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1.
通过离子液体氯化1-苄基-3-甲基咪唑(BenzMeIm-Cl)与PtCl2的反应,合成了配合物(BenzMeIm)2[PtCl4],并用元素分析、红外光谱、紫外-可见光谱、1H NMR、13C NMR和单晶X射线衍射对其进行了表征。单晶X射线分析表明,配合物结构属于P21/c空间群,晶胞参数和结构解析参数为:a=0.981 80(5)nm,b=0.861 47(3)nm,c=0.144 332(7)nm,β=92.480(2)°,V=121.96(1)nm3,R1=0.014 4,wR2=0.038 8。  相似文献   

2.
通过离子液体氯化1-苄基-3-甲基咪唑(BenzMeIm-Cl)与PtCl2的反应,合成了配合物(BenzMeIm)2[PtCl4],并用元素分析、红外光谱、紫外-可见光谱、1H NMR、13C NMR和单晶X射线衍射对其进行了表征。单晶X射线分析表明,配合物结构属于P21/c空间群,晶胞参数和结构解析参数为:a=0.981 80(5)nm,b=0.861 47(3)nm,c=0.144 332(7)nm,β=92.480(2)°,V=121.96(1)nm3,R1=0.014 4,wR2=0.038 8。  相似文献   

3.
2,7-二羟基萘-3, 6-二磺酸二钠盐(Na2H2dhns)与邻菲罗啉在乙醇/水溶液中自组装得到一新的配合物Na3[Na5(dhns)2]·(phen)4 ·2H2O (1),并用CHN元素分析、IR、TGA和X-射线单晶衍射分析进行了表征。晶体属正交晶系, Pna21空间群, a=2.829 85(12) nm,b=1.038 99(14) nm, c=2.259 23(13) nm, V=6.642 6(10) nm3, Z=4, Dc=1.573 g·cm-3, R1=0.050 6, wR2=0.124 0, S=1.05。  相似文献   

4.
大环双核铜(Ⅱ)配合物由N,N′-二甲基-N,N′-二(3-甲酰基-5-氯水杨醛)乙二胺和1,3-丙二胺,与铜(Ⅱ)反应形成的,经过X-射线单晶衍射结果表明:a=0.871 05(16) nm,b=0.957 78(18) nm,c=1.810 4(3) nm,β=100.761(18)°,V=1.483 8(5) nm3,Z=2,Dc=1.762 Mg·m-3,μ=1.85 mm-1,F(000)=796,and final R1=0.061,wR2=0.126。晶体结构表明:两个铜离子位于双核大环中间,与大环的胺、亚胺以及酚羟基的氧进行配位。磁性结果表明配合物为反铁磁性。  相似文献   

5.
标题配合物M=1892.01,单斜晶系,空间群P21/c, a=1.2975(3) nm, b=2.6591(9) nm, c=1.2118(3) nm, β=96.95(1)°, Z=2, Dc=1.577 g/cm3, T=293(2)K。最终的偏离因子R=0.0583。该配合物以二聚体形式存在,通过其中的桥联羧基形成了双核分子。该分子中羧基具有桥联双齿、桥联三齿和单齿三种配位模式,Eu-Eu之间的距离为0.4019(1) nm。在77K下测得配合物中Eu(Ⅲ)离子仅有一种格位。 5D07FJ(J=0~2)跃迁光谱说明Eu(Ⅲ)离子格位具有C2对称性。  相似文献   

6.
合成了一种锌配位聚合物{[Zn(H2O)2(L)(phen)]·3H2O}n (1), 其中, H2L=1-氨基-8-萘酚-3, 6-二磺酸并利用元素分析、红外、紫外、荧光、热重和X-射线单晶衍射分析进行了表征。标题配合物属正交晶系, Pnma空间群, a=1.698 90(12) nm, b=0.661 88(11) nm, c=2.480 40(14) nm, V=2.789 1(5) nm3, Z=4, Mr=634.92, Dc=1.512 g·cm-3, R=0.058 6, wR=0.121 4。标题配合物呈现一维链状结构, 链内L2-和phen配体之间存在π-π堆积作用, 链与链之间通过氢键扩展为二维超分子网络。  相似文献   

7.
郭金玉  张建国  张同来 《化学学报》2006,64(16):1693-1699
用水热法以5-硝基间苯二甲酸和吡啶为配体合成并培养了Co(nip)2(py)2(H2O)2的单晶. 对单晶进行了X射线单晶衍射分析、元素分析、傅里叶变换红外光谱分析、差热分析和热重-微商热重分析. 该配合物晶体为单斜晶系, 属于P2(1)/c空间群. 晶胞参数为a=1.1662(3) nm, b=1.7734(4) nm, c=0.6988(2) nm, β=102.46(4)°, V=1.4112(6) nm3, Z=2, Dc=1.585 Mg/m3, μ(Mo Kα)=0.688 mm-1. 所有晶体数据的R因子为: R1=0.1064, wR2=0.1270; 最终R因子[I>2σ(I)]为: R1=0.0467, wR2=0.1008. X射线单晶衍射分析的结果表明, 依靠分子内氢键、分子间氢键、硝基氧之间的弱相互作用以及π-π堆积作用, 配合物分子被连成二维无限平面结构. 根据配合物的热分析结果, 配合物及热分析各阶段残渣的傅里叶变换红外光谱, 我们推测出了配合物的热分解机理.  相似文献   

8.
用水热法以5-硝基间苯二甲酸和吡啶为配体合成并培养了Co(nip)2(py)2(H2O)2的单晶. 对单晶进行了X射线单晶衍射分析、元素分析、傅里叶变换红外光谱分析、差热分析和热重-微商热重分析. 该配合物晶体为单斜晶系, 属于P2(1)/c空间群. 晶胞参数为a=1.1662(3) nm, b=1.7734(4) nm, c=0.6988(2) nm, β=102.46(4)°, V=1.4112(6) nm3, Z=2, Dc=1.585 Mg/m3, μ(Mo Kα)=0.688 mm-1. 所有晶体数据的R因子为: R1=0.1064, wR2=0.1270; 最终R因子[I>2σ(I)]为: R1=0.0467, wR2=0.1008. X射线单晶衍射分析的结果表明, 依靠分子内氢键、分子间氢键、硝基氧之间的弱相互作用以及π-π堆积作用, 配合物分子被连成二维无限平面结构. 根据配合物的热分析结果, 配合物及热分析各阶段残渣的傅里叶变换红外光谱, 我们推测出了配合物的热分解机理.  相似文献   

9.
葛红光   范广  陈三平  高胜利 《化学学报》2006,64(24):2501-2504
在水溶液中合成了离子型配合物[Ni(phen)2(H2O)2][Ni(PDC)2]•7H2O (H2PDC=吡啶-2,6-二甲酸, phen=1,10-菲啰啉). 通过元素分析、红外光谱、单晶X射线衍射以及热重分析对配合物进行了表征. 晶体数据解析表明, 化合物属于三斜晶系, 空间群为P1, a=1.0092(4) nm, b=1.4599(6) nm, c=1.4933(5) nm, α=73.982(2)°, β=78.652(2)°, γ=75.184(3)°, V=2.0256(13) nm3, Z=2, F(000)=1004, μ=1.014 mm-1, R1=0.0538, wR2=0.1493. 配合物中的结晶水分子形成一个(H2O)12水簇, (H2O)12水簇通过氢键连接为二维水网, 最终构成三维超分子网络.  相似文献   

10.
[La(CH2ClCOO)2(NO3)(phen)(H2O)]n的合成和晶体结构   总被引:5,自引:0,他引:5  
合成了混合阴离子配合物[La(CH2ClCOO)2(NO3)(phen)(H2O)]n。配合物经元素分析、IR、DTA-TG和UV等表征。用X射线单晶结构分析解析了标题配合物的晶体结构,三斜,空间群P1,晶胞参数为a=10.533(2)?,b=13.136(3)?,c=7.776(1)?,α=96.59(1)°,β=95.76(1)°,γ=108.42(2)°,V=1003.3(3)?3,Z=2,Dc=1.940 g/cm3, F(000)=572, μ(Mo Kα)=24.36 cm-1。  相似文献   

11.
By replacing Mn in YCa3(MnO)3(BO3)4 with trivalent Al and Ga, two new borates with the compositions of YCa3(MO)3(BO3)4 (M=Al, Ga) were prepared by solid-state reaction. Structure refinements from X-ray powder diffraction data revealed that both of them are isostructural to gaudefroyite with a hexagonal space group P63/m. Cell parameters of a=10.38775(13)Å, c=5.69198(10)Å for the Al-containing compound and a=10.5167(3)Å, c=5.8146(2)Å for the Ga analog were obtained from the refinements. The structure is constituted of AlO6 or GaO6 octahedral chains interconnected by BO3 groups in the ab plane to form a Kagomé-type lattice, leaving trigonal and apatite-like tunnels. It is found that most rare-earth and Cr, Mn ions can be substituted into the Y3+ and M3+ sites, respectively, and the preference of rare-earth ions to locate in the trigonal tunnel is correlated to the sizes of the M3+ ions.  相似文献   

12.
A new ruthenium-rhodium mixed-metal cluster HRuRh3(CO)12 and its derivatives HRuRh3(CO)10(PPh3)2 and HRuCo3(CO)10(PPh3)2 have been synthesized and characterized. The following crystal and molecular structures are reported: HRuRh3(CO)12: monoclinic, space group P21/c, a 9.230(4), b 11.790(5), c 17.124(9) Å, β 91.29(4)°, Z = 4; HRuRh3(CO)10(PPh3)2·C6H14: triclinic, space group P1, a 11.777(2), b 14.079(2), c 17.010(2) Å, α 86.99(1), β 76.91(1), γ 72.49(1)°, Z = 2; HRuCo3(CO)10(PPh3)2·CH2Cl2: triclinic, space group P1, a 11.577(7), b 13.729(7), c 16.777(10) Å, α 81.39(4), β 77.84(5), γ 65.56°, Z = 2. The reaction between Rh(CO)4? and (Ru(CO)3Cl2)2 tetrahydrofuran followed by acid treatment yields HRuRh3(CO)12 in high yield. Its structural analysis was complicated by a 80–20% packing disorder. More detailed structural data were obtained from the fully ordered structure of HRuRh3(CO)10(PPh3)2, which is closely related to HRuCo3(CO)10(PPh3)2 and HFeCo3(CO)10(PPh3)2. The phosphines are axially coordinated.  相似文献   

13.
Two new compounds Pd2Os3(CO)12 , 13 and Pd3Os3(CO)12 , 14 have been obtained from the reaction of with Os3(CO)12 at room temperature. The products were formed by the addition of two and three groups to the Os–Os bonds of Os3(CO)12. Compounds 13 and 14 interconvert between themselves by intermolecular exchange of the groups in solution. Compounds 13 and 14 have been characterized by single crystal X-ray diffraction analyses.Dedicated to Professor Brian F. G. Johnson on the occasion of his retirement – 2005.  相似文献   

14.
The thermal decomposition reactions were determined for [Co(en)3](N03)3 and [Co(en)3(HSO4)3 in a dynamic nitrogen gas atmosphere and vacuo, where en represents ethylenediamine. Data were obtained using thermogravimetry, DTA, thermomagnetic analysis, and mass spectrometry. The dissociation reactions in nitrogen were found to be as follows:
and
In vacuo, the dissociation process for [Co(en)3](N03)3 is the same as in nitrogen. Also, the decomposition of [Co(en)3](HSO4)3 is the same except for the first step which is:
  相似文献   

15.
The magnetic properties of Cu(NH3)4(NO3)2 have been measured at low temperatures. Broad maxima in both the susceptibility and specific heat are observed and are consistent with linear chain behavior of a Heisenberg antiferromagnet, with J/k = 3.9 ± 0.1 K. Long-range order sets in at Tc = 0.15 ± 0.01 K, and the ratio kTc/|J| = 0.038 is the lowest observed as yet for a one-dimensional, S = 1/2 antiferromagnet.  相似文献   

16.
The nitrosation of Na[W(CO)5CN] using amyl nitrite and sulphuric acid in a two phase water— diethyl ether system gives the trinuclear compound W3(μCN)3(NO)3(CO)9. A single crystal X-ray diffraction study showed that the compound contains a nine-membered ring of three tungsten atoms and three bridging cyanide groups. The terminal carbonyl and nitrosyl ligands were not distinguishable.  相似文献   

17.
Electrical conductivities were measured for the ternary systems Y(NO3)3+La(NO3)3+H2O, La(NO3)3+Ce(NO3)3+H2O, La(NO3)3+Nd(NO3)3+H2O, and their binary subsystems Y(NO3)3+H2O, La(NO3)3+H2O, Ce(NO3)3+H2O, and Nd(NO3)3+H2O at (293.15, 298.15 and 308.15) K. The measured conductivities were used to test the generalized Young’s rule and the semi-ideal solution theory. The comparison results show that the generalized Young’s rule and the semi-ideal solution theory can yield good predictions for the conductivities of the ternary electrolyte solutions, implying that the conductivities of aqueous solutions of (1:3 + 1:3) electrolyte mixtures can be well predicted from those of their constituent binary solutions by the simple equations.  相似文献   

18.
The thermolysis of complexes [Co(NH3)6][Fe(CN)6] and [Co(NH3 6]4[Fe(CN)6]3 under an air or hydrogen atmosphere at 200, 350, and 500°C is studied. The composition and properties of thermolysis products are determined. The oxidative thermolysis yields mixtures of oxides of the central metals; the reductive thermolysis yields intermetallic compounds CoFe. The density of the complexes and the specific surface area of the intermetallic compounds are measured. Average particle sizes are calculated. The morphology and dispersion of the powders are dictated by the shape and density of the crystals of the precursor double salts and the thermolysis temperature. The thermolysis chemism in the oxidative and reductive atmospheres is discussed in the context of the nature of the complex anion. Original Russian Text ? S.I. Pechenyuk, D.P. Domonov, D.L. Rogachev, A.T. Belyavskii, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 7, pp. 1110–1115.  相似文献   

19.
X-ray crystallographic analyses of H2Os3(CO)10, H(SC2H5)Os3(CO)10 and (OCH3)2Os3(CO)10 are reported. Although hydrogen atom positions have not been located, the essential isostructural nature of the three commplexes establishes the hydride ligands as bridging two metal atoms, separated by 2.670 Å, with a formal bond order of two; the bridging hydrido- and thiolato-ligands span an osmium---osmium bond of length 2.863 Å and formal bond order one; the two μ-methoxy ligands bridge two metal atoms separated by 3.078 Å which, by simple 18 electron rule counting, has a metal---metal bond order of zero. Some general comments are made on the structures of polynuclear transition metal carbonyls.  相似文献   

20.
Phase equilibria in the Ba3(VO4)2-K2Ba(MoO4)2 and Pb3(VO4)2-K2Pb(MoO4)2 systems have been investigated. In the first system, a continuous series of substitutional solid solutions with the palmierite structure is formed, and in the second one, the polymorphic transition in lead orthovanadate at 100°C restricts the extent of the palmierite-type solid solution to 10–100 mol % K2Pb(MoO4)2. Original Russian Text ? V.D. Zhuravlev, Yu.A. Velikodnyi, A.S. Vinogradova-Zhabrova, A.P. Tyutyunnik, V.G. Zubkov, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 10, pp. 1746–1748.  相似文献   

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