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Monomeric tungsten oxo‐aminoalkoxides W(O)(OPri)3(L) [L = O(CH2)nNMe2; n = 2 (dmae, 1) and 3 (dmap, 2 )] were synthesized by alcohol exchange with [W(O)(OPri)4]2 and characterized spectroscopically. 1, 2 and [W(O)(OPri)4]2 were used as precursors for the aerosol‐assisted chemical vapour deposition of WO3 thin films, which were characterized by glancing angle X‐ray diffraction, SEM and transmission‐reflectance measurements. Copyright © 2008 John Wiley & Sons, Ltd. 相似文献
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S. G. Shova I. G. Cadelnic M. Gdaniec Yu. A. Simonov T. C. Jovmir V. M. Meriacre G. Filoti C. I. Turta 《Journal of Structural Chemistry》1998,39(5):747-761
The structure of two trinuclear iron acetates [Fe3O(CH3COO)6(H2O)3]Cl· 6H2O (I) and [Fe3O(CH3COO)6(H2O)3][FeCl4] · 2CH3COOH (II) was determined by X-ray diffraction analysis. Crystals I and II are ionic and belong to the orthorhombic system with parameters a = 13.704(3), b = 23.332(5), c = 9.167(2) Å, R = 0.0355, space goup P21212 for I and a = 10.145(4), b = 15.323(6), c = 22.999(8) Å, R = 0.0752, space group Pbc21 for II. The complex cation [Fe3O(CH3COO)6(H2O)3]+ has a μ3-O-bridged structure typical for trinuclear iron (III) compounds. As shown by Mössbauer spectroscopy, the iron(III) ions are in the high-spin state. In trinuclear cations, antiferromagnetic exchange interaction takes place between the Fe(III) ions with the exchange parameter J = -26.69 cm?1 for II (Heisenberg-Dirac-Van Vleck model for D3h, symmetry). 相似文献
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Wang Shutao Wang Enbo Hou Yu Li Yangguang Wang Li Yuan Mei Hu Changwen 《Transition Metal Chemistry》2003,28(6):616-620
A novel organic/inorganic hybrid molybdenum phosphate, [NH3(CH2CH2)2NH3]3[NH3(CH2CH2)2NH2]Na5-[Mo6O12(OH)3(PO4)(HPO4)3]2·4H2O (1), involving molybdenum presented in V oxidation, has been hydrothermally prepared and characterized by elemental analysis, i.r., u.v.–vis., x.p.s., t.g. and single crystal X-ray diffraction. The structure of the title compound (1) may be considered to consist of two [Mo6O12(OH)3(PO4)(HPO4)3] units bonded together with NaO6 octahedra, forming dimers. Further, these dimers connect with each other through four Na+ cations as bridges, giving rise to novel one-dimensional chain-like skeleton. Piperazines exist among inorganic chains acting as charge balancing cations. 相似文献
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利用水热法首次合成了具有两种配位环境Cd原子的新型杂多蓝化合物[NH3(CH2)2NH3]5[Cd(H2O)][CdMoV12O30(HPO4)6(H2PO4)2]·5H2O.通过元素分析、ICP、TG和X射线单晶衍射确定了其组成,使用IR和EPR进行了结构表征.通过N2吸附脱附测定了比表面积和孔径,为催化研究提供了基础数据.结果表明:该晶体为三斜晶系,P-1空间群;晶胞参数a=1.200 2(2)nm,b=1.465 1(3)nm,c=2.119 2(4)nm,V=3.5642(12)nm3,β=83.01(3)°,Z=2,F(000)=293 2,R1=0.0300,wR3=0.071 6. 相似文献
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Oxo-phosphoraneiminato Complexes of Molybdenum and Tungsten. Crystal Structures of [Mo(O)2(NPPh3)2] and [WO(NPPh3)3]2[W6O19] The dioxo-phosphoraneiminato complexes [Mo(O)2(NPPh3)2] ( 1 ) and [W(O)2(NPPh3)2] ( 2 ) originate from hydrolysis of the nitrido complexes [MN(NPPh3)3] (M = Mo, W). They form colourless crystals, which are characterized by IR and NMR spectroscopy as well as by mass spectrometry. According to the crystal structure analysis of 1 (space group Fdd2, Z = 8; lattice dimensions at –83 °C: a = 1953.3(1), b = 3275.8(3), c = 953.4(1) pm) there are monomeric molecules with tetrahedrally coordinated molybdenum atoms. The distances MoO of 171.2 pm and MoN of 185.9 pm correspond to double bonds. In dichloromethane solution 2 undergoes further hydrolysis with colourless crystals of [WO(NPPh3)3]2[W6O19] ( 3 ) originating, which are characterized crystallographically (space group Pbcn, Z = 4; lattice dimensions at –50 °C: a = 3225.1(6), b = 1803.6(3), c = 1811.9(3) pm). 3 consists of cations [WO(NPPh3)3]+ with tetrahedrally coordinated tungsten atoms and of the known [W6O19]2– anions. The tungsten atoms of the cations show distances WO of 171.8 pm and WN of 182 pm which correspond to double bonds as in 1 . 相似文献
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Combination of 2-aminoethanethiol hydrochloride and HgI2 in water in the presence of a base yielded a cyclic molecular structure, [Hg4I4(SCH2CH2NH2)4] (1). For the same reaction in the absence of the base, a similar structure with protonated amines was expected; however, polymeric [Hg4I8(SCH2CH2NH3)2]n.nH2O2 was formed instead. The structures are quite variable despite similar reaction conditions. For instance, there is an additional Hg-N interaction in 1 due to the use of base. The environment around tetracoordinate Hg in 1 is comprised of S, N, and I atoms, with the ligand forming a five-membered chelate and the I atoms present alternate to each other. In the repeating unit of 2, three independent types of Hg atoms are observed, with HgSI3, HgS2I2, and HgI4 bonding environments that have both bridging and terminal I atoms. A simple mechanistic pathway for the formation of 1 and 2 is proposed that includes the presence of three- and four-coordinate Hg intermediates in the solution. Intermolecular hydrogen bonding involving N, I, and S in 1 and N, I, and O atoms in 2 create extended three-dimensional networks. The shortest Hg... Hg distances are found to be intrachain in the range 3.938-3.962 A and indicate no interaction between these atoms. The solution studies (UV-vis and NMR) along with solid-state (IR, Raman, and X-ray) studies for 1 and 2 confirm retention of the structural configuration in the solution. The thermal study of 2 indicates that degradation of the complex occurs in a single step, in contrast to 1, which takes a more complicated decomposition pathway. 相似文献
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Novel polyoxometalate-based organic-inorganic hybrid [NH3-CH(CH3)COOH][H3O]8[PMo12O40]3.4NH3CH(CH3)COO was synthesized and characterized by 31P, 1H, 13C NMR and IR spectroscopies, elemental analysis and single crystal X-ray determination. Two of the PMo12O40 3? anions in the title hybrid are symmetrically equivalent. They are crystallographically independent from the third PMo12O40 3? polyoxoanion, in the case of various interactions with neighboring components in the crystal network (i.e. +NH3-CH(CH3)-COOH and H3O+ cations, +NH3CH(CH3)COO? zwitterions and polyoxoanions). The compound crystallizes in an orthorhombic C222 space group with a = 16.0392(16) Å, b = 34.480(4) Å, c = 12.8968(13) Å and Z = 2. 相似文献
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Harben SM Mosselmans JF Ryan ÁT Whitwood AC Walton PH 《Dalton transactions (Cambridge, England : 2003)》2012,41(1):208-218
We report the syntheses of imprinted polymers using iron-oxo-hydroxo clusters as templates. Three new iron clusters, [Fe(6)O(2)(OH)(2)(O(2)CC(Cl)=CH(2))(12)(H(2)O)(2)] (1), [{Fe(O(2)CC(Cl)=CH(2))(OMe)(2)}(10)] (2) and [Fe(6)O(2)(OH)(2)(O(2)C-Ph-(CH)=CH(2))(12)(H(2)O)(2)] (3) have been prepared from commercially-available carboxylic acids. Cluster-imprinted-polymers (CIPs) of 1, 2 and 3 were prepared with ethylene glycol dimethacrylate monomer, and of 1 with methyl methacrylate monomer. The imprinted sites within the CIPs were examined using EXAFS and diffuse reflectance UV/vis spectroscopy, demonstrating that the clusters 1, 2 and 3 were incorporated intact within the polymers. Extraction of the clusters from the CIPs imprinted with 1 and 3 gave new polymers that showed evidence of an imprinting effect. 相似文献
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Masahiro Yuki Masaaki Okazaki Shinji Inomata Hiroshi Ogino 《Angewandte Chemie (International ed. in English)》1998,37(15):2126-2128
Thermal and photochemical interconversion occurs between the isomeric pair of tetrathiotungstate [WS4]2− clusters 1 and 2 , which were formed by thermolysis of [Cp*2Ru2S4] and [W(CO)3(MeCN)3] [Eq. (1)] and then structurally characterized. During synthesis, a dramatic redistribution of ligands between the Ru and W atoms takes place without the loss of any CO and S ligands. 相似文献