Synthesis,Structure, and Fluorescence of a Novel Samarium Compound

A novel samarium compound, [Sm(Phen)₂(H₂O)₅]₂(Phen)₂(Bipy)Cl₆ · 7H₂O (I) (Phen = 1,10-phenanthroline and Bipy = 2,2'-bipyridine), was prepared by a solvothermal reaction. The crystal structure of I was characterized by X-ray single-crystal diffraction method (CIF file CCDC no. 1025736). Compound I is an isolated structure with the samarium ions possessing a nine-coordinated distorted monocapped square antiprism geometry. There are abundant hydrogen bonding and π–π stacking interactions which connect the molecules together to yield a three-dimensional (3D) supramolecular structure. The fluorescence spectra data reveals that I can display the characteristic emission ⁴G_5/2 → ⁶H _J transitions (J = 5/2, 7/2, 9/2 and 11/2, respectively) of Sm³⁺ ions.     

Synthesis,Structure and Spectra Properties of a Novel BOIMPY Compound

A bis-2-iminopyrrole compound(1) and its difluoroboron complex(2) were synthesized and characterized. The crystal of 2 is in the monoclinic system, P2_1/n space group with a = 21.5113(15), b = 6.3036(3), c = 21.5064(15) ?, V = 2826.3(7) ?~3, Z = 4, C_(26.5) H_(25) B_2 ClF_4 N_4 O, M_r = 548.57, D_c = 1.390 g/cm, F(000) = 1132 and μ(MoKα) = 1.787 mm~(-1). The final R = 0.0647 and wR = 0.1817 for 10346 observed reflections with I 2σ(I), and R = 0.0889 and wR = 0.1993 for all data. The molecules of complex 2 self-assemble through C–H×××F hydrogen bonds and form tubular structures which are filled by CH_2 Cl_2 molecules stabilized by C–H×××π interaction. The UV-Vis spectra of complex 2 show great bathochromic shift compared to that of compound 1 due to the difluoroboron complexing. Complex 2 shows fluorescence emission both in solid state and in solution, whereas compound 1 only exhibits fluorescence emission in solid state.     

一种新型吡啶鎓盐的合成、结构及光学性质

通过吡啶盐与3，4-二甲氧基苯甲醛在甲醇中反应，得到了一种新型的化合物，即4-[（3"，4"-二甲氧基)苯乙烯基]-N-甲基吡啶高氯酸盐，分子式为C16H18ClNO6。化合物的结构通过红外、元素分析、氢谱、电喷雾质谱和X-单晶衍射仪进行分析与表征。结果表明：该化合物属正交晶系，空间群Pbca，晶胞参数a = 13.5897(11) nm, b = 13.9126(11) nm, c = 17.3485(14) nm, α = 90 °, β = 90 °, γ = 90 °, Mr = 355.76, V = 3280.0(5) nm3, Z = 8, F(000) = 1488, Dc = 1.181 g/cm3, μ = 0.265 mm?1。而且还研究了该化合物的光学性质。     

一个新的二氮六元杂环化合物的合成、结构及表征

二氮杂环化合物及其衍生物在配合物的自组装和生物无机等领域中具有诱人的研究前景,因而引起各国化学家的广泛关注．这类化合物的合成可以追溯到60年前,Buhle等首次合成了1,5-二氮环辛烷(DACO)．随后,其一系列衍生物也被合成出来,并应用于配位化学及相关领域的研     

Synthesis and Structure of a Novel Disulfide-Containing Aniline

A novel disulfide-containing aniline, 8-dihydro-1H,4H-2,3,6,7-tetrathia-anthracen-9-ylamine (5) was synthesized.The single-crystal X-ray analysis of 4 indicates that the molecular has a non-planar structure, with its four sulfur atoms out of the plane of benzene ting. The designed molecular has the advantage of high theoretic specific capacity and reversibility,[1,2] when it is to be polymerized and used as the cathode material of the secondary lithium batteries.     

Synthesis, Crystal Structure and Electrochemical Properties of a Novel Phenothiazine Derivative

A new compound 1,1‘-bis(3-pyridyl)-propylene(3,7-diformyl-N-ethylphenothiazinyl)ketone (C30H23N3O2S, Mr = 489.4) has been synthesized, and its crystal structure was determined by single-crystal X-ray diffraction method. The crystal is of orthorhombic, space group Ima2 with a = 27.491 (5), b = 11.942(2), c = 7.389(2) A, V = 2425.8(7) A^3, Z = 8, Dc =1.340 g/cm^3,μ = 0,167 mm ^1, F(000) = 1024, the final R = 0.0363 and wR = 0.0869 for 2054 unique reflections with Rint = 0.0254. The structural determination shows that the molecule assumes a butterfly configuration with nearly planar wings. In addition, the electrochemical study indicates that there is a high electronic delocalization in the molecule.     

新型十八核聚氧钼酸盐的合成与结构

合成了新化合物(NH4)6•[Ca2(H2O)6(CH3COO)2]•{Ca@[O52(OH)4(CH3COO)2]}•14H2O，并运用元素分析和单晶X衍射对其结构进行了表征.测定结果证实,该化合物由十八个钼氧八面体相互连接而成，呈现一种有趣的环状结构.在环的中心有一个Ca2＋离子，它通过与环上的四个酰氧配位而与环骨架相连.有十个钼原子呈正六价，而其余八个钼原子呈正五价，且有Mo－Mo键存在.环上还有配位相连的四个乙酸配体.在环的上下各有两个Ca2＋离子，它通过与该环和其它环上的氧原子配位而把环连成一维链状结构.晶体属三斜晶系，空间群P1，晶胞参数：a=1.055 2(2) nm， b=1.515 0(3) nm， c=1.544 9(3) nm， α=60.84(3)， β=88.00(3)， γ=71.21(3)°，V=2.019 4(7) nm3， R1=0.036 6（对可观察点）， wR2=0.083 3（对独立点）.     

Facile Synthesis and Crystal Structure of a Novel Cyanopyridine

The title compound 2-amino-4-(4-hydroxy-3,5-dimethoxyphenyl)-5-methyl-6-phenyl nicotinonitrile,C 21 H 19 N 3 O 3,was synthesized via four-component reactions between propio-phenone,malononitrile,syringaldehyde and ammonium acetate in ethanol under reflux without catalyst and characterized by IR,1 H NMR,13 C NMR,MS,EA and single-crystal X-ray diffraction.Single-crystal X-ray diffraction analysis shows that the compound is of monoclinic system,space group P2 1 /n with a=8.4600(17),b=17.139(3),c=13.408(3),β=107.06(3)°,V=1858.6(6)3,Z=4,M r=361.39,F(000)=760,μ(MoKα)=0.088 mm-1,D c=1.292 g/cm 3,λ=0.71073,the final R=0.0751 and wR=0.0938 for 3333 observed reflections with I > 2σ(I).The crystal packing of the title compound is stabilized by intermolecular hydrogen bonds.     

新型镍配合物的溶剂热合成及其晶体结构

以2-乙氧基-6-亚氨甲基苯酚(HL)为配体,与氨水和Ni(ClO4)2.6H2O经溶剂热法合成了新型镍配合物[Ni(L)2](1),其结构经IR,元素分析和XRD表征。1属三斜晶系,Pī空间群,晶胞参数a=0.843 3(3)nm,b=1.009 4(2)nm,c=1.188 4(2)nm,α=111.16(3)°,β=97.43(3)°,γ=102.43(3)°,V=0.897 2(11)nm3,Mr=387.05,Z=2,Dc=1 433 g.cm-3,F(000)=404,μ=1.105 mm-1,S=1.015。1中Ni2-分别与两个L-上的两个N原子和两个O原子配位,形成了平面四边形几何构型。分子通过一对N-H┈O氢键形成二聚体;二聚体进一步通过N-H┈O氢键和C-H┈Ni氢键的相互作用形成二维网状结构。     

新型咔唑衍生物的合成及其晶体结构

通过9-乙基咔唑-3-甲醛与4-氨基-3,5-二甲基-1,2,4-三氮唑反应,合成了一种新型咔唑衍生物-- 9-乙基咔唑-3-甲醛缩4-氨基-3,5-二乙基-1,2,4-三氮唑(1),其结构经1H NMR, IR和X-射线单晶衍射表征.1属单斜晶系,P2(1)/n空间群,晶胞参数为:a=8.829(8)(A), b=9.863(10)(A), c=19.530(15)(A), β=101.65(5)°, V=1 666(3)(A)3, Dc=1.266 g·cm-3, Z=4, F(000)=672, μ=0.079 mm-1.最终偏离因子R1=0.075 6.     

Synthesis,Crystal Structure,and Fungicidal Activity of a Novel 1,2,3-Thiadiazole Compound

Abstract

A new 1,2,3-thiadiazole compound, C₁₈H₁₈Cl₂N₄O₂S, has been synthesized and the crystal structure was determined by single crystal X-ray diffraction study. The fungicidal activity of the title compound was determined and the results showed that it displays moderate fungicidal activity.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Synthesis,Structure,and Characterization of a Novel Coordination Polymer with Polythreading Feature

A novel coordination polymer 1 with formula of Zn₂(BDC)₂(TPPA) was built from 1,4-dicarboxybenzene (H₂BDC),tris(4-(pyridin-3-yl)phenyl)amine (TPPA),and Zn(Ⅱ) ion.It was characterized by single-crystal and powder X-ray diffraction,Fourier-transform infrared spectra (FT-IR),thermal gravimetric analysis (TGA),and UV-vis.1 crystallizes in triclinic space group P1 with a=14.589,b=14.606,c=16.108?,α=115.635~o,β=90.328~°,γ=114.662~o,V=2738.6A³,Z=2,M_r=935.52 g/mol,D_c=1.134 g/cm~3,F(000)=956,GOOF=1.062,the final R=0.0685 and w R=0.1817 for 7701 observed reflections with (I>2σ(I)),and R=0.0717 and w R=0.1843 for all data.In 1,Zn(Ⅱ) is coordinated with H₂BDC to form a 2D square grid,and TPPA ligands were arranged above and beneath the 2D layer.Two neighbor layers are interpenetrated each other byπ-πinteractions to generate a polythreading framework structure.Moreover,the photoluminescence of 1 was also studied.     

Synthesis,Crystal Structure and Electronic Structure of Novel Semiconducting KCdAsS_3

A new compound of KCdAsS_3(Mr = 322.60) was successfully synthesized using thiourea reactive flux method. The crystal structure was determined by single-crystal X-ray diffraction. The title compound crystallizes in a monoclinic system of space group P21/n with a = 5.9537(7), b = 16.633(3), c = 6.093(1) ?, b = 90.781(3)°, V = 610.0(1) ?3, Z = 4, Dc = 3.513 g/cm3, m(Mo Kα) = 10.52 mm-1, F(000) = 592, R = 0.057 and w R = 0.136 for 899 observed reflections with I 2σ(I). The crystal structure of KCdAsS_3 features [Cd As S3]-layers, which are separated by K+ ions. First-principles calculations show that KCdAsS_3 is an indirect band gap semiconductor with a band gap of 2.3 e V. The novel layered compound of tetrahedra CdS_4 and pyramids AsS_3 is potentially useful for photoluminescent, photocatalytic and photoelectric applications.     

Synthesis and Structure of Novel Organocycloborates

A series of α,ω‐boryl(bromo)alkanes of the general formula R₂B? (CH₂)_n? Br (n=3, 4, 5, 6) was obtained in high yield following a standard hydroboration protocol. Upon treatment with Mg turnings and formation of the respective Grignard species, all alkanes with n=4 to 6 underwent an unprecedented boron‐centered cyclisation reaction with formation of boratacyclopentanes, ‐hexanes, and ‐heptanes, respectively. All new compounds were isolated in high yields as colourless, crystalline materials and characterised in solution by multinuclear NMR spectroscopy. Four representative examples were chosen for X‐ray diffraction studies, thus providing the first structurally characterised ring systems of that size at a tetraalkyl borate centre.     

一种芴酮衍生物的合成、晶体结构及其光限幅性能

一种芴酮衍生物的合成、晶体结构及其光限幅性能;芴酮衍生物; 单晶结构; 光限幅性能     

含硅氨基甲酸酯衍生物的合成,结构及生物活性

通过１－甲硫基亚乙基氨－甲基氨基甲酸酯与二氯亚砜反应，制得一系列新的含硅氨基甲酸酯衍生物．化合物结构经１￣ＨＮＭＲ、元素分析ＩＲ和ＭＳ确证，测定了化合物３ａ的晶体结构．生物测定结果表明，该类化合物对蚊子、粘虫、玉米螟等多种害虫具有优良的杀虫活性，且与母体灭多威相比，在哺乳动物安全性方面有显著提高．     

一种新颖酰基硫脲金属簇合物的合成与晶体结构

报道了一种新型酰基硫脲金属簇合物[Cu₆(HL)₆] (HL＝N-乙氧羰基-N'-4-氟苯基硫脲)的合成和晶体结构. 对化合物用元素分析、红外光谱、核磁共振谱、差热-热重分析确定了配合物的组成, 并经X射线单晶衍射法确定了其单晶结构. 晶体结构表明, 该化合物属于三斜晶系, 空间群, a＝1.2508(11) nm, b＝1.3011(11) nm, c＝1.4686(12) nm, a＝102.401(14)°, β＝97.859(2)°, γ＝114.700(13)°, V＝2.051(3) nm³, Z＝1, D_c＝1.687 Mg/m³. 标题化合物是由六个铜离子和六个硫脲配体组成的笼状金属簇合物, 每一个硫脲配体上与乙氧酰基相连的氮原子与铜进行配位, 并且配体上硫羰基上的硫原子与铜也发生配位作用, 使它们互相连接形成畸变的多面体结构.     

Synthesis,Crystal Structure,and Spectral Study of a Novel Indenoimidazole Carboxylic Acid Amide

Russian Journal of Organic Chemistry - 3a,8a-Dihydroxy-2,8-dioxo-1,3a,8,8a-tetrahydro-2H-indeno[1,2-d]imidazole-3-carboxamide has been synthesized in 85% yield from ninhydrin and biuret via a green...