[Na(DB18C6)(CH3CN)]2Mo6O19的合成、晶体结构及谱学表征

A novel super-molecular complex, [Na(DB18C6)(CH₃CN)]₂Mo₆O₁₉, was obtained by solvothermal reaction and characterized by elementary analysis, IR, ¹H NMR, gumbc spectrum and X-Ray diffraction experiment. The compound crystallizes in monoclinic space group P2₁/n with a=1.187 1(3) nm, b=2.096 3(6) nm, c=1.415 8(4) nm, β=110.854(5)° and Z=4. The complex contains four basic units: Na⁺, CH₃CN, DB₁₈C₆和Mo₆O₁₉^2-. Sodium ions located in the cavity of dibenzo-18-crown-6 with 6 Na-O bonds and the crown ether-sodium ion complex is supported on the terminal oxygen atoms of the typical Lindqvist isopolyanion Mo₆O₁₉^2- via the coordinative interactions. Mo₆O₁₉^2- located between two DB₁₈C₆ and led to the formation of the “hamburger” structure. The crystal is stabilized by van der waals force and interaction of π-π system. CCDC: 272936.     

[Na(DB24C8)]3[α-AsMo12O40]·9H2O超分子的合成与晶体结构

The complex of [Na(DB24C8)]₃[α-AsMo₁₂O₄₀]·9H₂O was synthesized by hydrothermal techniques and cha-racterized by IR and X-ray diffraction analysis. Single crystal X-ray diffraction indicate that this complex is belong to monoclinic, space group P2₁/n with cell dimension: a=1.480 3(7) nm, b=2.692 7(3) nm, c=3.046 6(4) nm, α=90.00°, β=95.4120(10)°, γ=90.00°. V=12.090 28 nm³, Z=4, F(000)=6 440.0, R=0.050 9, wR₂=0.113 5. The crown ethers just coordinate with Na⁺ and have no direct interaction with the polyoxometalate, because the crown ethers have a contorted configuration. CCDC: 626686.     

[Zn(DMF)6]H2SiW12O40·(CH3)2NH的合成,晶体结构及性质

The title compound [Zn(DMF)₆]H₂SiW₁₂O₄₀·(CH₃)₂NH was synthesized in mixed solvent of aqueous and acetonitrile, and its crystal structure had been determined using single crystal X-ray diffraction. The crystal belongs to monoclinic, space group C2/m, a=2.0654(4)nm, b=1.3306(3)nm, c=1.3194(3)nm, β=119.59(3)°, V=3.1531(11)nm³, D_c=3.606Mg·m^-3, Z=2, R=0.0462, R_w=0.0836. The title compound comprises of a [Zn(DMF)₆]²⁺ unit, a polyanion and a free (CH₃)₂NH molecule. The ESR spectrum of the title compound shows that charge-transfer between organic groups and polyanion takes place under irradiation of the sunlight in solid state. The TG study of the title compound shows that it had four stages of the weight loss, and the increase of the de-composition temperature for the polyanion shows that the stability of the polyanion was enhanced due to the influence of Zn²⁺ ion. CCDC:175866.     

三维超分子化合物[H2bbi]3[α-PMo12O40]2的水热合成与晶体结构

利用水热技术合成了一个以Keggin型多金属氧酸盐和柔性有机配体为建筑块的三维超分子化合物[H2bbi]3[α-PMo12O40]2(1)(bbi=1,4-双-(咪唑-1-基)丁烷),用X-射线单晶衍射、元素分析、红外光谱和X-射线粉末衍射对晶体结构进行了表征.X-射线单晶衍射显示,该晶体属于三斜晶系,P-1空间群,a=1.183 60(9)nm,b=1.209 32(10)nm,c=1.77728(15)nm,α=74.089 0(10)°,β=70.949 0(10)°,γ=71.816 0(10)°,V=2.242 1(3)nm3,Z=2,Dc=3.109g/cm3,F(000)=2 300,μ=3.39mm-1,S=1.047,R1=0.035 0,wR2=0.077 6[I>2σ(I)].     

K3Na5(H2NCH2CH2NH3)2{(VO)12O6[B3O6(OH)]6}(H2O)•12H2O的合成与晶体结构

利用水热合成技术成功制备出一种新型多钒硼氧化合物， 用X射线单晶衍射分析技术对其晶体结构和分子结构进行了确定。结果表明在该化合物中多钒硼氧阴离子具有一个新颖的三明治结构。上下两个结构单元都是由六个VO₅四角锥交替地通过顺式和反式共边的方式连接起来构成的一个钒氧三角形结构。中间的结构单元是由BO₃平面三角形和BO₄四面体以共角的方式相互连接形成的一个折叠型的B₁₈O₃₆(OH)₆环。三明治结构中层与层之间通过桥氧相连。一个水分子处于它的核心位置上，与每个VO₅四角锥中的钒原子都保持几乎相等的距离。该化合物及其晶体中存在着丰富的化学结构和成键信息，同时也有作为氧化还原反应催化剂的潜能。     

Ln(NO3)3·C26H38N2O4(Ln=La、Ce)配合物的合成和La(NO3)3·C26H38N2O4·CH3CN的晶体结构

合成了2个新的希土冠醚配合物Ln(NO₃)₃·C₂₆H₃₈N₂O₄(Ln=La、Ce; C₂₆H₃₈N₂O₄=1, 7, 10, 16-四氧-4，13-二氮杂-N，N′-二苄基环十八烷)。通过元素分析，红外光谱，拉曼光谱及其 ¹H核磁共振谱进行表征。用四圆衍射仪测定了La(NO₃)₃·C₂₆H₃₈N₂O₄·CH₃CN的晶体结构。晶体属三斜晶系，P1空间群，晶胞参数：a=1.2869(4) nm, b=1.5868(6) nm, c=0.9147(2) nm; α=101.89(2)°, β=105.38(2)°, γ=71.96(3)°; Z=2。d_cald.=1.58 g·cm^-3, μ(MoKα)=13.25 cm^-1。中心镧离子与冠醚配体中的4个氧原子和2个氮原子配位，3个硝酸根中的6个氧原子也与La³⁺配位，形成配位数为12的配合物。     

配合物[Ce(CH2=C(CH3)COO)2(NO3)(Bipy)]的合成及晶体结构

The new complex [Ce(CH₂=C(CH₃)COO)₂(NO₃)(Phen)]₂ was prepared in ethanol-aqueous solution with 8-hydroxyquinoline as the acidity regulator. Its crystal structure was determined by X-ray diffraction analysis. The title complex is triclinic, space group P1, a=1.00832(3)nm, b=1.02858(8)nm, c=1.12350(8)nm, α=113.9250(10)°, β=103.8210(10)°, γ=81.4650(10)°, V=1.03252(14)nm³, Z=1, D_c=1.700g·cm^-3, F(000)=522. The coordination number of Ce³⁺ is nine. CCDC: 211278.     

四元混配配合物[Ce(CH2=C(CH3)-COO)2(NO3)(phen)]2的合成、表征及晶体结构

A new complex with mixed-quadriligand [Ce(CH₂=C(CH₃)-COO)₂(NO₃)(phen)]₂ has been synthesized in aqueous solution of slight acidity and characterized by elementary analysis, IR and TGA. The crystal structure determination shows that the complex belongs to triclinic, space group P1, a=9.614?, b=10.047?, c=11.821?, Z=2, α=100.88(3)°, β=106.29(3)°, γ=97.93(2)°, V=1054(5)?³, D_c=1.741g·cm^-3, F(000)=546.00, μ(MoKα)=22.06cm^-1. And the crystal is consisted of a binuclear molecule. The coordina-tion of Ce³⁺ is nine.     

[NH3(CH2)5NH3][Fe2{O3PC(CH3)(OH)(PO3H)}2]·2H2O:一个新的二膦酸亚铁化合物的合成、结构与性质研究

通过水热合成得到一个新的有机二膦酸亚铁化合物[NH₃(CH₂)₅NH₃][Fe₂^Ⅱ{O₃PC(CH₃)(OH)(PO₃H)}₂]·2H₂O,该化合物包含阴离子型共价双链[Fe₂^Ⅱ{O₃PC(CH相似文献   

超分子化合物[M(4，4′-bipy)2(H2O)4·(4，4′-bipy)2·(3，5-diaba)2·8H2O](M=Co，Ni，Cd)的合成及晶体结构

合成了3个超分子化合物[M(4，4′-bipy)₂(H₂O)₄]·(4，4′-bipy)₂·(3，5-diaba)₂·8H₂O(M=Co (1)，Ni (2)，Cd (3)；4，4′-bipy=4，4′-联吡啶；3，5-diaba=3，5-二氨基苯甲酸阴离子)，用红外光谱、元素分析及X-射线单晶衍射进行了表征。3个化合物的晶体都属于单斜晶系，空间群为P2/c。晶体学参数：化合物1：a=0.938 9(2) nm，b=0.775 1(1) nm，c=3.928 4(6) nm，β=90.14(2)°，V= 2.858 80(69) nm³，Z=4，D_c=1.397 g·cm^-3，F(000)=1 266，μ=0.380 mm^-1，R₁=0.034 9,wR₂=0.082 9;化合物2:a=0.938 3(2) nm,b=0.775 3(1) nm，c= 3.921 8(6) nm，β=90.09(1)°，V=2.852 80(68) nm³，Z=2，D_c=1.399 g·cm^-3，F(000)=1 268，μ=0.420 mm^-1，R₁=0.036 6，wR₂=0.080 5；化合物3：a=0.940 91(13) nm，b=0.778 85(11) nm，c=3.971 2(5) nm，β=90.10°，V=2.910 2(7) nm³，Z=2，D_c=1.433 g·cm^-3，F(000)=1 308，μ=0.454 mm^-1，R₁=0.046 8，wR₂=0.096 4。3，5-diaba未参与配位，在配位阳离子[M(4，4′-bipy)₂(H₂O)₄]²⁺中，金属离子M(II)与来自2个4，4′-bipy的2个氮原子和4个水分子的氧原子配位，呈八面体的几何构型。分子中还存在未配位的4，4′-bipy。通过配位阳离子、游离4，4′-bipy及未配位的3，5-diaba间的丰富氢键，构建成具有三维结构的超分子化合物。     

配合物[La(pic)3(phen)2]·CH3CN的合成及晶体结构

The Lanthanum picrate complex with 1,10-phenanthroline was synthesized, whose chemical formula can be written in [La(pic)₃(phen)₂]·CH₃CN. The crystal Xray diffraction analysis shows that crystal belongs to monoclinic with space group P2₁/a and unit cell parameters:a=17.072(4),b=16.083(4),c=17.789(4),β=106.34(2)°,V=4687(4)³, Z=4,Dc=1.735g·cm³, μ=10.106cm¹,F(000)=2448,R=0.0589,Rw=0.0589. The coordination number of La³⁺ is nine. Acetonitrile, a solvent molecule is not coordinated. Between three Pic ligands, that possesses 2 bidentate forms six member ring with La. The other is unidentate ligand. As usually, phen is bidentate ligand.     

六钨酸盐为模板的三维网状超分子化合物[La2(DNBA)4(DMF)8][W6O19]的合成和晶体结构

A new three-dimensional (3D) lanthanide-aromatic monocarboxylate dimer supramolecular network [La₂(DNBA)₄(DMF)₈][W₆O₁₉] (DNBA=3,5-dinitrobenzoate, DMF=dimethylfomamide) was synthesized using hexatungstate anion (W₆O₁₉^2-) as template. The crystal structure of the title compound has been determined by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a=1.334 54(18) nm, b=1.387 52(19) nm, c=1.426 06(19) nm, α=102.189(2)°, β=101.023(2)°, γ=116.349(2)°, V=2.187 2(5) nm³, D_c=2.364 g·cm^-3, Z=1, F(000)=1 453.40. The single crystal structure reveals that two La(Ⅲ) ions are bridged by four 3,5-dinitrobenzoate anions as asymmetrically bridging ligands, leading to dimeric cores, [La₂(DNBA)₄(DMF)₈]²⁺; [La₂(DNBA)₄(DMF)₈]²⁺ groups are joined together by π-π stacking interaction between the aromatic groups to form a two-dimensional grid-like network; the 2D supramolecular layers are further extended into 3D supramolecular network with a 1D box-like channels by hydrogen bonding interactions, in which hexatungstate polyanions reside. CCDC: 284694.     

超分子化合物{[8-hydroxyquinolineH]44+·[SiW12O40]4-·2H2O}的水热合成、晶体结构及热稳定性

A supermolecular compound, {[8-hydroxyquinolineH]₄⁴⁺·[SiW₁₂O₄₀]^4-·2H₂O} was synthesized by hydrothermal reaction with silico-tungstic acid and 8-hydroxyquinoline. The crystal of the compound belongs to monoclinic system, space group P2₁/n, with a=1.282 6(6) nm, b=2.292 7(4) nm, c=2.092 0(6) nm, β=95.495(2)°, Z=4, V=6.124 1(7) nm³, D_c=3.791 g·cm^-3, μ=22.568 mm^-1, F(000)=6 200, R₁=0.029 3, wR₂=0.069 3, GOF=1.079. Su-permolecular compound is composed of one SiW₁₂O₄₀^4- with Keggin structure, four protonated cations of 8-hydroxyquinoline, two hydrones. Thermal analysis results showed that the anionic skeleton construction of heteropoly acid in compound decomposed approximately at 349.0 ℃. CCDC: 622142.     

铜配位聚合物[Cu(C5H6S5)(SCN)]∞的合成和结构研究(英)

The Copper(Ⅰ) supramolecular complexes of 4,5-bis(methylthio)-1,3-dithiole-2-thione (C₅H₆S₅), [Cu(C₅H₆S₅)(SCN)]_∞ 1 and [Cu(C₅H₆S₅)I]_∞ 2, have been prepared and characterized. X-ray structure analysis for complex 1 reveals that the infinite chain structure with polymeric stairs of different lengths is formed through the coordination mode (μ₃) of the thiocyanate bridges. The shorter interchain S…S contacts give rise to a three-dimensional network structure. CCDC: 215668.     

[Ni(en)3]4[HVⅣ12VⅤ6O42(PO4)]复合物的合成及晶体结构

A new complex [Ni(en)₃]₄[HV^Ⅳ₁₂V^Ⅴ₆O₄₂(PO₄)] has been hydrothermally synthesized and characterized by X-Ray diffraction, IR and Elemental analysis. Single crystal X-ray analysis indicates that this compoud crystallizes in cubic system,space group Im 3m with a=17.4081(2)?, V=5275.38(10)?³, R=0.0420, wR=0.1055, Z=2, D_c=1.663g·cm^-3, μ=2.297mm^-1, F(000)=2636. The crystal structure consists of [Ni(en)₃]²⁺ cations and {HV₁₈O₄₂(PO₄)}^8- cluster anion which construct from 18 {VO₅} square pyramids. The VO₅ pyramids joined each other to form a {V₁₈O₄₂} cage hosting a tetrahedral {PO₄}^3- moiety with disordered oxygen atoms. CCDC: 185574.     

一个新的夹心型杂多钨酸盐Na6(C5N2H7){[Na(H2O)2]3Co(H2O)5-[Co(H2O)]3(AsW9O33)2}•27H2O的晶体结构及性质

在pH＝7.5的水溶液中, Na₂WO₄•2H₂O, NaAsO₂, CoCl₂•6H₂O与对氨基吡啶反应, 得到了一种新的夹心型杂多钨酸盐Na₆(C₅H₇N₂){[Na(H₂O)₂]₃Co(H₂O)₅[Co(H₂O)]₃(AsW₉O₃₃)₂}•27H₂O单晶, 用X射线单晶衍射法及元素分析确定了其结构, 晶体属三斜晶系, P 空间群, 其晶胞参数为: a＝1.3276(8) nm, b＝1.7581(10) nm, c＝2.4381(14) nm, α＝70.954(9)°, β＝86.663(9)°, γ＝72.885(9)°, V＝5.136(5) nm³, Z＝2, R₁＝0.0608, wR₂＝0.0848 [I＞2σ(I)]. 在{[Na(H₂O)₂]₃Co(H₂O)₅[Co(H₂O)]₃(AsW₉O₃₃)₂}^7－阴离子中, 一个Co^2＋与聚阴离子{[Na(H₂O)₂]₃[Co(H₂O)]₃(AsW₉O₃₃)₂}^9－的一个端基氧共价连接, Co^2＋呈现出5和6两种配位数, 质子化的氨基吡啶正离子作为抗衡离子存在于晶体之中. 对标题化合物进行了IR, UV-Vis, TG-DSC表征. 对该化合物、Na₂WO₄•2H₂O及CoCl₂•6H₂O催化H₂O₂氧化乙醛的活性进行了比较研究, 该化合物的催化活性远优于简单化合物Na₂WO₄•2H₂O和CoCl₂•6H₂O.     

一个多酸簇合物[Cu4(PPh3)6][Mo8O26]的合成、晶体结构和非线性光学性质

本文报道了一个多酸簇合物[Cu4(PPh3)6][Mo8O26]的合成、X-射线单晶结构分析及IR、XRD表征.单品结构表明中心对称的[Mo8O26]4-是由8个共边的MoO6八面体组成.该化合物具有较好的三阶非线性光学性质,其三阶非线性吸收和折射系数分别为12.9×10-11 MKS和3.13×10-11 esu.     

一个新的夹心型杂多钨酸盐Na6(C5N2H7){[Na(H2O)2]3Co(H2O)5-[Co(H2O)]3(AsW9O33)2}•27H2O的晶体结构及性质

在pH＝7.5的水溶液中, Na₂WO₄•2H₂O, NaAsO₂, CoCl₂•6H₂O与对氨基吡啶反应, 得到了一种新的夹心型杂多钨酸盐Na₆(C₅H₇N₂){[Na(H₂O)₂]₃Co(H₂O)₅[Co(H₂O)]₃(AsW₉O₃₃)₂}•27H₂O单晶, 用X射线单晶衍射法及元素分析确定了其结构, 晶体属三斜晶系, P 空间群, 其晶胞参数为: a＝1.3276(8) nm, b＝1.7581(10) nm, c＝2.4381(14) nm, α＝70.954(9)°, β＝86.663(9)°, γ＝72.885(9)°, V＝5.136(5) nm³, Z＝2, R₁＝0.0608, wR₂＝0.0848 [I＞2σ(I)]. 在{[Na(H₂O)₂]₃Co(H₂O)₅[Co(H₂O)]₃(AsW₉O₃₃)₂}^7－阴离子中, 一个Co^2＋与聚阴离子{[Na(H₂O)₂]₃[Co(H₂O)]₃(AsW₉O₃₃)₂}^9－的一个端基氧共价连接, Co^2＋呈现出5和6两种配位数, 质子化的氨基吡啶正离子作为抗衡离子存在于晶体之中. 对标题化合物进行了IR, UV-Vis, TG-DSC表征. 对该化合物、Na₂WO₄•2H₂O及CoCl₂•6H₂O催化H₂O₂氧化乙醛的活性进行了比较研究, 该化合物的催化活性远优于简单化合物Na₂WO₄•2H₂O和CoCl₂•6H₂O.     

[Pb2(TNR)(NO3)2(H2O)]的制备和晶体结构研究

[Pb₂(TNR)(NO₃)₂(H₂O)] was prepared by reaction of the aqueous solution of lead nitrate and magnesium styphnate. The crystal structure of Pb₂(TNR)(NO₃)₂(H₂O)was determined by single crystal diffraction analysis. The crystal is triclinic, space group P1 with crystal parameters a=0.7279(2)nm,b=1.0698(2)nm,c=1.0738(2)nm;α=86.82(1)°,β=89.52(2)°,γ=83.50(2)°;V=0.8295(3)nm³,Z=2,D_c=3.201g·cm^-3, F(000)=716. The final R value is 0.0358.In the crystal structure, one lead ion was represented by nine coor-dination geometry; the other was showed as ten coordination geometry.     

[CH3NH3][NH3(CH2)6NH3]H3[P2Mo2W16O62]·H2O的水热合成与表征

首次合成了[CH3NH3][NH3(CH2)6NH3]H3[P2Mo2W16O62]·H2O,通过元素分析、红外光谱和X射线单晶衍射对合成产物进行了表征,并用TGA-DSC研究了化合物的热稳定性.晶体属单斜晶系,P21/m空间群,a=1.2596(3)nm,b=1.8715(4)nm,c=1.9816(4)nm,α=γ=90°,β=90.16(3)°,V=4.671(2)nm3,Z=2,Mr=4358.66,Dc=3.100g·cm-3,μ=19.978mm-1,F(000)=3792,R=0.0835,Rw=0.2026.结果表明,在晶体结构内形成了0.7364nm×0.8354nm的微孔.