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1.
合成了一种新的双核倒反中心的稀土镧配合物{La[o-C6H4(NO2)(CO2)]3·(DMF)2}2. 通过元素分析、 核磁共振谱和红外光谱对配合物的组成和结构进行了表征,  用热重分析研究了该配合物的热稳定性,  用X射线单晶衍射法测定了其晶体结构. 镧配合物{La[o-C6H4(NO2)(CO2)]3·(DMF)2}2晶体属三斜晶系, 空间群P1,  晶胞参数a=1.902(2) nm, b=1.245 0(2) nm, c=1.298 7(2) nm, α=64.555(2)°, β=66.348(2)°, γ=71.920(2)°, V=1.569 5(5) nm3, Dc=1.658 Mg/m3, Z=2, μ=1.437 mm-1, F(000)=784. 配合物中有2个La(Ⅲ)被4个邻硝基苯甲酸的羧酸根的负氧离子桥联, 每个La(Ⅲ)的中心离子配位数为9,  配位原子分别来自于7个邻硝基苯甲酸的羧酸根的负氧离子和2个DMF的羰基氧原子. 化合物中的氢键和π…π堆积作用使其成为三维立体结构. 同时发现了标题化合物固体具有光致发光现象, 发光性能测试表明, 配合物具有很好的荧光性质.  相似文献   

2.
以哌嗪为模板剂, 在水热条件下合成了一个新的具有二维拓展骨架结构的稀土硫酸盐[C4N2H12]3[Ce2(SO4)6(H2O)2]·H2O, 并对其进行了结构表征和热分析. 单晶结构解析结果表明, 该化合物晶体属于单斜晶系, P21/c空间群, 晶体学参数a=0.66335(10) nm, b=2.8088(4) nm, c=1.02212(15) nm, β=96.160(2)°, V=1.8935(5) nm3, R1=0.0466, wR2=0.1226. 该化合物由[—Ce—S3—Ce—S1—Ce— S3—Ce—S1—]八元环连接形成二维层状结构, 无机层间通过氢键连接成三维无限结构.  相似文献   

3.
通过三缺位Keggin结构杂多阴离子[α-A-PW9O34]9-和二氯甲基苯基硅烷在乙腈溶液中反应,合成了一例结构新颖的甲基苯基硅衍生物[(C4H9)4N]3[α-A-PW9O34(C6H5SiCH3)3](1),并对其进行元素分析,红外光谱,紫外光谱,热分析和X-射线单晶衍射等表征。该配合物属于三方晶系,空间群为R3m,晶胞参数:a=2.261 3(2)nm,b=2.261 3(2)nm,c=1.797 6(4)nm,V=7.960 2(18)nm3,Z=3。在配合物中,阴离子[α-A-PW9O34(C6H5SiCH3)3]3-呈C3v对称,3个甲基苯基硅基团连接在三缺位的阴离子[α-A-PW9O34]9-表面,整个阴离子显示"开放结构"。  相似文献   

4.
A dinuclear Cd(Ⅱ) complex [Cdz (N3)2LzCl2]2·H2O (1) [L=4'-(4-eyanophenyl)-2,2':6',2"-terpyridine]was synthesized by reaction of ligand L with CdCl2 and NaN3 using solvothermal method and its structure was determined by X-ray crystal structure analysis. The structure indicates that the complex crystallizes in monoclinic, space group C2/c with a=1.644 5(16) nm, b=1.441 9(12) nm, c=1.9181(18) nm,β=100.349(11)°. V=4474(7) nm3, Z=2, Dc=1.570Mg·m-3,μ=1.120 mm-l, F(000)=2 100, and final R1=0.039 3, wR2=0.0811. The result shows a Cd(Ⅱ) ion was sixcoordinated by a tridentate 4'-(4-cyanophenyl)-2,2' :6',2"-terpyridine ligand and one bridging nitrogen atom of the azide group in the basal position and an chloride atom and the other bridging nitrogen atom of the azide group in the axialone, to form a distorted octahedral-pyramidal geometry. CCDC: 673291.  相似文献   

5.
The title complex with benzilic acid and 1,10-phenanthroline monohydrate has been synthesized and characterized in the solvent mixture of water and methyl-alcohol. It falls into the triclinic, characteristic of the space group P1 with a=1.142 8(3) nm, b=1.638 8(4) nm, c=1.645 6(4) nm, α=74.428(5)°, β=84.205(5)°, γ=74.917(5)°, V=2.864 9(12) nm3, Dc=1.347 g·cm-3. Z=2, F(000)=1 216, the reliability factor R1=0.068 9, wR2=0.189 9. The crystal structure shows that the nickel atom is coordinated with six nitrogen atoms from the three phens, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 274184.  相似文献   

6.
[C6N2H18]2[Mo5O15(HPO4)2]·H2O的水热合成与结构表征   总被引:6,自引:0,他引:6  
通过水热法合成了一个新化合物[C6N2H18]2[Mo5O15(HPO4)2]·H2O,并通过IR光谱、ICP、元素分析、差热与热重分析和X射线单晶衍射分析等手段进行了表征.结果表明,晶体属三方晶系,P3(2)21空间群,a=1.1231(1)nm,c=2.2802(5)nm,V=2.4911(7)nm3,Dx=2.835Mg/m3,Z=6,最后的一致性因子R=0.0227,wR=0.0675.阴离子中Mo5O15构成一环状结构,2个HPO4一个连在环的下方,一个连在环的上方,形成类似于“飞碟”状的结构,阳离子为2个质子化的四甲基乙二胺.  相似文献   

7.
(EnH2)2Ge2S6的合成与结构表征   总被引:2,自引:0,他引:2  
用溶剂热方法制备了(EnH2)2Ge2S6单晶.单晶X射线衍射分析结果表明,(EnH2)2Ge2S6属单斜晶系,P2(1)/n空间群,晶胞参数a=0.67125(5)nm,b=1.12290(4)nm,c=1.07518(4)nm,β=92.288(2)°,Z=2.利用DSC及TG分析研究了其热稳定性,结果表明,该化合物在200℃以下能够稳定存在.  相似文献   

8.
于中温水热条件下合成出一种三维亚磷酸铁(H3O)2·[FeⅡ5(HPO3)6], 并对其进行了单晶解析、热重及磁性等系列表征. 晶体属三方(Trigonal)晶系, P3c1空间群, a=1.026 9(5) nm, b=1.026 9(5) nm, c=0.929 5(6) nm, Z=2. 化合物中心铁原子采取略变形八面体构型, 与亚磷酸根假四面体连接形成三维骨架结构, 沿c轴方向有一六元环孔道.  相似文献   

9.
合成了双核银配合物[Ag2(μ-(4-MeC6H4O)2PS2)2(Phen)2](phen为1,10-邻菲咯啉),用元素分析、红外光谱、紫外-可见光谱和热重分析进行了表征,并用X-射线衍射法测定了晶体结构。该晶体属于正交晶系,Pbca空间群,晶胞参数为:a=1.2035(2)nm,b=1.638 3(3)nm,c=2.517 1(5)nm,V=4.963 1(17)nm 3,Dc=1.599 g.m-3,Z=4,F(000)=2 416,μ(Mo Kα)=1.072 mm-1,S=1.066,(Δ/σ)max=0.001,R1=0.037 6,wR2=0.088 8(I>2σ(I))。晶体结构研究表明每个Ag原子与不同配体(4-MeC6H4O)2PS2-的2个S原子和1个phen配体的2个N原子配位形成了具有椅式构型的八元环Ag2S4P2,Ag原子为畸变四面体AgS2N2构型,配合物通过phen的π-π堆积形成了一维结构,分子间的弱氢键C-H…O和C-H…π作用使分子进一步形成了三维网络结构。  相似文献   

10.
合成了新型含能配合物[Mn(DAT)6](ClO4)2(DAT=1,5-二氨基四唑), 用X射线单晶衍射法测定了其晶体结构. 该晶体属三方晶系, P3c1空间群, a=b=1.18435(17) nm, c=1.3081(3) nm, α=β=90°, γ=120°, V=1.5891(5) nm3, Z=2. 该配合物分子结构单元中有1个Mn2+离子、6个DAT分子和2个ClO4-离子. 由6个DAT分子中的6个N原子与中心Mn2+离子配位形成六配位、非中心对称的畸变八面体结构. 利用元素分析、差示扫描量热分析(DSC)、热重-微分热重分析(TG-DTG)等方法进行了表征, 研究了其感度性能. 研究结果表明, 该配合物对外界刺激具有很高的响应性和危险性.  相似文献   

11.
A three-dimensional (3D) cobalt phosphate: Co5(OH2)4(HPO4)2(PO4)2 (1), has been synthesized by hydrothermal reaction and characterized by single-crystal X-ray diffraction, thermogravimetric analysis, and magnetic techniques. The title compound is a template free cobalt phosphate. Compound 1 exhibits a complex net architecture based on edge- and corner-sharing of CoO6 and PO4 polyhedra. The magnetic susceptibility measurements indicated that the title compound obeys Curie-Weiss behavior down to a temperature of 17 K at which an antiferromagnetic phase transition occurs.  相似文献   

12.
The title compound Fe_3(CO)_8(C_6H_5NC)(μ_3-S)_2 (Ⅰ) was synthesized by the reaction of C_6H_5NCS with Fe_3(CO)_12 at room temperature. The crystal and molecular structure of the title compound were determined by single ctystal diffraction method. Crystal data: monoclinic, space group P2_1/C, a=12.718(4)Å, b=26.164(10) Å, c=l3.741(7) Å, β=117.18(2) °, V=4067(2) Å3, Z=8, Dc=1.825 g/cm3. The structure was solved by direct method and difference Fourier synthesis, and refined by full-matrix Least-squares with anisotropic thermal paramaters, using 1990 observed reflections [Ⅰ>3σ(Ⅰ)].The final residual factor was R=0.076, Rw=0.082. The substituted ligand (C_6H_5NC)in Fe_3(CO)_8(C_6H_5NC)(μ_3-S)_2 is connected to the Fe(3) atom of the distorted tetragonal pyramid Fe_3S_2 framework.  相似文献   

13.
The hydrothermal synthesis, crystal structure and some properties of a zinc phosphite with a neutral cluster, [Zn(2,2′-bipy)]2(H2PO3)4, are reported. This compound crystallizes in the triclinic system of space group P-1 (No. 2), a=8.3067(5) Å, b=8.9545(4) Å, c=10.0893(6) Å, α=95.448(2)°, β=99.7530(10)°, γ=103.461(2)°, V=712.23(7) Å3, Z=1. The cluster consists of 4-membered rings formed by alternating ZnO3N2 square pyramids and H2PO3 pseudo pyramids, with two “hanging” H2PO3 groups attached to each of the Zn centers. The clusters are linked together by extensive multipoint hydrogen bonding involving the phosphite units to form a sheet-like structure. This compound represents the first example of zinc phosphite with P---OH bonds. An intense photoluminescence was observed from this compound upon photoexcitation at 388 nm.  相似文献   

14.
采用[(Tp)Fe(CN)3]-(Tp=hydrotris(pyrazolyl)borate)与Mn(Ac)2·4H2O反应,合成了氰根桥联的异金属三核配合物[Mn(phen)2][(Tp)Fe(CN)3]2·5H2O (1)(phen=1,10-phenanthroline),并对其结构和磁性进行了研究。晶体结构分析结果表明该化合物晶体属于三斜晶系,P1空间群。在该配合物中,Mn(Ⅱ)与2个phen分子及2个[(Tp)Fe(CN)3]-配位,形成一种弯曲的三核结构。磁性测量结果表明,Mn(Ⅱ)和Fe(Ⅲ)之间通过氰根桥联产生弱的反铁磁相互作用。  相似文献   

15.
通过在介孔结构金属有机框架材料MIL-101(Cr)和MIL-100(Al)的孔洞中合成自旋交叉化合物[Fe(HB(pz)32]的方法,可以得到SCO@MOF复合物。通过红外光谱(FTIR)、粉末X射线衍射(PXRD)、原子吸收光谱(AAS)以及气体吸附-脱附等进行了进一步测试。通过变温磁测量对复合材料的温度诱导自旋转换行为的研究表明,复合材料的自旋转换行为发生改变甚至是消失了。复合材料的这一现象可以解释为[Fe(HB(pz)32]在MOF主体材料的孔洞中形成了一种新的结晶相,且孔壁压力将会阻碍[Fe(HB(pz)32]从低自旋态向高自旋态转变。不同SCO@MOF复合物得到了相似的自旋转换行为结果。这确认了当自旋交叉化合物在金属有机框架材料孔洞中形成时,MOFs材料的限制压力或基体效应对其自旋转换行为的影响显然是至关重要的。  相似文献   

16.
通过在介孔结构金属有机框架材料MIL-101(Cr)和MIL-100(Al)的孔洞中合成自旋交叉化合物[Fe(HB(pz)32] 的方法,可以得到SCO@MOF复合物。通过红外光谱(FTIR)、粉末X射线衍射(PXRD)、原子吸收光谱(AAS)以及气体吸附-脱附等进行了进一步测试。通过变温磁测量对复合材料的温度诱导自旋转换行为的研究表明,复合材料的自旋转换行为发生改变甚至是消失了。复合材料的这一现象可以解释为[Fe(HB(pz)3)2] 在MOF主体材料的孔洞中形成了一种新的结晶相,且孔壁压力将会阻碍[Fe(HB(pz)32] 从低自旋态向高自旋态转变。不同SCO@MOF复合物得到了相似的自旋转换行为结果。这确认了当自旋交叉化合物在金属有机框架材料孔洞中形成时,MOFs材料的限制压力或基体效应对其自旋转换行为的影响显然是至关重要的。  相似文献   

17.
[Pb2(TNR)2(CHZ)2(H2O)2]4H2O的结构及热分解机理   总被引:1,自引:0,他引:1  
The coordination compound of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O was prepared by using the aqueous solution of carbohydrazide, lead nitrate and sodium styphnate. The molecular structure of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O(C 7H 13 N 7O 12 Pb, Mr=594.43) was determined by using a single crystal diffraction analysis .The thermal decomposition mechanism of the title compound was studied by TGDTG, DSC and IR techniques. The crystal belongs to monoclinic with space group P2 1/n.The unit cell parameters are as follows: a=0.64700(10)nm, b=1.6074(3)nm, c=1.4883(3)nm,β=97.42(2)°,V=1.5349(5)nm3, Z=2, DC=2.572g•cm -3 ,μ(Mo, Kα)=11.080cm -1 , F(000)=1128. R=0.0422, Rw=0.0735. The binuclear lead coordination compound is bridged by two carbohydrazide molecules. The molecule has a symmetrical center. TNR 2- ,CHZ and H 2O coordinate with the central ions simultaneously.  相似文献   

18.
The title compound [C4H12N2] 3 [PMo12O40] was synthesized from the hydrothermal reaction and charac-terized by IR, elemental analysis and X-ray signal crystal structural analysis. The crystal of the title complex belongs to trigonal space group R3c with a=1.788 62 nm, c=2.354 3 nm, and V=6.522 62 nm3, Z=6, R1=0.038 4, wR2=0.102 0. The compound consisted of piperazine and PMo12O403-, and the structure is extended to three dimensional framework owing to the hydrogen bond between the O atoms and N atoms. The bulk-modified carbon paste electrode (APM-CPE) using this compound as modifier shows a good electrocatalytic activity toward the oxidation of ascorbic acid(AA). CCDC: 707968.  相似文献   

19.
王振庆  王成 《应用化学》2011,28(1):77-82
用水热法合成了含三价砷阴离子AsS3-4的化合物[InAsS4(2,2′-bipy)]2。 该化合物晶体为单斜晶系,空间群为P21/c,晶胞参数a=0.89799(9) nm,b=2.1794(2) nm,c=1.43736(14) nm,β=91.274(2)°,V=2.8123(5) nm3。 在此化合物中用金属螯合物[In(2,2′-bipy)]3+稳定了不常见的三价砷阴离子AsS3-4,讨论了金属价态对最终产物结构的影响,并且研究了该化合物的半导体性质(禁带带宽1.35 eV)。  相似文献   

20.
马运声  王君  袁荣鑫 《无机化学学报》2008,24(12):2043-2046
Azide-containing coordination polymers have received considerable attention for the construction of new molecule-based magnets. A three dimensional heteronuclear Mn-Na compound [MnNa(N3)4(C5H5N)4] was obtained by reaction of [Mn3O(O2CCH3)6(py)3]ClO4 and NaN3 in pyridine solvents. The title compound crystallizes in monoclinic space group C2/c, a=1.536 6(2), b=1.045 3(2), c=1.576 3(2) nm, β=90.309(3)°, V=2.531 8(6) nm3, Z=4. In the structure, each Mn3+ and Na+ ion coordinated with four N atoms from four N3- and two N atoms from two pyridine molecules. Each pair of Mn3+ and Na+ ion are linked by N3- bridges into a 3D polymer with PtS topology. CCDC: 706250.  相似文献   

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