Synthesis and Crystal Structure of Ag2（admtrz）2（CF3CO2）2（admtrz=4—amino—3,5—dimethyl—1,2,4—triazole）

1 INTRODUCTION Transition metal complexes bridged by 1, 2, 4-triazole group can produce interesting structures and specific properties[1]. Many attempts have been made to synthesize a variety of complexes with paramagnetic centers by using such ligands, and their structures and magnetic properties have been characterized[2]. However, the polynuclear Ag(I) complexes bridged by 1, 2, 4-triazole have been poorly studied[3]. Recently, we have prepared a series of silver(I) triazole complex…     

界面改性剂对刚性粒子增韧尼龙6熔体流变行为的影响

研究了界面改性剂对高岭土增韧尼龙６熔体流变行为的影响,并与硅烷偶联剂ＫＨ５５０进行了比较．结果表明,ＫＨ５５０的加入明显降低了高岭土填充尼龙６熔体的粘度和弹性,而界面改性剂显著地增强了它的粘度和弹性．这一差别应归因于同ＫＨ５５０相比,界面改性剂更有效地增强了高岭土与尼龙６基体之间的界面结合和其自身的回弹性能．同时,界面改性剂的用量对高岭土填充尼龙６流变行为具有很大影响．当界面改性剂的用量为高岭土和尼龙６总量的２％时,界面改性剂在高岭土表面上趋于“饱和”,再增加界面改性剂的用量,对流变行为的影响不大．     

一个新的噻二唑衍生物H2ADTZ与锰的二维聚合物的合成与晶体结构(英)

A new 1,3,4 thiadiazole-derivative ligand 2,5-(s-acetic acid) dimercapto-1,3,4 thiadiazole (H₂ADTZ) and its one-dimensional manganese polymer Mn(ADTZ)·4H₂O had been synthesized and structurally characterized by X-ray single crystal diffraction in this paper. The Mn(Ⅱ) ion is coordinated with a distorted octahedron by two oxygen atoms from neighboring two deprotonated ligands ADTZ^2- and other four oxygen atoms from four coordinated water molecules. The structural feature of the title compound is the formation of one-dimensional manganese chains polymer through the bridging of dioxygen O-O units. In the solid state structure of the complex, one-dimensional manganese chains are joined together by the weak intermolecular hydrogen bonds and vander Waals interactions forming a two-dimensional supramolecular compound. Furthermore, the UV spectra and electro-chemical properties of the title compound were also investigated. CCDC: 260532.     

钴的二苯甲酰甲烷配合物：晶体结构及其轴向置换反应

Cobalt(Ⅱ) can form complexes with Hdbm in different environments. Hdbm reacted with cobalt nitrate to give complex 1 [Co(dbm)₂·2H₂O]. When complex 1 reacted with pyridine， α-stilbazole or 4，4′-bipyridine respectively， complex 2 [Co(DBM)₂Py₂] (Py=pyridine)， 3 [Co(DBM)₂Sbz₂] (Sbz=α-stilbazole) or 4 [Co(DBM)₂BPy]_n was obtained in turn through metathetical reaction. The coordination modes are octahedral polyhedrons. In the crystal structures， the two dbms take the plane position and two other donor molecules take the axial position. CCDC： 196070 for complex 2; 186859 for complex 3.     

C60-地塞米松的激光激发

利用激光光解装置检测了C60-地塞米松(C60-DE)的苯溶液在355 nm激光照射下产生的激发三重态, 3C60-DE*出现四个吸收峰, 分别位于700、440、350 和310 nm. 在330 nm处观察到了它的漂白吸收最大值, 这与其基态吸收最大值相对应. 3C60-DE*能够将能量转移给O2分子而淬灭. 与3C60*相比, 3C60-DE*的三重态鄄三重态(T-T)淬灭速率常数减小(3C60*为(5.03±1.31)×109 L·mol-1·s-1, 3C60-DE*为(3.53±0.87)×109 L·mol-1·s-1), 而寿命增加了(3C60*为(12.0±2.6) μs, 3C60-DE*为(18.0±3.3) μs), 这可能是C60分子上连接了地塞米松分子后减小了C60球之间碰撞的几率所致.     

不同剂型药用抑肽酶纯度的胶束电动毛细管测定

 以十六烷基三甲基溴化铵 (CTAB)为阳离子表面活性剂 ,用胶束电动毛细管 (MECC)分别对抑肽酶粉针剂和抑肽酶注射液进行纯度测定。实验中选择了最佳缓冲液 (含 4mmol/LCTAB的 80mmol/LNa2 HPO4 H3 PO4,pH 7 0 0 ) ,考察了进样量与样品中高浓度盐对分离的影响。并对毛细管区带电泳、MECC和高效液相的分离效果加以比较 ,表明MECC的分离效果最佳。     

Solution self-assembly, spontaneous deprotonation, and crystal structures of bipyrazolate-bridged metallomacrocycles with dimetal centers

A series of nanosized cavity-containing bipyrazolate-bridged metallomacrocycles with dimetal centers, namely, {[(bpy)M]8L4}(NO3)8 [L=3,3',5,5'-tetramethyl-4,4'-bipyrazolyl, Pd, Pt; 1,4-bis-4'-(3',5'-dimethyl)-pyrazolylbenzene), Pd; and 1,4-bis-4'-(3',5'-dimethyl)-pyrazolylbiphenyl, Pd], {[(phen)M]8L4}(NO3)8 [L=3,3',5,5'-tetramethyl-4,4'-bipyrazolyl, Pd, Pt; 1,4-bis-4'-(3',5'-dimethyl)-pyrazolylbenzene, Pd; and 1,4-bis-4'-(3',5'-dimethyl)-pyrazolylbiphenyl, Pd], {[(bpy)Pd]6L3}(NO3)6 [L=1,4-bis-4'-(3',5'-dimethyl)-pyrazolylbenzene,], {[(phen)Pd]6L3}(NO3)6 [L=1,4-bis-4'-(3',5'-dimethyl)-pyrazolylbenzene,], {[(bpy)Pd]4L2}(NO3)4 [L=1,3-bis-4'-(3',5'-dimethyl)-pyrazolylbenzene, and 1,2-bis-4'-(3',5'-dimethyl)-pyrazolylbenzene,], and {[(phen)Pd]4L2}(NO3)4 [L=1,3-bis-4'-(3',5'-dimethyl)-pyrazolylbenzene, and 1,2-bis-4'-(3',5'-dimethyl)-pyrazolylbenzene,] (where bpy=2,2'-bipyridine and phen=1,10-phenanthroline) have been synthesized through a directed self-assembly approach that involves spontaneous deprotonation of the 1H-bipyrazolyl ligands in aqueous solution. These complexes, with weak Pd(II)...Pd(II) or Pt(II)...Pt(II) interactions, have been characterized by elemental analysis, 1H and 13C NMR, cold-spray ionization or electrospray ionization mass spectrometry, UV-visible spectroscopy, and luminescence spectroscopy. Complexes and have also been characterized by single-crystal X-ray diffraction analysis.     

Unsymmetric-1,3-disubstituted imidazolium salt for palladium-catalyzed Suzuki–Miyaura cross-coupling reactions of aryl bromides

A series of 1-(ferrocenylethyl)-3-substituted-imidazolium salts [3-substitute = 2,6-di(iso-propyl)phenyl (1a), 2,4,6-trimethylphenyl (1b), tert-butyl (1c), 1-Ad (1d), cyclohexyl (1e)] have been synthesized from a racemic ferrocenylethyl acetate and the corresponding N-substituted imidazole in high yields (70–94%). A combination of Pd(OAc)₂ and 1a–d was found to form an excellent catalyst system for the Suzuki–Miyaura cross-coupling reactions of aryl bromides with phenylboronic acid in the presence of Cs₂CO₃.     

Synthesis and Crystal Structure of Isonicotinic Acid [1-（3,5-Dibromo-2- hydroxyphenyl）methylidene]hydrazide Methanol

A new Schiff base compound, C13H9Br2N3O2·CH3OH, isonicotinic acid [1-(3,5- dibromo-2-hydroxyphenyl)methylidene]hydrazide methanol, has been synthesized and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The compound comprises a Schiff base moiety isonicotinic acid [1-(3,5-dibromo-2-hydroxyphenyl) methylidene]hydrazide and a methanol molecule. The crystal belongs to the triclinic system, space group P1 with a = 8.464(1), b = 9.511(2), c = 10.901(2) , α = 92.940(2), β = 110.456(2), γ = 96.040(2)o, Z = 2, V = 814.0(2) 3, Dc = 1.759 g/cm3, Mr = 431.09, λ(MoKα) = 0.71073 , μ = 4.994 mm-1, F(000) = 424, R = 0.0440 and wR = 0.1061. A total of 3284 unique reflections were collected, of which 2197 with I > 2σ(I) were observed. The molecule adopts a trans configuration about the C=N double bond. The dihedral angle between the benzene and pyridine rings is 22.0(4)o. The crystal structure is stabilized by intermolecular O-H···N and C-H···O hydrogen bonds, forming layers parallel to the ac plane. The preliminary biological tests show that the compound has potential antibacterial activities.     

Vibrational Spectroscopic Study on Ion Solvation and Association of Lithium Perchlorate in 4-Methoxymethyl-ethylene Carbonate

Solvation interaction and ion association in solutions of lithium perchlorate/4-methoxymethyl-ethylene carbonate （MEC） have been studied by using Infrared and Raman spectra as a function of concentration of lithium perchlorate. The splitting of ring deformation band and ring ether asymmetric stretching band, and the change of carbonyl stretching band suggest that there should be a strong interaction between Li^＋ and the solvent molecules, and the site of solvation should be the oxygen atom of carbonyl group. The apparent solvation number of Li^＋ was calculated by using band fitting technique. The solvation number was decreased from 3.3 to 1.1 with increasing the concentration of LiClO4/MEC solutions. On the other hand, the band fitting for the ClO4^- band revealed the presence of contact ion pair, and free ClO4^- anion in the concentrated solutions.