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在甲醇与水的混合溶剂中 ,经浓硝酸硝化的Ho2 O3 与 1,10 邻菲啉反应形成氢氧根桥联的双核钬配合物[Ho2 (phen) 4(H2 O) 4(OH) 2 ](phen) 2 (NO3 ) 4(phen =1,10 邻菲啉 ) .单晶X射线衍射晶体结构测定表明晶体属三斜晶系 ,P 1(no .2 )空间群 ,晶胞参数a =1.12 41(1)nm ,b =1.1439(1)nm ,c =1.40 5 8(1)nm ,α =93.989(7)°,β =98.173(7)° ,γ =10 8.19(1)°,V =1.6 874(4 )nm3 ,Z =1,Dc=1.737g/cm3 ,F(0 0 0 ) =880 ,775 2个独立衍射点中 ,5 70 2个可观测点满足Fo2 ≥ 2σ(Fo2 ) ,R1=0 .0 499,wR2 =0 .0 85 8.标题配合物由中心对称的双核 [Ho2 (phen) 4(H2 O) 4 (OH) 2 ]4 + 配阳离子 ,邻菲啉phen分子及硝酸根NO-3 阴离子组成 .每个稀土原子与 2个邻菲啉配体 ,2个水分子和 2个氢氧根配位形成配位数为 8的 [HoN4 O4 ]四方反棱柱 .配位多面体通过两氢氧根基团形成共棱的 [Ho2 N8O6]双四方反棱柱 [d(Ho—N) =0 .2 5 49～ 0 .2 5 6 5nm ,d(Ho—OH2 O) =0 .2 35 6 ,0 .2 36 6nm ,d(Ho—OOH) =0 .2 2 2 3,0 .2 2 40nm].通过氢键和芳环堆积作用 ,配阳离子和邻菲啉分子排列形成平行于 (10 1)的两维层结构 ,NO-3 阴离子位于层之间 .标题配合物为顺磁物质 ,在 5～ 30 0K区间内遵循Curie Weiss定律 ?
In a mixed solvent of methanol and water, Ho2 O3 nitrated by concentrated nitric acid reacts with 1,10-phenanthroline to form a hydroxide-bridged binuclear holmium complex [Ho2 (phen) 4 (H2O) 4 2] (phen) 2 (NO3) 4 (phen = 1,10-phenanthroline). The crystal structure determination of single crystal X-ray diffraction shows that the crystal belongs to triclinic system, space group P 1 The parameters a = 1.12 41 (1) nm, b = 1.1439 (1) nm, c = 1.40 5 8 (1) nm, α = 93.989 (7) °, β = 98.173 (7) °, ), V = 1.6 874 (4) nm3, Z = 1, Dc = 1.737g / cm3, F (0 0 0) = 880, 775. Among the 2 independent diffraction spots, 5 70 2 observable points satisfy Fo2 ≥ 2σ (Fo2), R1 = 0.0499, wR2 = 0.8585 8. The title complex consists of a centrosymmetric binuclear [Ho2 (phen) 4 (H2O) 4 (OH) 2] 4 + Phenanthroline phen molecules and nitrate NO-3 anions each rare earth atoms with two adjacent phenanthroline ligands, two water molecules and two hydroxide coordination with the formation of 8 [HoN4 O4 ] Tetragonal antipolyposite. The coordination polyhedron forms a rhombic [Ho2N8O6] double tetragonal antiprime [d (Ho-N) = 0.2449 ~ 0.2565nm, d -OH 2 O) = 0 .2 35 6, 0 .2 36 6 nm, d (Ho-OOH) = 0.222 2, 0 .2 2 40nm] .According to the hydrogen bonding and aromatic ring stacking, the cations and phenanthroline molecules are arranged in parallel to form two The layer structure, NO-3 anion is located between the layers.The title complex is paramagnetic material, in the range of 5 ~ 30 0K follow the Curie Weiss law?