Syntheses and X-Ray Crystal Structures of Cassiferaldehyde and Analogs

Cassiferaldehyde, a recently discovered naturally occurring tyrosinase inhibitor, and six of its analogs, in which the aldehyde group has been replaced by various other functionalities, have been synthesized by a short and simple sequence starting from 2,3-dihydroxybenzaldehyde. Single-crystal x-ray structures of cassiferaldehyde as well as its methyl ketone, nitrile, and carboxylic acid analogs are reported.     

Syntheses and X-Ray Crystal Structures of 2-Aminoindenes and Aminocymantrenes

Substituted 2-aminoindenes have been synthesized in almost quantitative yields by reactions of amines such as methylpiperazine, trimethylethylenediamine, 1,4-diaza-cycloheptane and N,N′-dimethylethylenediamine with 2-indanone. The 2-aminoindenes can be deprotonated and reacted with BrMn(CO)₃(Py)₂ to produce the respective aminoindenyl-cymantrenes in yields between 55–70%. The X-ray crystal structures of 2-(methylpiperazine)indenyl-cymantrene 5 (P1 , a = 12.667(3) Å, b = 16.630(3) Å, c = 17.382(3) Å, α = 72.70(3)°, β = 74.59(3)°, γ = 88.66(3)°, V = 3364.1(12) Å ³, Z = 8, R1(2σ(I)) = 4.02%, wR2(2σ(I)) = 10.30%) and the HClO₄ adduct of 2-(trimethylethylenediamine)-indenyl-cymantrene 6 (Cc, a = 23.722(5) Å, b = 6.9080 Å, c = 13.264 Å, β = 111.77(3)°, V = 2018.6(7) Å 3, Z = 4, R1(2σ(I)) = 2.94%, wR2(2σ(I)) = 7.90%) were determined. In both complexes the indenyl-carbon bonded to nitrogen displays significantly longer bonds to manganese [223.5(3)–225.8(3) pm] than the other four carbon atoms [213.3(3)–219.1(3) pm]. The short indenyl-nitrogen bonds of 136.2(4) and 137.8(4) pm are indicative of a substantial multiple bond character. The complexation of Zn²⁺ by the nitrogen atoms of 6 results in significant shifts of the CO stretching frequencies.     

Syntheses and Crystal Structures of Two New Macrocyclic Compounds

Two new macrocyclic compounds, [Cu2(L)2](ClO4)4·2CH3OH (1) and [Cu(L)](ClO4)2·2H2O (2) (L = 1,3,10,12,15,18-hexaazatetracyclodocosane) were synthesized by condensation reactions involving amines and formaldehyde in the presence of copper anion. Compound 1 crystallizes in triclinic, space group Pí with a = 10.442(2), b = 14.197(3), c = 17.388(4), α = 91.218(4), β = 90.69(3), γ = 93.756(4)o, V = 2520.4(9)3, Z = 2, F(000) = 1260, Dc = 1.589 Mg/m3, Mr = 1205.92, μ = 1.137 mm-1, λ = 0.71073, the final R = 0.0668 and wR = 0.1573 for 9703 observed reflections with I > 2σ(I). Compound 2 crystallizes in monoclinic, space group C2/c with a = 16.911(2), b = 11.4172(15), c = 27.059(4), β = 107.787(2)o, V = 4974.7(12)3, Z = 8, F(000) = 2504, Dc = 1.610 Mg/m3, Mr = 602.92, μ = 1.155 mm-1, λ = 0.71073 , the final R = 0.0419 and wR = 0.1131 for 4374 observed reflections with I > 2σ(I).     

Syntheses and Structures of Two Copper Compounds Supported by Octamolybdate

1INTRODUCTION More and more chemists have currently been inte-rested in the transition metal oxides(so-called polyoxometalates)mainly owing to their structural varieties and promising potential applications in catalysis,biology,medicine and materials science[1].Of the various polyoxometalate structures,the most interesting one is the molybdate family with a va-riety of structural polymers including{Mo2},{Mo4},{Mo6},{Mo8}.etc.These molybdate polymersmight act as versatile building blocks …     

Syntheses, Crystal Structures and Properties of Two Lanthanide Selenite-carboxylate Compounds

Two lanthanide selenite-carboxylate （LSC） compounds, namely, [Ln8（SeO3）4（2,6- pdc）8（H2O）10]·2H2O （Ln = Pr 1, Sm 2; 2,6-pdcH2 = pyridine-2,6-dicarboxylic acid） have been hydrothermally synthesized and structurally characterized. Both compounds possess two-dimensional layer structures constructed by Ln8（SeO3）4（2,6-pdc）8（H2O）10 clusters connected to each other via bridging carboxylate groups. The structures are further extended into three-dimensional architectures through extensive inter-layer H-bonding between coordinated water molecules and carboxylate groups. The luminescent properties and thermal stability of both compounds have been investigated.     

Cd-Ln杂双核配合物的合成、结构及发光性质

采用混合溶剂热方法合成了3个新颖的杂双核d-f配合物, [LnCd(C8H7O3)5(phen)(H2O)](Ln=Dy(1), Pr(2), Gd(3); C8H7O3=对甲氧基苯甲酸根, phen=1,10-菲啰啉), 通过单晶X射线衍射确定了配合物的晶体结构. 结果表明, 3个化合物是同构的. 在同一个分子中, Cd2+与Ln3+通过3个对甲氧基苯甲酸根桥联, Cd2+为五配位, Ln3+为八配位. 在晶体中, 两个相邻的分子被氢键连成二聚体. 测定了3个配合物在室温下的IR, UV-Vis-NIR以及激发和发射光谱. 对比分析了化合物的UV-Vis-NIR吸收光谱与发射光谱的关系, 讨论了d-块(d-L部分)对Ln3+发光的影响.     

由芳香羧酸和4,4'-二(1-咪唑基)苯砜为配体构筑的两个配合物的合成、晶体结构及荧光性质

通过水热法得到了2个配位聚合物{[Cd(L)(oba)]·3.5H₂O}_n(1)和{[Cd(L)₂](p-bdc)}_n(2)(L=4,4’-二(1-咪唑基)苯砜,H₂oba=4,4’-联苯醚二甲酸,p-H₂bdc=对苯二甲酸),对它们进行了元素分析、红外光谱分析,并利用X射线衍射测定了它们的单晶结构。晶体结构分析表明,配合物1具有四连接二重穿插的三维网络结构,其拓扑为{6⁵·8}。配合物2具有四连接的二维结构,其拓扑为{4⁴·6²}。此外,在室温下对2个配合物进行了荧光分析。     

由芳香羧酸和4,4'-二(1-咪唑基)苯砜为配体构筑的两个配合物的合成、晶体结构及荧光性质

通过水热法得到了2个配位聚合物{[Cd（L）（oba）]·3.5H₂O}_n （1）和{[Cd（L）₂]（p-bdc）}_n （2）（L=4,4＇-二（1-咪唑基）苯砜,H₂oba=4,4＇-联苯醚二甲酸,p-H₂bdc=对苯二甲酸）,对它们进行了元素分析、红外光谱分析,并利用X射线衍射测定了它们的单晶结构。晶体结构分析表明,配合物1具有四连接二重穿插的三维网络结构,其拓扑为{6⁵·8}。配合物2具有四连接的二维结构,其拓扑为{4⁴·6²}。此外,在室温下对2个配合物进行了荧光分析。     

一系列基于杂多酸构筑的配合物的合成,晶体结构及光催化性能

通过引入菲咯啉衍生物配体并改变反应体系中的金属盐,得到了3个新的含有杂多酸的金属-有机配合物（MOCs）,{[Cu₂（Do）₂（H₂O）₄(SiW₁₂O₄₀)]·10H₂O}_n（1）,[Ag₃（Do）₅][Ag（Do）₂](SiW₁₂O₄₀)（2）,[Cu₂（Do）₄（H₂O）₂Cl](PMo₁₂O₄₄)·2CH₃OH（3）（Do=1,10-菲咯啉-5,6-二酮）。在配合物1中,Keggin型杂多酸与Cu（Ⅱ）连接形成了二维网状结构。配合物2中的Ag（Ⅰ）显示了多种不同的配位模式,构建了一个新颖的线性三核簇状结构。在配合物3中,Cu（Ⅱ）通过氯原子连接形成了一个双核结构。结构多样性表明金属离子与第二配体Do在构建不同结构的POMs中起到很重要的作用。光催化研究表明,配合物3不仅能在UV光照射下有效地催化降解罗丹明B（RhB）,而且很稳定,能够从反应体系中分离以循环利用。     

一系列基于杂多酸构筑的配合物的合成, 晶体结构及光催化性能

通过引入菲咯啉衍生物配体并改变反应体系中的金属盐, 得到了3个新的含有杂多酸的金属-有机配合物(MOCs), {[Cu₂(Do)₂(H₂O)₄(SiW₁₂O₄₀)]·10H₂O}_n (1), [Ag₃(Do)₅][Ag(Do)₂](SiW₁₂O₄₀;2), [Cu₂(Do)₄(H₂O)₂Cl](PMo₁₂O₄₄)·2CH₃OH (3)(Do=1, 10-菲咯啉-5, 6-二酮)。在配合物1中, Keggin型杂多酸与Cu(Ⅱ)连接形成了二维网状结构。配合物2中的Ag(Ⅰ)显示了多种不同的配位模式, 构建了一个新颖的线性三核簇状结构。在配合物3中, Cu(Ⅱ)通过氯原子连接形成了一个双核结构。结构多样性表明金属离子与第二配体Do在构建不同结构的POMs中起到很重要的作用。光催化研究表明, 配合物3不仅能在UV光照射下有效地催化降解罗丹明B(RhB), 而且很稳定, 能够从反应体系中分离以循环利用。     

Syntheses and Crystal Structures of 9-Ethyl-1,3,6,8-tetra-aryl-9H-carbazole Compounds

The title compounds 9-ethyl-1,3,6,8-tetra-p-tolyl-9H-carbazole (1) and 9-ethyl-1,3,6,8-tetrakis-(4-fluoro-phenyl)-9H-carbazole (2) were synthesized and characterized by single-crystal X-ray diffraction. Thereinto, the crystal structures of compounds 1 and 2 were composed by asymmetry units. The ratio of compounds 1 and 2 to the solvent molecule cyclohexane (CYH) is 4/3. X-ray analysis reveals that the 1,3,6,8-phenyl groups are distorted at large angles relative to the planar carbazole ring. Furthermore, the luminescent and thermal properties of 1 and 2 have also been investigated. It can be seen that thermal stability of compound 1 with p-tolyl is better than that of 2 with 4-fluoro-phenyl. Fluorescence spectra analysis showed that compounds 1 and 2 have strong UV emission.     

Aryl Compounds of Pentavalent Antimony: Syntheses,Reactions, and Structures

Russian Journal of Coordination Chemistry - The synthesis methods, some reactions, and specific features of the structures of aryl compounds of pentavalent antimony and examples of their possible...     

聚酰亚胺的预聚体—聚酰胺酯的研究进展

聚酰胺酯是聚酰亚胺的重要预矛体，本文介绍和讨论了芳香聚酰胺酯的合成方法，物理化学性质及其在微电子等高技术领域的应用。     

Syntheses and Crystal Structures of Two Coordination Polymers with Aromatic Dioxide as Bridge Ligands

Two coordination polymers, namely, two-dimensional complex 1 {[Cu(μ- L)1.5(ClO4)2(H2O)].(H2O)0.5}n (L = pyrazine-1,4-dioxide) and one-dimensional complex 2 [Co(μ-L)Br2(H2O)2]n, have been synthesized with pyrazine-1,4-dioxide as bridging ligands, and their crystal structures were determined by X-ray crystallography. Crystal data for complex 1: monoclinic system, space group C2/c, with a = 23.310(3), b = 12.2338(17), c = 10.6075(15) , β = 110.487(2)°, V = 2833.6(7) 3, Z = 8, C6H9Cl2CuN3O12.5, Mr = 457.60, Dc = 2.145 g/cm3, F(000) = 1832 and μ = 1.998 mm-1; and those for 2: monoclinic system, space group C2/c, with a = 11.012(3), b = 7.483(2), c = 11.451(3) , β = 101.654(4)°, V = 924.2(4) 3, Z = 4, C4H8Br2CoN2O4, Mr = 366.87, Dc = 2.637 g/cm3, F(000) = 700 and μ = 10.487 mm-1. 1 shows a two-dimensional sheet structure on the ac plane through the coordination of μ-L bridging ligands with Cu(II) ions, while 2 displays a zigzag one-dimensional chain along the c axis via the coordination of μ-L bridging ligand with Co(II) ions. Hydrogen bonds in 1 and 2 make the sheets (or chains) connect each other to form a three-dimensional structure.     

New Tetracobalt Cluster Compounds for Electrocatalytic Proton Reduction: Syntheses,Structures, and Reactivity

Reaction of Co₂(CO)₈ and 1,3‐propanedithiol in a 1:1 molar ratio in toluene affords a novel tetracobalt complex, [(μ₂‐pdt)₂(μ₃‐S)Co₄(CO)₆] (pdt=‐SCH₂CH₂CH₂S‐, 1 ), which possesses some of the structural features of the active site of [FeFe]‐hydrogenase. Carbonyl displacement reaction of complex 1 in the presence of mono‐ or diphosphine ligands leads to the formation of [(μ₂‐pdt)₂(μ₃‐S)Co₄(CO)₅(PCy₃)] ( 2 ) and [(μ₂‐pdt)₂(μ₃‐S)Co₄(CO)₄(L)] [L=Ph₂PCH?CHPPh₂, 3 ; Ph₂PCH₂N(Ph)CH₂PPh₂, 4 ; Ph₂PCH₂N(iPr)CH₂PPh₂, 5 ]. Complexes 1 – 5 have been fully characterized by spectroscopy and single‐crystal X‐ray diffraction studies. Cyclic voltammetry has revealed that complexes 1 – 5 show a reversible first reduction wave and are active for electrocatalytic proton reduction in the presence of CF₃COOH. Protonation reactions have been monitored by ³¹P and ¹H NMR and infrared spectroscopies, which revealed the formation of different protonated species. The mono‐reduced species of 1 – 5 have been spectroscopically characterized by EPR and spectro‐electro‐infrared techniques.     

Syntheses and Crystal Structures of two Ring—like {Mo18}Cluster Compounds

1INTRODUCTIONThepolyoxomolybdateshavebeenwidelyresearchedinmanyfieldssuchascatalysis,biology,medicineandmaterialsciencebecauseoftheirrichphysicalandchemicalproperties[1].Thoughmanypolyoxomolybdateshavebeenreported[2],furtherresearchisstillnecessaryforthestudyof搑eduction-oxidation-reconstitution?self-assemblyprocesses[3,4].Polyoxomolybdatesarenormallybuiltupundersuitableconditionsbyafewbuildingblockssuchas{Mo2},{Mo8}and{Mo9}inself-assemblyway[5,6].The{Mo18}clustershaveseveralstructuralty…     

Syntheses,Crystal Structures and Antibacterial Activities of Two Heterocyclic Schiff Base Compounds

Two heterocyclic Schiff bases were synthesized via the condensation reactions of primary amines with carbonyl compounds. 2-[(4-pyridylmethylene)-amino] phenol(compound 1) was synthesized by the interaction of 4-pyridinecarboxaldehyde with o-aminophenol in ethanol solvent; N,N‘-bis(3-(furan-2-yl)allylidene)benzene-1,4-diamin(compound 2) was synthesized by the interaction of 3-(2-furyl)acrolein with p-phenylenediamine in ethanol medium. The compounds were characterized by elemental analysis, IR, MS and single-crystal X-ray diffraction. Compound 1(C12H10N2O) crystallizes in the monoclinic system, space group P21/c with a = 7.0771(7), b = 7.2820(7), c = 19.849(2),β= 96.3390(10)°, V = 1016.66(17) ?3, Z = 4, Mr = 198.22, Dc = 1.295 g/cm3, F(000) = 416, GOOF = 1.060, μ= 0.085 mm-1, the final R = 0.0371 and wR = 0.0929 for 1497 observed reflections with I 2σ(I). Compound 2(C20H16N2O2) crystallizes in the orthorhombic system, space group Fdd2 with a = 26.344(15), b = 48.50(3), c = 5.293(3), V = 6764(7) ?3, Z = 16, Mr = 316.35, Dc = 1.243 g/cm3, F(000) = 2656, GOOF = 1.043, = 0.081 mm-1, the final R = 0.0526 and wR = 0.1267 for 2059 observed reflections with I 2σ(I). 1 and 2 molecules are connected through hydrogen bonds to generate a 2D network and a 1D chain structure, respectively. The preliminary antibacterial activity results showed that the title compounds display excellent antibacterial activities to Escherichia coli, Staphylococcus aureus and Bacillus subtilis.     

Polyamide Layer Chromatography. VIII. Preparation of Polyamide Layer on Poly(ethylene terephthalate) Film and its Application to Aromatic Nitro Compounds

Poly(ethylene terephthalate) film was used as supporter for preparation of polyamide layer. The most convenient method of preparation was described. This layer can be cut into any size and its sensitivity is higher than the glass plate supported layer. Twenty aromatic nitro compounds were used to show the behavior of polyester film based polyamide layer.