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本文报道了配体 2 ,2′-对苯二甲硫基二乙酸和过渡金属铜 ( )、钴 ( )、镍 ( )配合物的合成。经元素分析、X射线衍射分析、红外光谱、差热 -热重分析等推算了它们的组成并指认了谱带的归属。对铜 ( )配合物进行了电子顺磁共振谱研究。 相似文献
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我们制得了硫氨酸轮与二苯并-18-冠-6(DBC)的固体络合物,进行了元素分析、X光衍射、红外光谱、紫外光谱和差热、热重分析,对其合成条件及性质进行了一些探讨。 相似文献
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本文报道了配体2,2′-对苯二甲硫基二乙酸和过渡金属铜(Ⅱ)、钴(Ⅱ)、镍(Ⅱ)配合物的合成。经元素分析、X射线衍射分析、红外光谱、差热-热重分析等推算了它们的组成并指认了谱带的归属。对铜(Ⅱ)配合物进行了电子顺磁共振谱研究。 相似文献
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以1,3,5-三羟基苯、新戊二醇、三氯氧磷等为原料,采用简洁、高效的合成路线,通过两步反应合成了新型阻燃剂1,3,5-三(5,5-二甲基-1,3-二氧杂己内磷酸酯基)苯.通过红外光谱、核磁共振氢谱、质谱、元素分析以及热失重分析等对产物结构和热性能进行了表征和研究.热失重分析表明:该阻燃剂起始分解温度为295.26℃ ,在295.26℃ ~343.38℃和350.40℃ ~578.04℃温区迅速炭化;当阻燃剂被加热到681.03℃时,炭残余量高达43.33 %. 相似文献
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合成了通式为(C_(15)H_(15)N_2O_3)_xRE(NO_3)_y(当RE=La~Gd时,x=3,y=6;RE=Tb~Lu,Y时,x=2,y=5)的一个系列十五种五、六硝酸根合稀土(Ⅲ)酸4-[2-(3-硝基-4-甲氧基苯基)乙烯基]-1-甲基吡啶配合物.通过元素分析、紫外光谱、红外光谱、’H核磁共振谱、热重-差热分析、摩尔电导和X射线粉末衍射分析等对各配合物的结构和性质进行了表征.并对影响其组成变化的因素作了初步探讨. 相似文献
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Anew sodium zincosilicate single crystal Na1.0Zn1.62Si1.38O4.84·0.6H2O with size of 0.3mm×0.3mm×0.3 mm was prepared by hydrothermal synthesis method. Powder X-ray diffraction analysis result shows that this compound is a new phase.The compound is stable up to 500℃. The results of ACimpedance measurement shows that its ionic conductivity at 450℃ is 2×10-4S·cm-1 and the activation energy for ionic conduction is 79.64 KJ/mol. 相似文献
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NAD+ is degraded by horse liver alcohol dehydrogenase in a reaction with p-methylbenzyl hydroperoxide, which acts as a pseudo-substrate. An unstable intermediate product (called compound I) is formed, and this is converted into the final product NADX. The reaction can be monitored by capillary electrophoresis. NADX migrates as two well resolved peaks (NADX1 and NADX2), which belong probably to the tautomers of the same substance. The intermediate product, compound I, has the same effective mobility as the conformer NADX2 and it was impossible to separate compound I from NADX2. The spectra taken during the separation show clearly that the “9-min” peak contains different compounds during the course of the reaction and the NADX2 is not identical with compound I. 相似文献
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Pérez-Bustamante JA 《Talanta》1974,21(12):1291-1295
The preparation and spectrophotometric properties of a new type of complex compound of arsenazo I with Pu(IV) in the presence of H2O2 are described. The new compound has a blue colour, derived from a wide absorption band with a maximum at 610 nm. and a corresponding molar absorptivity of 4 × 104 l. mole−1.cm−1. From 2 hr after its preparation this curious new compound undergoes for several days a steady decomposition accompanied by decolorization. The formation of similar peroxy Pu(IV) complexes has not so far been shown to take place with arsenazo III or with any other “arsenazo-type” reagent. 相似文献
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The lack of suitable lignin model compound limits the understanding of the characteristics of lignin, and hence hinders the efficient utilization of this kind of bioresource. A tetramer phenolic lignin model compound composed of 5-5, α-O-4 and β-5 linkages was prepared by a two-step of free radical reaction with hydrogen peroxide/horseradish peroxidase and S2O82- /Fe2+ as the initiator. Compared with enzymatic process, this synthetic process gives a higher yield of 33.8% within a shorter time. HRMS and 13C NMR spectroscopy show that synthesized model compound contains phenylpropane structure linked by 5-5, α-O-4 and β-5 bonds, which can mimic some chemical characteristics of lignin. 相似文献
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Ana S.J. Wery Juan M. Gutierrez-Zorrila Antonio Luque Pascual Roman Martin Martinez-Ripoll 《Polyhedron》1996,15(24):4555-4564
Two tert-butylammonium decavanadate(V) salts with the formulae [(CH3)3CNH3]6[V10O28] · 8H2O (1) and [(CH3)3CNH3]4[H2V10O28] (2), have been synthesized and their crystal structures have been determined by means of single-crystal X-ray diffraction. The crystal structure of compound 1 is stabilized by electrostatic forces and an extensive network of hydrogen contacts involving anions, cations and water molecules. The anions and cations of this compound are arranged in layers perpendicular to the [010] direction following the sequence, cation-anion-cation. In the crystal structure of compound (2), each dihydrogen decavanadate(V) anion is joined to three adjacent polyanions by means of O(6)---H ··· O(4) hydrogen contacts forming layers parallel to the plane (
01) and the hydrophobic groups of the cations are disposed in layers parallel to the anionic sheets. The thermal behaviour of both compounds has been studied. Compound 1 is an octahydrate and its thermal decomposition begins at 70°C with the loss of water of crystallization, while compound 2 is anhydrous and is consequently more stable, with decomposition starting at 200°C. 相似文献
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[Ru3(CO)12]与Lawesson试剂[(MeOC6H4PS2)2]反应,合成、分离并用谱学表征了产物三核钌羰合簇[(μ-H)2Ru3(CO)9(μ3-P)](Ⅰ)和四核钌羰合簇[(Ru4(CO)10(μ3-S)(μ3-PC6H4OMe)](Ⅰ).X射线衍射测定了的晶体分子结构,表明含有1个裸磷原子作为面桥基配体,并具有颇短的Ru-Ru键距,该价电子数为49e的簇合物对氧和水稳定.谱学分析表明,化合物具有四面体型的Ru4簇心,其三角形面上分别具有面桥基μ3-S和μ3-PC6H4OMe基配体. 相似文献
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The new isocyanato carborane anion, [7-O=C=N-7-CB10H12]− was prepared by the reaction of 7-H3N-7-CB10H12 with triphosgene in the presence of triethylamine. The structure of this compound was established by 1H, 11B and 13C NMR as well as IR spectroscopy. The reactivigty of this compound with a series of organic amines was investigated. The resulting ureas were obtained in good to excellent yields. This approach is suitable for development of compounds for use in tumor selective Boron Neutron Capture Therapy (BNCT). 相似文献
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HU Rong-zu +{ ** } YANG De-suo + GAO Sheng-li + ZHAO Feng-qi + CHEN San-ping + CHEN Pei + LUO Yang + ZHAO Hong-an + SHI Qi-zhen +. Department of Chemistry Northwest University Xi′an P. R. China . Xi′an Modern Chemistry Research Institute Xi′an P. R. China 《高等学校化学研究》2004,20(5):624-626
The thermal behavior, mechanism and kinetic parameters of the exothermic first-stage decomposition of the title compound in a temperature-programmed mode were investigated by means of DSC, TG-DTG and IR. The reaction mechanism was proposed. The kinetic model function in differential form, apparent activation energy(Ea) and pre-exponential factor(A) of this reaction are (3/2)(1-a)[-ln(1-a)]1/3, 185.52 kJ/mol and 1017.78 s-1, respectively. The critical temperature of the thermal explosion of the compound is 201.30 ℃. The values of ΔS≠, ΔH≠ and ΔG≠ of this reaction are 72.46 J/(mol · K), 175.1 kJ/mol and 141.50 kJ/mol, respectively. 相似文献
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Bogumil Brzezinski 《Journal of Molecular Structure》1984,118(3-4):311-318
Heteroconjugated NO+H … N NO … H+N and homoconjugated NO+H … ON NO … H+ON intramolecular hydrogen bonds formed in semisalts of mono- and di-N-oxides of N,N′-tetraalkyl-o-xylyldiamines were studied by IR and NMR spectroscopy. All these hydrogen bonds show large proton polarizability. In the case of the heteroconjugated hydrogen bonds the proton transfer equilibrium shifts from compounds 1 to 3 to the left hand side since the interaction of the hydrogen bond with the solvent environment decreases in this series of compounds. With compound 1 the hydrogen bonds are slightly weaker and longer, hence the wavenumber dependence of the intensity of the continuum caused by these hydrogen bonds is slightly changed with compound 1 compared with compound 2. In the case of compound 3 the intensity of the continuum decreases because of increasing screening of the hydrogen bonds. In the series of homoconjugated hydrogen bonds, from compound 4 to 6 the intense continuum vanishes, and only the band of the 0–1 proton transition at 950 cm−1 remains. The vanishing of the continuum is caused by increasing screening of the hydrogen bonds against their solvent environments by bulky groups, and thus, this change demonstrates again that the interaction of the hydrogen bond with large proton polarizabilities is a necessary prerequisite for IR continua to appear. 相似文献
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Wagner J. Barreto Henrique de Santana Flaveli A. S. Almeida Dilson N. Ishikawa Yoshio Kawano 《Journal of Analytical and Applied Pyrolysis》2003,70(2):719-210
The synthesis, characterization, and thermal decomposition of the [Ni(SCN)2(H+SCN)2(4-mepy)2] compound with an octahedral structure in polymeric chain were reported, in which SCN groups form bridges among Ni(II) ions. The compound decomposes in water resulting in a pH<4 solution. The FT-IR spectrum presented doublet bands at 2117; 2128 cm−1, 788; 773 cm−1 assigned to ν(C---N) and ν(C---S) stretching modes, respectively, and δ(SCN) deformation modes at 468; 476 cm−1. The Raman spectrum of the compound presented the ν(C---N) stretching as a strong doublet at 2122; 2128 cm−1, ν(C---S) at 783; 770 cm−1, and δ(SCN) at 468; 477 cm−1. No significant changes were observed in the 4-mepy ligand bands compared with the vibrational frequencies of the pure compound or the compound in aqueous solution 0.2 mol l−1. The crystal UV–vis reflectance spectrum presented two bands centered in 626 and 424 nm tentatively assigned to the d→d type transitions, 3A2g→3T1g and 3A2g→3T1g, for a symmetry close to Oh. The TG curve showed a mass loss between 120 and 200 °C assigned to the loss of the two 4-mepy molecules; from 200 to 265 °C, the loss of the two H+SCN groups; and from 265 to 450 °C, the loss of the two SCN groups that formed the bridges among the nickel atoms. Based on these mass loss data, a mechanism of thermal decomposition for the compound was proposed. 相似文献