Novel Copper（Ⅱ） and Zinc（Ⅱ） 2-D Supramolecular Structures Based on Carboxylate and 1-Substitutedimidazole Mixed-ligands

Using the ligand bis(3-(1H-imidazol-1-yl)-1-phenylpropan-1-one) L, two novel com- plexes [CuL2(ph))]·H2O 1 and [ZnL2(tp)] 2 (ph = phthalic acid, tp = terephthalic acid) have been synthesized and their crystal structures were determined by single-crystal X-ray diffraction analysis. Crystal data for 1: triclinic, space group P1, a = 9.4300(17), b = 12.148(2), c = 13.721(2) , α = 109.620(2), β = 94.351(2), γ = 94.830(2)°, C32H30N4O7Cu, Mr = 646.14, V = 1466.2(4) 3, Z = 2, Dc = 1.464 g/cm3, μ(MoKα) = 0.801 mm-1, F(000) = 670, the final R = 0.0337 and wR = 0.0859 for 5122 observed reflections with I > 2σ(I). And those for 2: monoclinic, space group P2/n, a = 7.1866(11), b = 14.144(2), c = 14.407(2) , β = 101.427(2)°, C32H28N4O6Zn, Mr = 629.95, V = 1435.4(4) 3, Z = 2, Dc = 1.457 g/cm3, μ(MoKα) = 0.908 mm-1, F(000) = 652, the final R = 0.0438 and wR = 0.0821 for 2546 observed reflections with I > 2σ(I). In 1 and 2, ph or tp ligands bridge the six-coordinated copper(II) or four-coordinated zinc(II) ions forming 1D zigzag chains while L ligands act as the terminal monodentate ligand. It is noted that weak non-classical C–H···O plays the important and dominating roles in the formation of 2D supramolecular architectures of 1, but in 2 non-classical C–H···O and aromatic π-π stacking interactions are quite important and play dominant roles in the self-assembly of 2D supramolecular architectures.     

WaterLOGSY NMR experiments in conjunction with molecular-dynamics simulations identify immobilized water molecules that bridge peptide mimic MDWNMHAA to anticarbohydrate antibody SYA/J6

X-ray crystallographic data of the carbohydrate mimic MDWNMHAA when bound to an anti-Shigella flexneri Y mAb SYA/J6 indicate the immobilization of water molecules, that is, the presence of "bound" waters, in the active site. Water Ligand Observed via Gradient Spectroscopy (WaterLOGSY) was used in conjunction with saturation transfer difference (STD)-NMR spectroscopy to probe the existence of immobilized water molecules in the complex of MDWNMHAA 1 bound to mAb SYA/J6. Molecular dynamics simulations using the ZymeCAD Molecular Dynamics platform were then used to specify the likely locations of these water molecules. Of note, those waters involved in providing complementarity between the peptide and mAb SYA/J6 remained throughout the course of the simulation. Together, the experimental and computational protocols have been used to identify the bound water molecules present in the antibody-peptide complex.     

蓝光激发的Y2.93Al5O12∶0.07Ce3+黄色荧光粉的制备及光致发光

以Al₂(SO₄)₃·18H₂O、尿素为原料,采用水热-热解法制备了球形α-Al₂O₃粉体。以自制α-Al₂O₃、Y₂O₃及CeO₂为原料,固相法制备了白光LED用Y_2.93Al₅O₁₂∶0.07Ce3+黄色荧光粉,通过X射线衍射（XRD）、扫描电镜（SEM）、X射线能谱（EDS）及荧光光谱（PL）等对产物的物相、形貌及光致发光性能进行了表征。结果表明：水热-热解法制备出了物相纯净、分散性良好的球形α-Al₂O₃粉体,以该α-Al₂O₃为原料,合成出可被460 nm蓝光有效激发,发射光谱为峰值在550 nm宽带的Y_2.93Al₅O₁₂∶0.07Ce3+荧光粉,色坐标为（0.453,0.531 9）,采用GSAS软件对Y_2.93Al₅O₁₂∶0.07Ce3+荧光粉的XRD图进行了Rietveld结构精修,精修图与XRD测试图完全吻合,Y,Al,Ce,O四元素均匀地分布在黄色荧光粉产物中,Y_2.93Al₅O₁₂∶0.07Ce3+黄色荧光粉的激发光谱由两个部分组成,在340和460 nm处有两个非常明显的吸收峰,Ce3+的4f能级由于自旋-耦合而劈裂为两个光谱支项2F_7/2和2F_5/2,其中2F_5/2为基谱项。340 nm的激发峰对应于2F_5/2→5D_5/2的跃迁,460 nm的激发峰属于2F_7/2→5D_3/2的跃迁,并且460 nm处的激发强度强于340 nm处激发强度。以460 nm为监测波长得到的发射光谱,最强发射峰位于550 nm,Y_2.93Al₅O₁₂∶0.07Ce3+荧光粉是一种适用于白光LED的高性能黄色荧光粉。     

ChemInform Abstract: Two New Compounds, β-ScTe and Y3Au2, and a Reassessment of Y2Au.

The title compounds are prepared by solid state reaction of the elements (Ta containers; 1573 K, 200 h for β-ScTe and 1323 K, 7 d for Y₃Au₂ and Y₂Au).     

毛细管离子分析仪中电解液稳定性研究

毛细管离子分析仪测定水中氟离子时,常出现氟化物峰与水负峰相连的情况,通常是电解液失效造成的。通过跟踪试验,研究了毛细管离子分析仪使用的电解液的稳定性。     

荧光素-曙红Y能量转移荧光猝灭法测定微量白蛋白研究

在λex/λem=405/547 nm,于缓冲溶液和表面活性剂存在的情况下,荧光素和曙红Y能够发生有效能量转移,而牛血清白蛋白(BSA)的加入使得曙红Y荧光猝灭,该体系可用于微量蛋白质的测定。系统探讨了荧光素-曙红Y能量转移体系发生荧光猝灭的条件,最佳条件为:2.0 mL pH=3.8的B-R缓冲溶液,0.4 mL 0.05%曲拉通X-100,1.5 mL 1.0×10-4mol/L的荧光素水溶液,2.0 mL 1.0×10-4mol/L的曙红Y水溶液,最佳实验时间为溶液配制完成静置15 min后60 min内,最佳加入顺序为pH=3.8缓冲溶液+荧光素+曙红Y+曲拉通+蛋白质标准溶液或样品。在优化的实验条件下,蛋白质含量在0～2.0μg/mL范围内与荧光猝灭强度呈良好的线性关系。检出限为6.6 ng/mL;测定样品的相对标准偏差(RSD)在±5%以内;样品加标回收率为90.4%～95.3%。该法可用于人血清、牛奶中蛋白质含量的测定。     

硫酸氢钾催化一锅法合成1-乙酰胺烷基-2-萘酚

以硫酸氢钾为催化剂,在无溶剂条件下催化2-萘酚和乙酰胺分别与苯甲醛、对硝基苯甲醛、水杨醛、茴香醛、香兰素等五种芳香醛的三组分反应,利用一锅法合成了系列1-乙酰胺烷基-2-萘酚.以1-乙酰胺基苯甲基-2-萘酚(AAN)的合成为模板反应考察了催化剂用量、反应温度、原料配比及反应时间等因素对产物收率的影响.结果表明,硫酸氢钾催化合成AAN反应的适宜条件为:n(2-萘酚)∶n(苯甲醛)∶n(乙酰胺)∶n(硫酸氢钾)=1∶1.2∶1.2∶0.05,90℃下反应40min,AAN的收率达92.1%.硫酸氢钾对其他四种反应也有较理想的催化作用,目标产物收率为69.1%～94.0%.     

氧化钇对高速CBN砂轮用陶瓷结合剂玻璃料性能的影响

在CaO-Al2O3-SiO2(CAS)系统微晶玻璃中引入稀土氧化物Y2O3,制备出用于高速CBN砂轮的微晶玻璃结合剂。结合DTA,XRD,SEM等检测手段,研究了Y2O3的加入对微晶玻璃结合剂微观结构及其性能的影响。结果表明:随Y2O3含量的增加,微晶玻璃结合剂的耐火度降低,流动性增大。当Y2O3含量为0.8%(质量分数)时,钙铝硅系微晶玻璃结合剂具有最佳的力学性能(显微硬度753.26 MPa,抗折强度167.50 MPa,磨耗比1∶8.23)。加入Y2O3会影响玻璃的析晶性能,当加入Y2O3为0.8%时,促进析出新晶相Li2Al2SiO10和β-石英,尺寸大小约为0.2～1μm,其具有致密的微观结构,利于用于作CBN砂轮的结合剂。     

A Dodecahedrane-like Molecule C_（12）H_（12）B_8 with Uncommon T_h Symmetry

The molecule with Th symmetry is rare.A dodecahedrane-like molecule C12H12B8 with uncommon Th symmetry has been reported here.Density functional calculations and minimization techniques have been employed to characterize its structural and electronic properties.Its geometry,electronic properties,vibrational frequencies and heat of formation have been calculated at the B3LYP/6-311+G(d,p) level of theory.The absence of imaginary vibrational frequency confirms that it corresponds to true minimum on the potential energy hypersurface.Its vibrational bands in the IR intensity have been discussed and compared with future experimental identification.At the B3LYP/6-311+G(d,p) level,the heat of formation has been calculated to be 720.9 kJ mol-1 using the isodesmic reaction.According to this value,it is a potential high energy density molecule.     

HCl处理后局部有序Y沸石的二次晶化

将商品 Y 型沸石用 HCl 处理后, 运用 X 射线粉末衍射, 透射电镜和扫描电镜、红外光谱及 27Al 和 29Si 魔角旋转核磁共振对其进行了表征. 结果表明, 酸处理后 Y 沸石接近无定形, 其长程有序性遭到破坏, 但还保留部分局部结构. 以不同浓度酸处理后的 Y 沸石为前驱体, 在 150 oC, 0.3 mol/L NaOH 条件下采用蒸汽辅助干胶转化法进行二次晶化, 可以获得丝光沸石, 其相纯度与前驱体的 Si/Al 密切相关. 随 Si/Al 比不同, 所得丝光沸石形貌由纳米针状堆积逐渐向微米单块状变化, 且其比表面积可达 400 m2/g 以上, 微孔孔容在 0.19 cm3/g.