Crystal Structure and Characterization of a Large Polyoxotungstate (NH4)21{La(H2O)5[Ni(H2O)]2As4W40O140}·53H2O

The heteropolytungstate (NH4)₂₁{La(H₂O)₅[Ni(H₂O)]₂As₄W₄₀O₁₄₀}·53H₂O is obtained by the reaction of Na₂₇[NaAs₄W₄₀O₁₄₀]· 60H₂O with NiCl₂·6H₂O, La(NO₃)₃·6H₂O and NH₄Cl at pH‐4.5. The structure and chemical composition are determined by X‐ray diffraction analysis and elemental analysis. The crystal data and main structure refinement are a = 1.9551(3) nm, b = 2.4156(4) nm, c= 3.7068(6) nm, β = 91.505(3)°, V = 17.500 (5) nm³, monoclinic crystal system with space group P2₁/n, Z = 4, R₁ = 0.0573, wR₂ = 0.0717 [I >2<s?(I)], R₁, = 0.2463 and wR₂ = 0.1199 (all data). [La(H₂O)₅] {Ni(H₂O)}₂AS₄W₄₀O₁₄₀ has C₂, symmetry. IR spectra of the ligand [NaAs₄W₄₀O₁₄₀]^27‐ and its three complexes were discussed.     

多功能沸点仪的研究

本文提出了两种新型沸点仪——CP-Ⅰ型和CP-Ⅱ型沸点仪, 阐述了仪器各部分结构的设计思想和原理, 并对仪器的性能和各部分功能进行了较为完整的实验考核, 获得了预期的效果。     

健康猕猴血液和毛发微量元素含量的正常值测定和差异比较

对猕猴(Macaca mulatta)血液和毛发的镁、锰、钼、镍、铅、铬、镉、锌、铁、铜、钙等11种元素的含量，用电感耦合高频等离子体发射光谱仪进行了测定．给出了各个元素在血液和毛发中的平均含量值和变动范围．指出毛发中的微量元素含量一般较血液为高，且变动较小．与人体内含量比较，猴毛发的Cu、Mo、CA、Ni的含量与人发接近；猴血液的Zn、Fe、Ca、Mn、Ca亦与人的接近．对猴血液微量元素含量随年龄、体重、性别变化及血液含量和毛发含量的相关关系进行了统计学检验．通过对测定值的比较分析，认为尽管动物体内的微量元素含量随种类、环境、个体差异变化较大，就群体平均含量而言，仍存在着相似的变化规律。本文的测定结果对了解猕猴对微量元素的需要提供了初步依据．     

Extended applications and potential limitations of ring-fused 2,3-oxazolidinone thioglycosides in glycoconjugate synthesis

The utility of ring-fused 2,3-oxazolidinone derivatives of 2-amino-2-deoxy-thioglycosides in the synthesis of glycopeptide intermediates and building blocks for the synthesis of heparan sulfate oligosaccharides is reported. These unique ring-fused monosaccharides afford a novel and efficient route to alpha-O-linked 2-amino-2-deoxy amino acid derivatives and heparan sulfate oligosaccharide intermediates.     

AB5型球形合金粉的表面处理研究

由雾化（Gas－atomization）技术制备的AB5型球形合金粉，作为镍氢电池负极材料具有很多优点：粉粒呈球状便于在多孔基片内装填；耐压耐磨性好；抗碱能力强且不易解胶．但它的电化学初活性差，难于活化．有碍电池中的应用．采用适宜的氧化剂（铜盐水溶液）处理，使球粒表面形成一个富铜、富镍亚层，显著地改善了合金粉的电化学活性．经处理的MlNi3.8CO0.5Mn0.3Al0.4球形合金粉，仅3次充放电循环其放电量便可达到240mA·h·g-1；而未经处理的同一合金粉即便经6次充放电循环其放电量也只有103mA·h·g-1．     

四（对羟基苯基）卟啉—硅胶固定相的合成及在核苷酸分析中的应用

以大孔微硅胶作基体，经γ－氨丙基三乙氧基硅烷活化与间隔臂氯代环内烷反应后，再与预先合成的四（对羟基苯基）卟啉配体键合，构成电荷转移型亲和色谱固定相。以ＰＨ＝７．０的磷酸盐缓冲溶液作流动相，成功实现对一些核苷酸的高效液相亲和色谱分离。     

热定型聚酯纤维内应力与晶格变形的关系

<正> 结晶学家认为低分子物结晶虽可能存在一定缺陷和变形,但一般都具有一定的晶胞参数。这一概念对于高分子物结晶已不再正确。Bosley认为成形、热处理、冷却速率和杂质的存在皆可引起晶格变形;Fakirov故意在PET中加入少量杂质,却未引起变形。至今,PET已累积了7组晶胞参数,8个计算所得的晶区密度显示了较大幅度的波动(见     

A spectroscopic study on the 12-heteropolyacids of molybdenum and tungsten (H3PMo12−nWnO40) combined with cetylpyridinium bromide in the epoxidation of cyclopentene

The epoxidation of cyclopentene with hydrogen peroxide catalyzed by 12-heteropolyacids of molybdenum and tungsten (H₃PMo_12−nW_nO₄₀, n = 1–11), 12-tungstophosphoric acid and 12-molybdophosphoric acid combined with cetylpyridinium bromide as a phase transfer reagent was carried out in acetonitrile. Among 13 heteropolyacids investigated, catalyst of H₃PMo₆W₆O₄₀ showed the highest activity, giving a conversion of 60% and a selectivity of 95% in the epoxidation of cyclopentene. The fresh catalysts and the catalysts under reaction condition were characterized by UV–vis, FT-IR and ³¹P NMR spectroscopy, which has revealed that all of the molybdotungstophosphoric acids were degraded in the presence of hydrogen peroxide to form a considerable amount of phosphorus-containing species. The active species resulted from H₃PMo₆W₆O₄₀ are new kinds of phosphorus-containing species, which is different from {PO₄[WO(O₂)₂]₄}³⁻.     

Zirconium and hafnium complexes containing bidentate diarylamido-phosphine ligands

The first examples of mononuclear, structurally characterized triarylphosphine complexes of zirconium and hafnium are reported. The metathetical reactions of MCl4(THF)2 (M = Zr, Hf) with [iPrNP]Li(THF)2 ([iPrNP]- = N-(2-(diphenylphosphino)phenyl)-2,6-diisopropylanilide) or [MeNP]Li(THF)2 ([MeNP]- = N-(2-(diphenylphosphino)phenyl)-2,6-dimethylanilide) in toluene at -35 degrees C produced the corresponding [iPrNP]MCl3(THF) and [MeNP]2MCl2, respectively, in high yield. In contrast, attempts to prepare [MeNP]MCl3(THF) and [iPrNP]2MCl2 led to the concomitant formation of mono- and bis-ligated complexes, from which purification proved rather ineffective. The solution and solid-state structures of [iPrNP]MCl3(THF) and [MeNP]2MCl2 were studied by multinuclear NMR spectroscopy and X-ray crystallography. The geometry of these six-coordinate complexes is best described as a distorted octahedron in which the chloride ligands in [iPrNP]MCl3(THF) adopt a virtually meridional coordination mode whereas those in [MeNP]2MCl2 are trans to each other.     

新铌酸盐Ba5NdTi3Nb7O30的合成与介电性能

The New Niobate Ba₅NdTi₃Nb₇O₃₀ was synthesized by solid state reaction at 1250℃ for 48h. The crystal structure and dielectric properties of Ba₅NdTi₃Nb₇O₃₀ were determined by X-ray powder diffraction and dielectric measurements. The results show that Ba₅NdTi₃Nb₇O₃₀ belongs to ferroelectric phase of tetragonal tungsten bronze structure at room temperature with unit cell parameters: a=1.24424(4)nm, c=0.39476(2)nm, calculated density 5.719g·cm^-3. Ba₅NdTi₃Nb₇O₃₀ belongs to relaxor ferroelectrics. The phase transition temperature (T_c) of Ba₅NdTi₃Nb₇O₃₀ from ferroelectric to paraelectric is found to shift toward higher temperature side at higher fre-quency, and T_c is 90℃ at 1kHz. At room temperature, the dielectric constant (ε_r) and dielectric loss of Ba₅NdTi₃Nb₇O₃₀ decrease with the increase of frequency, and Ba₅NdTi₃Nb₇O₃₀ ceramic have high dielectric constant 489 at 1kHz.