含有溶剂水分子的硫酸缩氨基硫脲合镍配合物的晶体结构和表征

合成了标题化合物NiCH3N3S]2 SO4·3H2 O ,得到深绿色晶体。晶体属于单斜晶系 ,空间群P2 /m。晶胞参数 :a =0 632 60 ( 3)nm ,b =1 6365 ( 3)nm ,c =0 6961 0 ( 3)nm ,β=99 1 1 ( 3)°,V =0 71 1 5 ( 2 )nm3,Z =4。化合物的晶体结构中包括一个独立的Ni(CH3N3S) 2 ]2 +阳离子 ,一个硫酸根阴离子和三个溶剂水分子。 Ni(CH3N3S) 2 ]2 +的中心镍原子与两个氨基硫脲配体以NiS和NiN键螯合 ,形成一个以NiN2 S2 为中心的四配位的扭曲的平面正方形几何构型。NiS和NiN键长分别为 0 2 1 638( 3)nm和 0 1 90 1 ( 5 )nm。在固体状态下 ,Ni(CH3N3S) 2 ]2 +、未配位的水分子和SO42 - 离子形成三维氢键网络从而使晶体结构稳定。同时 ,用元素分析、红外、紫外光谱和热重分析对化合物结构进行了表征

Crystal Structure and Characterization of Thiosemicarbazone Nickel (Ⅱ) Sulfate Water Containing Complex

The title compound, Ni\ 2SO 4·3H 2O, was synthesized and structurally characterized. It crystallizes in monoclinic, space group P2/m, with M r = 195.55 (C 2H 14N 6NiO 7S 3), a=0.63260(3) nm, b=1.6365(3) nm, c=0.69610(3) nm, β=99.11(3)°, V=0.7115(2) nm 3, Z=4. The structure of the title complex contains an independent cation,\Ni(CH 3N 3S) 2\] 2+, one sulfate anion and three water molecules. Each nickel atom is chelated by two thiosemicarbazide ligands by the bonds of NiS and NiN.The distances of them are 0.21638(5) nm and 0.1901(5) nm respectively. Thus the central nickel(Ⅱ) is four-coordinated and forms a distorted square-planar geometry with the NiN 2S 2 core. In solid state,\Ni(CH 3N 3S) 2\] 2+, uncoordinated water moieties and sulfate anion form three dimensional hydrogen bonds network which stabilizes the crystal structure. The title compound was also examined by elemental analysis, FT-IR, UV and TG-DTA.