通过氢键构筑的含3-硝基邻苯二甲酸的层状超分子化合物

合成了含大量氢键的层状超分子化合物[C₄H₁₂N₂](HL)₂ (I)和[YL(HL)(H₂O)₃]₂•2H₂O (II) (H₂L＝O₂NC₆H₃- (CO₂H)₂, 3-硝基邻苯二甲酸), 并通过元素分析、红外分析和单晶X衍射表征了组成与结构. 化合物I为双质子化哌嗪阳离子和3-硝基邻苯二甲酸氢根阴离子组成的加合物, 阴离子之间靠强烈的O—H…O氢键形成无限链状结构, 同时阴离子链通过N—H…O氢键与阳离子扩展成网状结构, 相邻的网状结构再由分子间弱作用力构筑成层状超分子. 化合物II则是在双核稀土配合物结构单元通过O—H…O氢键构成的网状结构基础上再进一步由层间弱作用力构筑成的层状超分子化合物. 化合物II的网格结构中, 菱形单元空隙里填充的两个结晶水通过氢键将结点上的双核单元更牢固地结合在一起. 化合物I为单斜晶系, P2₁/c空间群, a＝1.3176(3) nm, b＝1.1096(2) nm, c＝0.75950(15) nm, b＝97.14(3)°, V＝1.1017(4) nm³, Z＝4, μ＝0.129 mm^－1, D_c＝1.533 Mg/m³. 化合物II为三斜晶系, P-1空间群, a＝0.81262(16) nm, b＝0.86942(18) nm, c＝1.5011(3) nm, α＝99.84(3)°, β＝91.26(3)°, γ＝104.55(3)°, V＝1.0091(4) nm³, Z＝1, μ＝2.983 mm^－1, D_c＝1.910 Mg/m³.     

稀土与间硝基苯甲酸三元配合物的合成与光谱表征

本文合成了稀土(RE=Nd,Sm,Tb,Gd)与间硝基苯甲酸(HL)、邻菲罗啉(phen)和稀土(RE=Nd,Sm,Tb,Gd)与间硝基苯甲酸(HL)、2,2-联吡啶(bipy)的三元固体配合物.通过元素分析、摩尔电导、红外光谱、紫外光谱、热分析等手段确定了稀土配合物的组成为REL3phen.nH2O(n=0,1)和REL3bipy.K.nH2O(n=2,4,).并对该类配合物的结构与性质进行了表征.     

稀土与对硝基苯乙酸配合物的合成、表征及荧光性质

本文合成了三种稀土与对硝基苯乙酸 (HL)的二元固体配合物 ,通过元素分析等手段确定了其配合物的组成为ReL3·H2 O(Re=Eu ,Sm ,Tb)。用红外光谱、紫外光谱、荧光光谱对该类配合物的结构与性质进行了表征。红外谱表明配体以—COO- 形式与中心离子配位 ,同时这一点也被自由配体和配合物的UV谱所证实。EuL3·H2 O的强红色荧光分属于Eu3+ 的 5D0 → 7F1 和5D0 → 7F2 跃迁。     

cis-Diaquabis（di-2-pyrimidinyl sulfide- K2N,N） Cobalt（II） Ditetrafluoridoborate： Lone Pair-aromatic and Anion-П Interactions in the Self-assembly of Coordination Complex

The title complex, [Co(DprS)2 (H2O)2]2(BF4)4 (DprS is di-2-pyrimidinyl sulfide), was obtained and characterized by elemental analysis, FT-IR and X-ray crystallography. The complex crystallizes in space group P21/c with a=11.742(1), b=22.439(2), c=20.538(2) , β=109.713(5)°, Z=4, V=5094.3(3)3 , Dc=1.692 g·cm-3 , μ=0.929 mm-1 , F(000)=2600, R=0.0756 and wR=0.1929. The asymmetric unit of the title complex is comprised of two isomeric cobalt(Ⅱ) centers (Co(1) and Co(2)) with a cis-[Co(DprS)2(H2O)2]2+ moiety. Each Co(Ⅱ) center exhibits a similar distorted N4O2-octahedral coordination geometry surrounded by a pair of DprS in a N,N’-chelate mode and two aqua ligands in a cis-relationship. Unconventional S···π(pyrimidinyl), N···π(pyrimidinyl), and anion(BF4-)···π(pyrimidinyl) are found to combine with the C H···F and O H···F interactions to stabilize a whole three-dimensional framework with the mononuclear units (Co(1) and Co(2)). The ligand conformation will be also discussed.     

Layered Lanthanum Complex with 3-Nitrophthalic Acid Assembled via Hydrogen Bonds-Synthesis, Structure and Characterization of [LaL(HL)(H_2O)_3]_2·2H_2O (H_2L=3-NO_2C_6H_3(CO_2H)_2)

A new dinuclear centrosymmetric complex [LaL(HL)(H2O)3]2·2H2O (H2L = 3-nitro- phthalic acid, NPA) was synthesized in water/ethanol solution and characterized by X-ray diffraction, IR spectrum and TGA-DTA. The complex crystallizes in triclinic system, space group P1 with a = 8.1549(16), b = 8.8856(18), c = 15.277(3) , α = 100.93(3), β = 90.81(3), γ = 104.56(3)°, V = 1049.8(4) 3, Z = 1, μ = 2.125 mm-1, Dc = 1.994 g/cm3, R = 0.0259 and wR = 0.0679. Two 3-nitrophthalates(2-) coordinate with the La3+ ions in a bridging mode, and two monohydrogen- 3-nitrophthates(1-) and three waters in terminal ways, respectively. Each La3+ ion is nine- coordinated to exhibit a distorted tricapped trigonal prism coordination polyhedron. Both the coordinated and crystal waters are involved in the inter- and intramolecular hydrogen bonds. The dinuclear units are linked into a 2D network structure in the ab plane via intermolecular hydrogen bonds along the axes a and b. Two crystal waters fill each rhombic pore of the network. The networks are further packed along the c axis forming a layered supramolecular structure through the C–H…O weak forces between the adjacent sheets. TGA analysis shows the complex undergoes the loss of waters of crystallization and coordination and the decomposition of ligands sequentially.     

稀土与桂皮酸、2,2'-联吡啶三元配合物合成、表征及荧光性质

以2,2'-联吡啶(bipy)、桂皮酸(HL)为配体与稀土离子(RE=Tb, Gd, Eu, Sm, Nd)在乙醇溶液中合成了三元稀土配合物. 通过元素分析、摩尔电导、紫外光谱、红外光谱、差热-热重分析, 确定了配合物的组成为REL3·bipy. 并讨论了配合物的谱学性质及EuL3和EuL3·bipy·H2O的荧光性能. EuL3的荧光强度比EuL3·bipy·H2O的荧光强度强4.5倍.