一种新颖的稀土-2-羟基烟酸的配合物的结构和光谱性质研究

通过水热反应合成了一种新颖的稀土2-羟基烟酸的配合物{[LaL(HL)(H2O)3]1/3(SO4)2/3(H3O)2H2O}(H2L=2-hydroxynicotinic acid)。X-ray单晶衍射分析可知,2-羟基烟酸通过羧基O和羟基O原子桥连La离子,形成二维层状结构,层与层之间通过弱作用力拓展为三维结构。二维相关光谱分析表明N—H面外弯曲振动和C—H面外弯曲振动对磁微扰比较敏感,这可能是吡啶环上π电子云在磁微扰下变形引起C—H和N—H面外弯曲振动的响应,SO24-的ν4振动和羧基不对称伸缩振动对磁微扰也比较敏感;热微扰下N—H伸缩振动比较敏感。此外还对化合物进行了紫外和热重分析。     

Indium(I) Heptachlorodigallate(III), InGa2Cl7

Indium(I) heptachlorodigallate(III), InGa₂Cl₇, has been obtained from a mixture of In, Bi and GaCl₃ in a melt of [bmim][Al(nftb)₄] under argon at 373 K. The crystal structure of InGa₂Cl₇ [orthorhombic, Pna2₁ (no.33), a = 1185.7(2), b = 891.4(4), c = 1071.6(2) pm, V = 1132.6(3)·10⁶ pm³, Z = 4, T = 298 K, R₁ for 1994 reflections with I₀>2σ(I₀): 0.0692] contains discrete indium(I) cations and Ga₂Cl₇ anions. InGa₂Cl₇ crystallizes isotypic with Ga₃Cl₇ and KGa₂Cl₇. In^I is coordinated by ten chloride anions in an irregular (4+6) mode. No evidence was found for the stereochemical activity of the In‐5s² electron pair.     

Indium(I) Tetraiodoaluminate,InAlI4

Indium(I) tetraiodoaluminate, InAlI₄, was obtained from the respective molar amounts of In, InI₃ and AlI₃ at 553 K. The crystal structure [monoclinic, P2₁/m (no. 11), a = 713.5(4), b = 1182.2(3), c = 1108.3(6) pm, β = 96.32(6)°, V = 1013.2(8)·10⁶ pm³, Z = 4, R₁ for 981 reflections with I₀>2σ(I₀): 0.0404] contains discrete indium(I) cations and tetraiodoaluminate anions. No evidence was found for a stereochemical activity of the In‐5s² electron pair. InAlI₄ (Person code mP24) represents a new structure type within the ABX₄ structure family.     

Crystal Structure of the B‐type Dierbium Oxide ortho‐Oxosilicate Er2O[SiO4]

The crystal structure of B‐type Er₂O[SiO₄] has been determined by single crystal X‐ray diffraction. It crystallizes with the (Mn,Fe)₂[PO₄]F type structure in the monoclinic space group C2/c (a = 14.366(2), b = 6.6976(6), c = 10.3633(16) Å, ß = 122.219(10)°, Z = 8) and shows anionic tetrahedral [SiO₄]^4– units and non‐silicon‐bonded O^2– anions in distorted [OEr₄]¹⁰⁺ tetrahedra. The [(Er1)O₆₊₁] and [(Er2)O₆] polyhedra form infinite chains which are connected by common edges.     

双三苯基锡(Ⅳ)哌嗪荒酸盐的谱学和结构分析

利用三苯基氯化锡和哌嗪荒酸二钠在二氯甲烷中反应,合成了双核有机锡(Ⅳ)配合物双三苯基锡(Ⅳ)哌嗪荒酸盐。研究了该配合物的谱学性质和晶体结构;在该配合物的晶体中,锡原子呈五配位畸变三角双锥构型。