over bar, a = 9.578(2), b = 11.541(2), c = 12.297(2) Angstrom, alpha = 62.55(1), beta = 85.75(1), gamma = 89.44(1)degrees, V = 1202.6(4) Angstrom(3), Z = 2, and II in the monoclinic space group C2/c, a 32.611(2), b = 13.680(1), c = 19.997(1) Angstrom, beta = 117.237(5)degrees, V = 7931.7(8) Angstrom(3), Z = 4. In I the Mn2+ cation is surrounded by one tetradentate tren molecule, one protonated tren acting as a monodentate ligand and a monodentate [SbS4](3-) anion yielding a distorted octahedral environment. In II one unique Mn2+ ion is in an octahedral environment of three bidentate chxn molecules and the second independent Mn 21 ion is coordinated by two chxn ligands and two monodentate [SbS4](3-) units leading to a distorted octahedral surrounding. The compounds were investigated and characterized with thermal and spectroscopic methods.
引用
收藏
页码:1912 / 1918
页数:7
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