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[Ni(hmta)][SSP(OC_(10)H_7-2)_2]_2的合成、谱学性质与晶体结构 被引量:1

Synthesis,spectroscopic properties and crystal structure of [Ni(hmta)][SSP(OC_(10)H_7-2)_2]_2
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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.
出处 《化学研究与应用》 CAS CSCD 北大核心 2006年第2期178-181,185,共5页 Chemical Research and Application
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 tetraazamacrocycle O, 0'- di ( 2 - naphthyl) dithiophosphate acid spectrum crystal structure
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