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作 者:黄桂珍[1]
出 处:《闽西职业技术学院学报》2017年第1期116-120,共5页Journal of Minxi Vocational and Technical College
摘 要:利用溶液法制备了稀土元素Sm(Ⅲ)与N,-N′-二乙酸基咪唑内盐(分子式:HOOCCH_2(C_3H_3N_2)+CH_2COO-,缩写HDAM)的配合物{[Sm(trans-DAM)_2(H_2O)_2]NO_3·3H_2O}n(1),即按一定的比例将选择的金属盐及配体溶解在适当的溶剂中,常温下静置、挥发,使配位化合物缓慢结晶析出。经X-射线单晶衍射法测定,该化合物属三斜晶系,P-1空间群,a=8.509(2),b=10.847(2),c=13.440(3),α=81.39(3)°,β=74.79(3)°,γ=79.81(3)°,V=1 171.2(4)~3,Z=2,Dc=1.896 mg/m^3,F(000)=666,R1=0.1068,wR_2=0.285 0。同时,利用红外光谱、紫外-可见光谱和荧光光谱对化合物1进行了结构表征。在化合物的结构中trans-DAM-(i)采取μ4-模式,两羧基均表现为μ_2-η~1:η~2配位;trans-DAM-(ii)中一羧基为单齿μ_1-η~0:η~1连接,另一羧基则未配位。trans-DAM-(i)和(ii)连接Sm(Ⅲ)构成在ab平面的二维层状结构。A new compound {[Sm (trans-DAM)2 (H2O)2]NO3·3H2O}n (1) was synthesized by selecting Sm(NO3)3 and imidazolium-N, N'-diacetate (HDAM) in solvents (H2O) under the pH =3 at room temperature. By X-ray single crystal diffraction method, the compound belongs to triclinic crystal system, space group P-1 (α=8.509(2)A, b=10.847(2)A, c=13.440(3)A, a=81.39(3)°, β=74.79 (3)°, γ=79.81(3)°, V=1171.2(4)A3, Z=2, Dc=1.896 mg/m3, F(000)=666, R,=0.1068, wR2=0.2850). At the same time, compound 1 based on the data from X-ray single-crystal diffraction was discussed. The structures and properties were characterized with the FTIR, UV-Vis DRIS, and fluorescence spectroscopy. In the structure of compound 1, trans-DAM-(i) took the μ4- coordination mode, with coordination mode μ1-η1:η2 at the two ends of carboxyl, while in trans-DAM-(ii) only one carboxyl connected μ1-η1:η2 Compound 1 showed a two dimensional layered structure in the ab plane by connecting trans-DAM-(i), trans-DAn (ii) and Sm(Ⅲ).
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