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机构地区:[1]浙江师范大学物理化学研究所浙江省固体表面反应重点实验室,浙江金华321004 [2]金华职业技术学院材料与化工学院,浙江金华321017
出 处:《中国稀土学报》2005年第5期641-644,共4页Journal of the Chinese Society of Rare Earths
基 金:浙江省科学技术厅基金资助项目(012061)
摘 要:合成了金刚烷甲酸与稀土Nd(Ⅲ)和La(Ⅲ)离子配合物,并测定了配合物的晶体结构。配合物的组成为[LnL3(HL)(H2O)]2.2EtOH.2H2O(Ln=Nd(1),La(2),HL=金刚烷甲酸)。配合物晶体均属三斜晶系,空间群为P1,晶胞参数:配合物(1)a=1.0556(2)nm,b=1.4913(3)nm,c=1.4920(3)nm,α=106.26(3)°,β=93.51(3)°,γ=97.23(3)°,V=2.2253(5)nm3,Dcal=1.409 g.cm-3,Z=1,F(000)=990,μ(Mo Kα)=1.225 mm-1,Mr=1888.54。配合物(2)a=1.0453(2)nm,b=1.4971(3)nm,c=1.5052(3)nm,α=106.07(3)°,β=93.58(3)°,γ=97.56(3)°,V=2.2391(5)nm3,Dcal=1.397 g.cm-3,Z=1,F(000)=984,μ(Mo Kα)=1.015 mm-1,Mr=1877.88。两个配合物属异质同晶,呈双核结构,Ln(Ⅲ)为九配位,形成畸变三帽三棱柱配位多面体。The title complexes ( LnL3 (HL) ( H2O ) ] 2· 2EtOH·2H2O (Ln= Nd (1), La (2), HL=adamantanecarboxylic acid) were prepared and determined by single-crystal X-ray diffraction. Both complexes crystallize in triclinic system with space group P 1, cell parameters are : complex (1) a=1.0556(2) nm, b=1.4913(3) nm, c=1.4920(3) nm , α=106.26(3)°, β=93.51(3)°, γ= 97.23(3)°, V=2.2253(5) nm3, Dcal=1.409 g·cm^-3, Z=1, F(000)=990, μ(Mo Kα)=1.225 mm^-1, Mr=1888.54. 配合物(2) a=1.0453 (2) a = 1.0453(2) nm, b = 1.4971(3)nm, c = 1.5052(3) nm, α=106.07(3)°, β=93.58(3)°, γ=97.56(3)°, V=2.2391(5) nm^3, Dcal=1.397 g·cm^-3, Z=1, F(000)=984, μ(Mo Kα)=1.015 mm-1, Mr= 1877.88. The final R and wR are 0.0396 and 0. 1062 for 8589 (I ≥ 2σ (I)) observed reflections for complex (1), 0.0505 and 0. 1344 for 8417 (I ≥ 2σ(I)) observed reflections for complex (2), respectively. The crystals are consisted of a binuclear molecule. The coordination geometry of the Ln( Ⅲ ) ion can be described as tricapped trigonal prism.
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