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A Deep Analysis on Widely Used Condensation Route for Preparing Aminophosphines: Synthesis and Spectral Characterization of an Aminobis(chlorophosphine), (NC4H8N)[P(i-Pr2N)Cl]2 广泛应用的缩合合成氨基膦途径的深入分析:氨基合成物(氯膦)(NC4H8N)[P(i-Pr2N)Cl]的合成与光谱表征
Pub Date : 2016-04-14 DOI: 10.1080/15533174.2015.1040163
J. Gopalakrishnan
Aminophosphines are useful as ligands and the most convenient method to synthesize is the condensation route that is straightforward, simple and easy to execute and get the products. RxPClz (x = 0–2, y = 1–3) and amines are widely used as phosphorus and nitrogen substrates. Vast examples such as Phx(R2N)yPClz [x < 3; y > 0; z < 3] are available in the literature which used condensation route. A deep analysis was carried out on this route and the author analyzes various parameters that affect product formation, purity, and yield. Using the optimized conditions, (NC4H8N)[P(i-Pr2N)Cl]2 was prepared and spectrally characterized.
氨基膦作为配体是很有用的,而最方便的合成方法是直接、简单、易于执行的缩合途径。RxPClz (x = 0-2, y = 1-3)和胺被广泛用作磷和氮的底物。例如Phx(R2N)yPClz [x < 3;Y > 0;采用缩合途径的文献中有Z < 3]。对这条路线进行了深入的分析,分析了影响产物形成、纯度和收率的各种参数。在优化条件下,制备了(NC4H8N)[P(i-Pr2N)Cl]2,并对其进行了光谱表征。
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引用次数: 1
Halogenation Reactions of Phosphiniminocyclotrithiazenes: Search for New Inorganic Heterocycles 膦亚胺环三噻吩的卤化反应:寻找新的无机杂环
Pub Date : 2016-04-14 DOI: 10.1080/15533174.2015.1066804
J. Gopalakrishnan, U. Swarnalatha, S. M. Rao
Though the chemistry of tetrasulfur tetranitride is very well developed and studied, that of phosphiniminocyclotrithiazenes is not. Reactions of symmetrically substituted R3PN-S3N3 [R = Ph, OC4H8N, MeNC4H8N, and C5H10N] with halogens and halogen sources (SO2Cl2, PhICl2, Br2, and I2) gave rise to various products. In case of R = Ph, the ring-retained product, while for others, ring-degraded products were obtained. A novel cyclotrithiazene heterocycle, [Ph3PN]2S3N3+I3− containing a tetracoordinated sulfur atom with two phosphinimino substituents was obtained, which was further established by IR, NMR (1H-, 13C-, and 31P-) and elemental analysis. Cyclic voltammetric studies indicated the redox behavior as well as the presence of triiodide. Theoretical calculations clearly indicate the residence of maximum positive charge (close to unity) on the tetracoordinated sulfur atom.
虽然四氮化四硫化合物的化学性质已经得到了很好的发展和研究,但磷酰亚胺环三噻吩的化学性质还没有得到很好的研究。对称取代R3PN-S3N3 [R = Ph, OC4H8N, MeNC4H8N, C5H10N]与卤素及卤素源(SO2Cl2, PhICl2, Br2, I2)反应生成多种产物。当R = Ph时,得到环保留产物,当R = Ph时,得到环降解产物。通过红外光谱、核磁共振(1H-、13C-和31P-)和元素分析,得到了一种新型环三噻吩杂环[Ph3PN]2S3N3+I3−,含一个四配位硫原子和两个磷酸亚基取代基。循环伏安法研究表明了氧化还原行为以及三碘化物的存在。理论计算清楚地表明,最大正电荷(接近单位)驻留在四配位硫原子上。
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引用次数: 0
Hydrothermal Synthesis, Crystal Structure, and Luminescent Property of a New Cd(II) Coordination Polymer With Three-Fold Interpenetrated pcu Topology 一种具有三层互穿pcu拓扑结构的新型Cd(II)配位聚合物的水热合成、晶体结构和发光性能
Pub Date : 2016-04-14 DOI: 10.1080/15533174.2015.1004452
Xiuling Feng, Wanping Chen, B. Xiang
A new three-dimensional (3D) coordination polymer, [Cd(pda)(bib)0.5] n(1), [H2pda=1,4-phenylenediacetic acid and bib=1,4-bis(2-methyl-imidazol-1-yl) butane] was prepared by hydrothermal syntheses and characterized by single-crystal X-ray diffraction, FT-IR spectroscopy, and elemental analysis. Crystal structure determination revealed that complex 1 features a threefold interpenetrated pcu framework. Furthermore, the luminescent property for complex 1 is also investigated in solid state at room temperature.
采用水热合成方法制备了一种新的三维配位聚合物[Cd(pda)(bib)0.5] n(1), [H2pda=1,4-苯二乙酸,bib=1,4-双(2-甲基咪唑-1-基)丁烷],并用单晶x射线衍射、FT-IR光谱和元素分析对其进行了表征。晶体结构测定表明,配合物1具有三层互穿pcu框架。此外,还研究了配合物1在室温下的固态发光特性。
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引用次数: 0
Synthesis, Spectroscopic elucidation, Pharmacological and docking studies of N, N'-bis(pyridin-4 ylcarbonyl)benzene-1,2-dicarboxamide ligand based bioactive Copper(II) complexes N, N'-双(吡啶-4羰基)苯-1,2-二羧基酰胺配体生物活性铜(II)配合物的合成、光谱解析、药理及对接研究
Pub Date : 2016-04-05 DOI: 10.1080/15533174.2015.1137040
M. A. Malik, R. Sheikh, M. Wani, S. Al‐Thabaiti, Salman A. Khan
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引用次数: 0
Synthesis and Magnetism of a Dimeric Complex 二聚体配合物的合成及磁性
Pub Date : 2016-04-05 DOI: 10.1080/15533174.2015.1137043
Lu Lu, Wang Jun, Xiren Wu, B. Xie, Yu Wu
A new Cu-based complex of {[Cu2(L)2(phen)2(NO3)]·NO3} (1) (HL = p-hydroxy phenylacetic acid, phen = 1,10-phenanthroline) has been synthesized and structurally characterized. Single-crystal X-ray analyses reveal that compound 1 has a dinuclear Cu(II) unit linking by two carboxylate groups and one nitrate group. The chelating N-donor ligand with phen binds to Cu(II) centers and there is weaker Cu-Cu bond interaction as well. Furthermore, the magnetic property of compound 1 was discussed in detail.
合成了一种新的cu基配合物{[Cu2(L)2(phen)2(NO3)]·NO3} (1) (HL =对羟基苯乙酸,phen = 1,10-菲罗啉),并进行了结构表征。单晶x射线分析表明,化合物1具有双核Cu(II)单元,由两个羧酸基和一个硝酸盐基连接。与phen螯合的n -供体配体与Cu(II)中心结合,存在较弱的Cu-Cu键相互作用。此外,还详细讨论了化合物1的磁性能。
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引用次数: 0
Syntheses, Structures, and Luminescence of Two Complexes 两种配合物的合成、结构和发光
Pub Date : 2016-04-05 DOI: 10.1080/15533174.2015.1137041
Z. Xiang, Tao Wang, Jun Wang, Yu Wu, Yanchun Sun, B. Xie
Two new complexes, namely {[La(L3)3(2,2′-bipy)]n·H2O} (1), and [Zn(L3)2(4,4′-bipy)]n (2) (HL3 = o-hydroxy phenylpropionic acid, 2,2′-bipy = 2,2′-bipyridine and 4,4′-bipy = 4,4′-bipyridine), have been synthesized and structurally characterized by single-crystal diffraction analysis. 1 has a dinuclear motif, which is further linked into 2D layer via the hydrogen bond interactions. 2 shows 1D covalent zigzag chain constructed by 4,4′-bipy ligands. Furthermore, the luminescent properties of 1–2 show the mild emissive power and feature.
合成了两个新的配合物{[La(L3)3(2,2′-bipy)]n·H2O}(1)和[Zn(L3)2(4,4′-bipy)]n (2) (HL3 =邻羟基苯基丙酸,2,2′-bipy = 2,2′-联吡啶和4,4′-bipy = 4,4′-联吡啶),并通过单晶衍射分析对其结构进行了表征。1具有双核基序,通过氢键相互作用进一步连接成二维层。图2显示了由4,4 ' -bipy配体构成的1D共价之字形链。此外,1-2的发光特性显示出温和的发射功率和特征。
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引用次数: 2
Synthesis, Crystal Structures, and Insulin Enhancement of Vanadium(V) Complexes Derived From 2-Bromo-N’-(2-hydroxybenzylidene)benzohydrazide 2-溴- n ' -(2-羟基苄基)苯并肼衍生钒(V)配合物的合成、晶体结构和胰岛素增强
Pub Date : 2016-04-05 DOI: 10.1080/15533174.2015.1137039
Yubin Sun, Qinglan Xie, Wei Li, Yi Ding, Y. Ye
Two new mononuclear vanadium(V) complexes with the formula [VOLX] [X = benzohydroxamate for 1, and X = 8-hydroxyquinoline for 2; L = 2-bromo-N’-(2-hydroxybenzylidene)benzohydrazide], have been prepared. The complexes have been characterized by physicochemical methods and single crystal X-ray determination. The V atoms in both complexes are coordinated by the three donor atoms of L, two donor atoms of X, and one oxo group, forming octahedral coordination. Insulin-mimetic tests on C2C12 muscle cells using biovision glucose assay indicates that the complexes significantly stimulated cell glucose utilization with cytotoxicity at 0.10 g L−1.
两种新的单核钒(V)配合物,其式为[VOLX][1 =苯甲羟酸酯,2 = 8-羟基喹啉];L = 2-溴- n′-(2-羟基苄基)苯并肼]。用物理化学方法和单晶x射线测定对配合物进行了表征。两个配合物中的V原子与L的三个给体原子、X的两个给体原子和一个氧基配位,形成八面体配位。用生物视觉葡萄糖测定法对C2C12肌肉细胞进行胰岛素模拟试验表明,该复合物在0.10 g L−1时显著刺激细胞葡萄糖利用,具有细胞毒性。
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引用次数: 3
Effect Ancillary Ligands on the Zn(II) Complexes: Syntheses, Structure, and Luminescence 辅助配体对Zn(II)配合物的影响:合成、结构和发光
Pub Date : 2016-04-05 DOI: 10.1080/15533174.2015.1137042
Z. Xiang, Tao Wang, Lu Lu, Xiren Wu, Yanchun Sun
Two Zn-based complexes, namely {[Zn(L3)(2,2′-bipy)(H2O)2]n·L3} (1), and [Zn(L3)2(phen)(H2O)] (2) (HL3 = 3-(4-hydroxyphenyl)propanoic acid, 2,2′-bipy = 2,2′-bipyridine and phen = 1,10-phenanthroline), have been synthesized and structurally characterized by single-crystal diffraction analysis. Both 1 and 2 have mononuclear units, which are further linked into different 2D layers via the hydrogen bond interactions. Furthermore, the luminescent and stable properties of 1–2 are also discussed.
合成了两个Zn基配合物{[Zn(L3)(2,2′-bipy)(H2O)2]n·L3}(1)和[Zn(L3)2(phen)(H2O)] (2) (HL3 = 3-(4-羟基苯基)丙酸,2,2′-bipy = 2,2′-联吡啶,phen = 1,10-菲罗啉),并通过单晶衍射分析对其结构进行了表征。1和2都有单核单元,它们通过氢键相互作用进一步连接成不同的二维层。此外,还讨论了1-2的发光特性和稳定性。
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引用次数: 0
Microwave-Assisted Iodination: Synthesis of Heavily Iodinated 10-Vertex and 12-Vertex Boron Clusters 微波辅助碘化:重碘化10顶点和12顶点硼团簇的合成
Pub Date : 2016-04-02 DOI: 10.1080/15533174.2014.988819
M. Juhasz, G. R. Matheson, Paul Chang, Aaron J. Rosenbaum, D. Juers
Microwave-assisted syntheses of heavily iodinated 10-vertex and 12-vertex closo boron clusters are reported. Salts of closo-B10I102−, 1-carba-closo-CHB9H4I5−, 1-carba-closo-CB11H6I6−, 1-carba-closo-CHB11I11−, and B12I122− were prepared in yields of 80% or better. All molecules were characterized by NMR and IR spectroscopy and mass spectrometry. The crystal structure of [Et4N][CHB9H4I5] was determined by single crystal X-ray diffraction. This salt crystallizes in the monoclinic P2(1)/c space group, a = 9.74427(12) Å, b = 20.7512(2) Å, c = 13.06589(17) Å, b = 101.2176(12)°, V = 2591.52(6) Å3, Z = 4, and rc = 2.262 g/cm3.
报道了微波辅助合成重碘化的10顶点和12顶点紧密硼团簇。制备了closo-B10I102−、1-carba-closo-CHB9H4I5−、1-carba-closo-CB11H6I6−、1-carba-closo-CHB11I11−和B12I122−盐,产率达到80%以上。所有分子均通过核磁共振、红外光谱和质谱进行了表征。用单晶x射线衍射测定了[Et4N][CHB9H4I5]的晶体结构。该盐在单斜晶型P2(1)/c空间群中结晶,a = 9.74427(12) Å, b = 20.7512(2) Å, c = 13.06589(17) Å, b = 101.2176(12)°,V = 2591.52(6) Å3, Z = 4, rc = 2.262 g/cm3。
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引用次数: 13
Synthesis, Morphological and Optical Properties of Nano-Crystalline Solid CuxS Thin Films 纳米固相CuxS薄膜的合成、形貌及光学性能
Pub Date : 2016-04-02 DOI: 10.1080/15533174.2014.988815
Swati Mehra, Ajaya K. Singh, Gautam Sheel Thool, V. Ganesan
Metal chalcogenide thin films of copper sulfide (CuxS) were grown on glass substrate using the chemical bath deposition. The CuxS thin film XRD studies reveal chalcocite low and covellite phases called as copper-rich and copper-poor form. The average grain size was calculated in the range of 8.87–69.65 nm. The optical band gap was estimated using Tauc's plot and found to be 3.02–4.06 eV. Optical properties exhibit that film find application in photovoltaic and photo thermal fields. AFM studies show formation of spherical shaped nanoparticle together with fine particles ranging 10 to 500 nm, evenly distributed showing homogeneity in polycrystalline thin film formation. SEM studies reveal spherical grain formation with cracks and pin holes at some places.
采用化学镀液法在玻璃衬底上生长了硫化物金属硫化铜薄膜。CuxS薄膜XRD研究揭示了低辉铜矿和钴矿相,称为富铜和贫铜形式。平均晶粒尺寸为8.87 ~ 69.65 nm。利用Tauc图估计光学带隙为3.02-4.06 eV。光学性质表明,薄膜在光电和光热领域有广泛的应用。原子力显微镜研究表明,在多晶薄膜形成过程中,形成球形纳米颗粒和10 ~ 500 nm的细颗粒,分布均匀,表现出均匀性。扫描电镜研究显示球形颗粒形成,在一些地方有裂纹和针孔。
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引用次数: 3
期刊
Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry
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