Solvothermal Synthesis and Structure Studies of a Mixed-valence Oxochloromolybdenum Complex

Emerald green crystals of a new mixed-valence oxochloromolybdenum complex,Mo(OH)2(2,2′-bipy)Cl2.[MoO(2,2′-bipy)Cl3]2, were obtained in an attempt to synthesize the Mo-S cluster compounds under solvothermal conditions. The title compound was characterized by EPR and X-ray single-crystal diffraction techniques. Crystallographic data: orthorhombic, space group Fdd2, a = 12.684(1), b = 21.518(2), c = 29.096(3)A, Mr = 1103.97, V= 7941(1)A^3, Z= 8, Dc =1.843 g/cm^3,μ= 1.514 mm^-1, F(000) = 4304, R = 0.0654 and wR = 0.1544 for 1944 observed reflections with 1 ≥/ 2σ(I). The compound consists of two different neutral molecules, Mo^IV-(OH)2(2,2′-bipy)Cl2 and MoVO(2,2′-bipy)Cl3. Both Mo^IV and Mo^V ions are in a distorted octahedral environment. The Mo(1)^IV atom is surrounded by two Cl^- ions and two O atoms from OH^- and two N atoms from a 2,2′-bipy ligand. The Mo(2) atom is surrounded by three Cl^- ions, one O^2- anion and two N atoms from another 2,2“-bipy ligand. The bipyridine occupies two cis-equatorial sites, while the Cl^- ions are located at the axial and equatorial positions.     

Efficient Synthesis of 5‐Carboxanilide‐Dihydropyrimidinones Using Cobalt(II) Nitrate Hexahydrate

5‐Carboxanilide‐dihydropyrimidinone derivatives were synthesized in good yield in a three‐component and efficient process by the condensation reaction of acetoacetanilide, aldehyde and urea/thiourea in the presence of cobalt(II) nitrate hexahydrate as catalyst in ethanol at ambient condition.     

Negative Modulation of the Angiogenic Cascade Induced by Allosteric Kinesin Eg5 Inhibitors in a Gastric Adenocarcinoma In Vitro Model

Eg5 is a kinesin essential in bipolar spindle formation, overexpressed in tumours, thus representing a new target in cancer therapy. We aimed at evaluating the anti-cancer activity of Eg5 thiadiazoline inhibitors 2 and 41 on gastric adenocarcinoma cells (AGS), focusing on the modulation of angiogenic signalling. Docking studies confirmed a similar interaction with Eg5 to that of the parent compound K858. Thiadiazolines were also tested in combination with Hesperidin (HSD). Cell cycle analysis reveals a reduction of G1 and S phase percentages when 41 is administered as well as HSD in combination with K858. Western blot reveals Eg5 inhibitors capability to reduce PI3K, p-AKT/Akt and p-Erk/Erk expressions; p-Akt/Akt ratio is even more decreased in HSD+2 sample than the p-Erk/Erk ratio in HSD+41 or K858. VEGF expression is reduced when HSD+2 and HSD+41 are administered with respect to compounds alone, after 72 h. ANGPT2 gene expression increases in cells treated with 41 and HSD+2 compared to K858. The wound-healing assay highlights a reduction in the cut in HSD+2 sample compared to 2 and HSD. Thus, Eg5 inhibitors appear to modulate angiogenic signalling by controlling VEGF activity even better if combined with HSD. Overall, Eg5 inhibitors can represent a promising starting point to develop innovative anti-cancer strategies.     

用水热法和溶剂热法合成LiSrAlF6

用水热和溶剂热法（甲苯作溶剂）合成了LiSrAlF6单相多晶。研究了反应物摩尔比、反应温度和反应时间等对产物的影响。采用环境扫描电子显微镜观察到LiSrAlF6晶体的形貌特征为六角晶形,并聚集成花朵形。试探了LiCaAlF6多晶粉末的水热和溶剂热合成,但未能获得纯相产物。     

Synthesis of Nickel Sulfide Particles by Solvothermal Process

Pyrite nickel disulfide and millerite nickel monosulfide have been successfully prepared by solvothermal method based on the reaction of Ni(NO3)26H2O and H2NC(S)NH2 in benzene and ethylenediamine (EDA). The final products were characterized by X-ray powder diffraction(XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM). The effects of the solvent, reaction temperature and time on the morphology and phase of the products have been discussed.     

Morphological Profiling Identifies the Motor Protein Eg5 as Cellular Target of Spirooxindoles

Oxindoles and iso-oxindoles are natural product-derived scaffolds that provide inspiration for the design and synthesis of novel biologically relevant compound classes. Notably, the spirocyclic connection of oxindoles with iso-oxindoles has not been explored by nature but promises to provide structurally related compounds endowed with novel bioactivity. Therefore, methods for their efficient synthesis and the conclusive discovery of their cellular targets are highly desirable. We describe a selective Rh^III-catalyzed scaffold-divergent synthesis of spirooxindole–isooxindoles and spirooxindole–oxindoles from differently protected diazooxindoles and N-pivaloyloxy aryl amides which includes a functional group-controlled Lossen rearrangement as key step. Unbiased morphological profiling of a corresponding compound collection in the Cell Painting assay efficiently identified the mitotic kinesin Eg5 as the cellular target of the spirooxindoles, defining a unique Eg5 inhibitor chemotype.     

溶剂热合成法制备Mn3O4纳米粉体

溶剂热合成法制备Mn3O4纳米粉体;四氧化三锰;纳米粉体;溶剂热合成     

溶剂热合成法制备(Zn,Hg)S微晶和薄膜

近年来，由于Ⅱ～Ⅵ族半导体纳米材料的特殊物理、化学性质及其在半导体、光学器件、激光二极管、IR探测器等方面的广泛应用，它们的制备和表征引起了人们越来越大的兴趣犤１～１１犦。现在（Zn，Hg）S微晶正被广泛而深入的研究和应用。例如：一种发蓝光的激光二极管已经设计成功，它包含一夹在两衬层间的活性层，无论是在衬层还是在活性层中都包含有（Zn，Hg）S犤５犦。Sugao也曾报道过一种以（Zn，Hg）S为基础的半导体激光器件犤６犦。Parkin曾用MCl２（M＝Zn，Cd，Hg）和Li２E（E＝O，S，Se，Te）混合热解法制备ME或MxM'yS…     

Synthesis,X-ray structure,in vitro HIV and kinesin Eg5 inhibition activities of new arene ruthenium complexes of pyrimidine analogs

Three new ruthenium(II)-arene complexes of the general formula [{(η⁶-p-cymene)Ru(L)}₂](Cl)₂), where L are monastrol (L¹), ethyl 4-(3-hydroxyphenyl)-6-methyl-2-thioxo-pyrimidine-5-carboxylate (L²) or its 4-bromophenyl analog (L³), have been synthesized and characterized by elemental analysis, ¹H, ¹³C, and 2-D NMR spectroscopy. The X-ray diffraction study of complex 1 showed the presence of a dicationic diruthenium complex where two thioxopyrimidines act as tridentate μ,κN:κ²S ligand, bridging two Ru ions through the pyrimidine nitrogen and sulfur atoms. All new complexes were evaluated in vitro for their antiviral activity against the replication of HIV-1 and HIV-2 in MT-4 cells using MTT assay. Additionally, complexes 1–3 were screened for their inhibitory activity against the ATPase enzyme and the motor-protein Kinesin Eg5. Complex 1 was found to inhibit microtubule-stimulated ATPase activity of kinesin of IC₅₀ = 30 μM (monastrol, IC₅₀ = 10 μM).     

二氧化钛柱撑蒙脱土的溶剂热合成及光催化活性

以乙醇水溶液为溶剂,以六亚甲基四胺为沉淀剂,以TiCl3为前驱体,通过醇-水溶剂热的方法合成出二氧化钛柱撑蒙脱土复合纳米光催化剂,通过XRD、BET、AAS等对其物相组成、比表面积及元素含量等进行了表征．结果表明,复合光催化剂具有良好的介孔结构,其孔径分布主要集中在6～10nm,且比表面积明显增大．光催化降解亚甲基蓝活性结果表明,当m（TiO2）／m（蒙脱土）=0．2：1时,复合催化剂由于柱化后具有较大的比表面积、孔容和适当的孔分布而表现出良好的光催化活性．     

一种新的有机胺为模板剂的稀土硫酸钐合成，结构表征以及荧光性质

本文采用正丁醇与水的混合溶剂合成一种新的以有机胺为模板剂的硫酸钐盐:[C2N2H10]1.5[Sm(SO4)3(H2O)].2H2O(1),并通过X-射线衍射、红外、热重及元素分析对其进行了表征。该化合物晶体属于单斜晶系,P21/c空间群。其中a=0.65515(9)nm,b=2.648 3(4)nm,c=0.996 15(13)nm,β=104.067 0(10)°,V=1.676 5(4)nm3,Z=4。晶体结构分析显示化合物1中的波浪形层状结构由SmO9多面体与SO4多面体构成,同时非配位水与乙二胺通过氢键连接相邻的两个层。化合物1具有较强的荧光。     

含过渡金属镉或汞的四元硫化物的溶剂热合成及性能

利用溶剂热法合成了2种四元硫化物Rb₂CdSbS₃（SH）（1）和Rb₂HgSb₄S₈（2）。单晶X射线衍射分析表明,化合物1为一维链状结构,由[CdSbS₃（SH）]^2-阴离子和Rb⁺阳离子组成。化合物2为二维层状结构,由[HgSb₄S₈]^2-阴离子和Rb⁺阳离子组成。固体紫外可见漫反射光谱分析结果表明,化合物1和2的带隙分别为2.06和2.15 eV。荧光分析结果表明化合物1和2均具有黄光发射特性。     

两种蓝矾衍生物的合成、结构及光谱性质研究

溶剂热体系下采用咪唑（im）、2,2’-联吡啶（bpy）为配体与硫酸铜合成了2种蓝矾衍生物：[Cu(im)4SO4]n (1)和[Cu(bpy)(H2O)2SO4]n (2),产率分别为67%和82%。重点考察了体系酸度对结构形成的影响,体系中加入的硝酸量分别控制在0.35–0.6 mmol和1.2–1.45 mmol时,得到纯相的1和2。通过元素分析、红外光谱、热重、电感耦合等离子体发射光谱、粉末X射线衍射及X射线单晶衍射测试技术对其结构及性质进行了表征。晶体结构解析表明,化合物1和2均属单斜晶系,C2/C空间群,具有蓝矾结构特征,但由于配体的空阻效应,1呈一维“之”字链状结构,2为一维“一”字链。通过紫外－可见漫反射对其性质进行了测试,结果表明2个化合物在近紫外区有一定的红移,可见光区发生蓝移。     

六方硼碳氮化合物的溶剂热合成与表征

采用溶剂热合成方法,以无水乙腈、叠氮化钠和四氟硼酸钠为原料,以苯为溶剂,在温度为400℃条件下,成功合成出了硼碳氮(BCN)三元化合物.利用X射线粉末衍射(XRD)、Fourier变换红外光谱(FTIR)、透射电子显微镜(TEM)、选区电子衍射(SAED)、X射线能谱(EDS)和电子能量损失谱(EELS)对合成产物进行了表征.XRD和SAED分析表明,合成产物为六方相,晶格常数为a=0.2678nm,c=0.6639nm;TEM结果表明,合成产物中存在纳米棒和四方柱状块体BCN;EELS和EDS分析表明,产物由B,C,N三种元素组成,化学式为B0.23C0.60N0.17;FTIR分析表明样品中存在C—N,B—C和B—N键,表明B,C,N三元素之间达到了原子级化合.     

Solvothermal Synthesis and Crystal Structure of a Zn（II） Microporous Metal-organic Framework

A novel three-dimensional Zn(Ⅱ) coordination polymer, Zn3(C2H2N3)4(SiF6), has been synthesized under solvothermal conditions using 1H-1,2,4-triazole-3-carboxylic acid and zinc fluoride as the starting materials. The complex has been characterized by elemental analysis, IR, TG analysis and single-crystal X-ray diffraction analysis. The complex crystallizes in the tetragonal I4/mmm space group with a=11.592(0), c=7.526(1), V=1011.3(2)3 , Z=2, Mr=610.46, Dc=2.005 g/cm3 and F(000)=596. The final R=0.0312 and wR=0.067 for 319 observed reflections with I>2σ(I). In the title complex, the Zn centers are interconnected by μ 3 -bridging triazole ligands to form a microporous three-dimensional metal-organic framework.     

溶剂热制备氧化锌纳米线

ZnO nanowires were synthesized mildly through an absolute alcohol solvothermal process at 120 ℃ for 12 h using ZnAc₂·2H₂O and NaOH as raw materials and PEG400 as a soft template. The cyrstal structure and morphology of the nanowires were characterized by XRD, SEM, TEM and HRTEM. The results indicate that the diameter of ZnO nanowires is 40 nm, the length can reach 2 μm and the nanowires are of high purity, homogeneity and well crystallinty. The influence of the various factors on the formation of ZnO nanowires and formation mechanism were also discussed.     

溶剂热合成单分散硫化镉纳米晶

在双表面活性剂十八胺和油酸存在条件下, 以氯化镉和硫粉作为反应前驱物, 通过简单的溶剂热方法合成单分散性闪锌矿硫化镉纳米晶, 粒径大小在13 nm. 用X射线衍射(XRD)、透射电子显微镜(TEM)对产物的结构和形貌进行了表征, 同时对硫化镉纳米晶的紫外吸收谱和光致发光谱(PL)性能进行了表征. 实验结果表明合成的样品具有很好的发光性能, 此外溶剂热反应的温度对纳米晶的单分散性有重要影响. 并对硫化镉纳米晶的形成机理做了初步的研究.     

多孔柿饼状BiOBr光催化剂的简易溶剂热法合成（英文）

以硝酸铋和十六烷基三甲基溴化铵(CTAB)为Bi和Br源,采用聚乙烯吡咯烷酮(PVP)辅助溶剂热法首次成功制备了多孔纳米片聚结的柿饼状溴氧化铋(BiOBr)。通过多种分析技术对分级微米结构BiOBr材料的物化性质进行了表征,并对其在可见光照射下降解亚甲基蓝(MB)的光催化活性进行了评价。结果表明,溶剂热时间和PVP的加入量对产物的颗粒形貌和结晶度有显著影响。当加入0.7 g PVP时,120℃溶剂热处理12 h,可得到多孔纳米片聚结的柿饼状BiOBr样品。多孔柿饼状BiOBr样品的比表面积为4 m2·g^-1,带隙能为2.64 eV,在可见光区具有较强的光吸收性能,具有良好的可见光驱动降解MB的光催化活性和稳定性。我们推断,多孔纳米片聚结的柿饼状BiOBr样品具有优良的可见光催化性能,这与该样品的较高比表面积、多孔结构、低带隙能以及独特的颗粒形貌有关。     

一种具有梯状链结构有机模板硫酸铽的合成、结构表征以及荧光性质

本文采用溶剂热法合成了一种具有梯状链结构新的有机模板硫酸铽盐:(C2H8N)[Tb(SO4)2.H2O](1),并通过X-射线衍射、红外、热重及元素分析对其进行了表征。该晶体属于单斜晶系,P21/n空间群。其中a=0.568 1(3)nm,b=1.972 7(10)nm,c=0.862 7(4)nm,β=90.658(6)°,V=0.966 7(8)nm3,Z=4。化合物1的骨架结构由TbO8多面体和SO4四面体构成。S(1)和S(2)与Tb(1)相连接,通过3个S-O-Tb连接构成双链,而相邻的双链通过μ3-O(O5)连接形成一个新的梯状链。