【Abstract】 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,D_C=1.377g/cm³,F（000）=582,μ（Mo K_α）=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.更多还原