[Ni(hmta)][SSP(OC_(10)H_7-2)_2]_2的合成、谱学性质与晶体结构  

Synthesis,spectroscopic properties and crystal structure of [Ni(hmta)][SSP(OC_(10)H_7-2)_2]_2

作　　者：谢斌[1] 邹立科[1] 毛治华[2] 洪洲[2] 

机构地区：[1]四川理工学院化学系,四川自贡643000 [2]四川大学分析测试中心,四川成都610064

出　　处：《化学研究与应用》2006年第2期178-181,185,共5页Chemical Research and Application

摘　　要：We reported the synthesis of [Ni（hmta）][SSP(OC10H7-2)2]2(where hmta is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane,and 2-C10H7O-is 2-nathphthyloxy).The complex is characterized by elemental analysis,IR spectra,1HNMR spectra,electronic spectra and TG-DTA thermal analysis,and its crystal structure has been determined.The compound belongs to triclinic system,space group P ī with the following crystallographic parameters:a=7.691（2）,b=10.505（5）,c=17.692（5）,α=105.52（3）°,β=90.09（3）°,γ=103.92（4）°,V=1333.5（8）3,DC=1.377g/cm3,F（000）=582,μ（Mo Kα）=0.631mm-1,Z=1,and final R=0.0752,wR=0.1957 for 2425 observed reflections（I>2σ（I））.The analytical results of crystal structure and spectroscopic properties show that a square planar complex cation [Ni（hmta）]2+ is formed by coordination of four nitrogen atoms of ligand hmta to Ni（Ⅱ）.There isn’t interaction of Ni（Ⅱ） with sulfur atom of (2—C10H7O)2PSS-anion,but there are three N-H…S hydrogen bonds between [Ni（hmta）]2+ complex cation and(2—C10H7O)2PSS-anion in the compound.We reported the synthesis of [ Ni（hmta） ] [SSP（OC10H7 -2）2 ]2 （where hmta is 5,7,7,12,14,14 - hexarnethy1-1,4, 8,11 - tetraazaeyelotetradecane, and 2 - C10 H7O - is 2 - nathphthyloxy）. The complex is characterized by elemental analysis, IR spectra, 1^HNMR spectra, electronic spectra and TG - DTA thermal analysis, and its crystal structure has been determined. The compound belongs to trielinic system, space group P i with the following crystallographic parameters ： a=7. 691 （2）A, b = 10. 505 （5）A, c=17. 692（5）A,α = 105.52（3）°,β =90.09（3）°,γ = 103. 92（4）°V = 1333.5（8）A^3,Dc = 1. 377g/cm^3 ,F（000） = 582,μ（ Mo Kα ） = 0. 631 mm^-1, Z = 1, and final R = 0. 0752, wR = 0. 1957 for 2425 observed reflections （ Ⅰ 〉 2σ（Ⅰ） ）. The analytical results of crystal structure and spectroscopic properties show that a square planar complex cation [ Ni（hmta） ]^2＋ is formed by coordination of four nitrogen atoms of ligand hmta to Ni（ Ⅱ ）. There isnI interaction of Ni（Ⅱ1 ） with sulfur atom of （2-C10H7O）2PSSanion,but there are three N- H…S hydrogen bonds between [Ni（hmta） ]^2＋ complex cation and （2-C10H7O）2PSS＇ anion in the compound.

关 键 词：四氮杂大环O O’-二(2-萘基)二硫代磷酸 光谱 晶体结构 

分 类 号：O614[理学—无机化学]