稀土冠醚配合物的研究ⅩⅩⅠ.单羟基冠醚与钙、稀土元素间的竞争配位及其钙配位化合物的晶体结构

研究了单羟基冠醚配位体6-羟基-2,3,9,10-二苯并-1,4,8,11,14-五氧杂环十六-2,9-二烯(L)对钙和镧系元素的竞争配位反应,发现该配位体在我们的实验条件下对钙的配位能力要明显大于对重稀土的配位能力;同时研究了标题大环配位体和钙的配位化合物的晶体结构,该配位化合物的分子结构式为[Ca(NO3)(H2O)L](NO3),Mr=528.47,晶体属单斜晶系,a=1.5285(6),b=0.9713(3),c=1.5134(7)nm,β=98.79(3)°,V=2.2205nm3,Dex=1.531g/cm3,Dc=1.527g/cm3,Z=4,空间群为P21/c.     

超分子化合物[M(4,4''''-bipy)2(H2O)4]·(4,4''''-bipy)2·(3,5-diaba)2·8H2O](M=Co,Ni,Cd)的合成及晶体结构

合成了3个超分子化合物[M(4,4'-bipy)2(H2O)4]·(4,4'-bipy)2·(3,5-diaba)2·8H2O(M=Co(1),Ni(2),Cd(3);4,4'-bipy=4,4'-联吡啶;3,5-diaba=3,5-二氨基苯甲酸阴离子),用红外光谱、元素分析及X-射线单晶衍射进行了表征。3个化合物的晶体都属于单斜晶系,空间群为P2/c。晶体学参数:化合物1:a=0.9389(2)nm,b=0.7751(1)nm,c=3.9284(6)nm,β=90.14(2)°,V=2.85880(69)nm3,Z=4,Dc=1.397g·cm-3,F(000)=1266,μ=0.380mm-1,R1=0.0349,wR2=0.0829;化合物2:a=0.9383(2)nm,b=0.7753(1)nm,c=3.9218(6)nm,β=90.09(1)°,V=2.85280(68)nm3,Z=2,Dc=1.399g·cm-3,F(000)=1268,μ=0.420mm-1,R1=0.0366,wR2=0.0805;化合物3:a=0.94091(13)nm,b=0.77885(11)nm,c=3.9712(5)nm,β=90.10°,V=2.9102(7)nm3,Z=2,Dc=1.433g·cm-3,F(000)=1308,μ=0.454mm-1,R1=0.0468,wR2=0.0964。3,5-diaba未参与配位,在配位阳离子[M(4,4'-bipy)2(H2O)4]2 中,金属离子M髤与来自2个4,4'-bipy的2个氮原子和4个水分子的氧原子配位,呈八面体的几何构型。分子中还存在未配位的4,4'-bipy。通过配位阳离子、游离4,4'-bipy及未配位的3,5-diaba间的丰富氢键,构建成具有三维结构的超分子化合物。     

对甲苯磺酰谷氨酸桥联的一维双链锰配合物的合成、表征与晶体结构

A one-dimensional double-chain coordination polymer [Mn(phen)(tsgluo)] was synthesized in a mixed solution and its crystal structure was determined by X-ray diffraction method. It crystallizes in orthorhombic system with space group P2₁2₁2₁. The crystal data are: a=0.530 78(17) nm, b=1.723 9(5) nm, c=2.456 9(8) nm, Z=4, μ=0.729 mm^-1, D_c=1.579 g·cm^-3, V=2.248 1(12) nm³, R₁=0.033 1, ωR₂=0.078 9. In the title complex, each Mn(Ⅱ) ion presents a octahedral geometry with the coordination of two nitrogen atoms from 1,10-phenanthroline and four oxygen atoms from three different tsgluo^2- ligands. The γ-carboxyl coordinates to Mn(Ⅱ) in the mode of bidentate chelate, while the α-carboxyl coordinates in a bidentate bridging mode. CCDC: 253910.     

层状LiMnO2的固相合成及电化学性能

以Mn₂O₃和氢氧化锂为原料，通过焙烧合成出o-LiMnO₂。用X射线衍射和扫描电镜对不同温度下合成的粉末样品进行了表征，并研究了材料的电化学性能。通过对不同温度条件下烧结样品的晶胞参数、布拉格(110)晶面峰半高宽及电化学性能研究发现：600 ℃下合成样品的半高宽最大，堆垛层错率高，同时电化学性能也最好，首次放电容量达到156 mAh·g^-1，20次循环后仍保持在140 mAh·g^-1以上。中高温固相合成的o-LiMnO₂材料，在晶粒范围大小相近时，材料电化学性能与材料堆垛层错率相关。     

月光花素甲(Ⅰ)、(Ⅱ)整体分子结构的测定

本文对月光花素甲(Calonyctin A)的整体分子结构分析加以完善并进行总结。前文报道月光花素甲是两个分子量相差28a.m.u的糖甙类同系物分子的混合物。这两个分子(简称M_1和M_2)分别称为月光花素甲(Ⅰ)与月光花素甲(Ⅱ)(Calonyctm A_1,CalonyctinA_2),分子量分别为938与910。它们分别含     

Detection of Tumor Necrosis Factor Gene by Piezoelectric Nucleic Acid Sensor

ＩｎｔｒｏｄｕｃｔｉｏｎＴｈｅｇｅｎｅｄｉａｇｎｏｓｉｓｔｅｃｈｎｏｌｏｇｙ ,ａｌｓｏｃａｌｌｅｄｎｕｃｌｅｉｃａｃｉｄｐｒｏｂｅｔｅｃｈｎｏｌｏｇｙ ,ｈａｓｂｅｃｏｍｅａｎａｔｔｒａｃｔｉｖｅｍｅｔｈｏｄｉｎｔｈｅｆｉｅｌｄｓｏｆｂｉｏｃｈｅｍｉｓｔｒｙａｎｄｃｌｉｎｉｃａｌｍｅｄｉｃｉｎｅ .Ｉｔｉｓｐｒｏｖｅｄｔｏｂｅｃｏｎｖｅｎｉｅｎｔａｎｄｓａｆｅｕｓｉｎｇｎｏｎ ｒａｄｉｏａｃｔｉｖｅｒｅａｇｅｎｔｓｗｉｔｈｅｌｅｃｔｒｏｃｈｅｍｉｃａｌａｎｄｏｐｔｉｃａｌｄｅｔｅｃｔｏｒ.Ｅｓｐｅ ｃ…     

C60,C70与过氧苯甲酰反应的动力学研究

Ｃ_（６０）、Ｃ_（７０）与过氧苯甲酰反应的动力学研究胡波，薛万华，张法义，尚振锋，马克勤，臧雅茹，赵学庄（南开大学化学系，天津，３０００７１）关键词Ｃ_（６０），Ｃ_（７０），动力学Ｋｒａｔｓｃｈｍｅｒ等人［１］的发现使制备宏观量的Ｃ（６０）和Ｃ（７０...     

LC-MS/MS定量测定大鼠和人肝微粒体孵育液中丁苯酞浓度方法的建立

正丁苯酞(n-butylphthalide,NBP),又名芹菜甲素,是我国心脑血管领域第一个拥有自主知识产权的药物,它具有很强的抗脑缺血损伤作用,而毒副作用较低[1-2].     

水/油型微乳液中球形及棒状钛酸锶钡纳米粒子的控制合成

Barium strontium titanate nanoparticles with spherical and rod-like morphologies were synthesized in water/Triton X-100/n-hexanol/cyclohexane quaternary reverse microemulsion solution. The influences of the molar ratio of water to surfactant (ω₀) and the concentration of reactants on the morphology and size of barium strontium titanate nanoparticles were studied. The structure, compositions and morphology of the prepared products were characterized by XRD, SAED, ICP, EDS and TEM. The results show that the obtained Ba_0.7Sr_0.3TiO₃ spherical nanoparticles with diameters of 20～100 nm and the Ba_0.7Sr_0.3TiO₃ nanorods with diameters of 70～120 nm and lengths up to 600～800 nm are a single crystal, with a cubic phase. The molar ratio for barium, strontium and titanate in products is about 0.7:0.3:1.     

Hydrothermal Synthesis and Structural Characterization of a Novel Organic—Inorganic Hybrid Compound {[Cu（2,2′—bpy）2]2—Mo8O26}

A novel organic-inorganic hybrid compound {[Cu(2,2′-bpy)2]2Mo8O26} has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group, Pna21,with a=2.4164(5),b=1.8281(4),c=1.1877(2)nm,V=5.247(2)nm^3,Z=4,and final R1=0.0331,wR2=0.0727.The structure consists of discrete {[Cu(2,2′-bpy)2]2Mo8O26} clusters,constructed from a β-octamolybdate subunit[Mo8O26]^4- covalently bonded to two [Cu(2,2′-bpy)2]^2 coordination complex cations via bridging oxo groups.In addition,the spectroscopic properties and thernal behavior of this compound have been investigated by spectroscopic techniques (UV-vis,IR,Raman and EPR spectra) and TG analysis.