3,5-二甲基-2-(3-氟苯基)-2-吗啉醇盐酸盐的不对称合成及晶体结构解析

以(S)-2-氨基丙醇和(R)-2-氨基丙醇为手性源与α-溴代间氟苯丙酮反应,分别合成手性纯化合物(2R,3R,5S)-3,5-二甲基-2-(3-氟苯基)-2-吗啉醇盐酸盐(4A),(2S,3S,5R)-3,5-二甲基-2-(3-氟苯基)-2-吗啉醇盐酸盐(4B).利用X射线单晶解析仪测晶体结构和空间结构.化合物4A晶体属正交体系,空间群为P21212,晶胞参数a=8.6886(11) nm,b =20.059(2) nm,c=7.6052(8) nm,Z=4,V=1.3255(3) nm3,Dc=1.311 g/cm3,F(000) =552,R1 =0.0257,wR2 =0.0650,S=1.021.化合物4B属于正交体系,空间群为P21212,晶胞参数a=8.6887 (9) nm,b=20.064(2) nm,c=7.6135(7) nm,Z=4,V=1.3272(3) nm3,Dc=1.310 g/cm3,F(000) =552,R1 =0.0356,wR2 =0.0653,S=1.033     

2-苯基-咪唑[4,5]-1,10-菲咯啉的合成和晶体结构

以1,10-菲咯啉-5,6-二酮为原料,合成了标题化合物。通过质谱、1H N M R对其进行了表征。X-射线单晶衍射测试进一步确定了化合物的结构,结果表明：化合物为单斜晶系,空间群P 21/n,晶胞参数：a=1.1492（5）nm,b=1.2622（6）nm,c=1.2506（5）nm,α=90.00°,β=100.354（12）°,γ=90.00°,V=1.784nm 3,Z=4,D c=1.274m-3,μ=0.082m m-1,最终偏离因子：R=0.0467,w R=0.1386。     

化合物2,2’-二硫代二苯甲酸·乙腈的合成与表征

利用水热反应合成了化合物2,2’-二硫代二苯甲酸·乙腈化合物[（H2DTBB）·（CH3CN）]n（1）,H2DTBB=2,2’-二硫代二苯甲酸],并用红外光谱和X-射线单晶衍射对其结构进行了表征,该配合物属单斜晶系,C2/c空间群,晶胞参数为：a=1.6423（3）nm,b=1.2785（3）nm,c=2.1119（4）nm,β=109.12,V=4.1897（15）nm3,Z=4。该化合物是由邻巯基苯甲酸经原位合成H2DTBB与溶剂分子乙腈构成,分子间通过π...π堆积和氢键作用链接形成三维的超分子结构。同时还测定了该化合物的荧光性质和紫外-可见固体漫反射光谱。     

Zn（dpq）2Cl2（dpq=二-吡啶-（3，2-d：2＇，3＇-f）-二氮萘）的水热合成、晶体结构和荧光性质

利用中温水热方法合成了一种未见报道的三维超分子化合物Zn（dpq）2Cl2（dpq=二-吡啶-（3,2-d：2’,3’-f）-二氮萘）．采用元素分析、红外光谱、单晶X射线衍射对化合物的结构进行了表征．结果表明：该化合物属于单斜晶系,C2／c空间群;晶胞参数a=0．84251（6）nm,b=1．24562（6）nm,c=2．26093（11）nm,Z=4,V=2．3648（2）nm^3,R=0．0294,wR：0．0829．该固态化合物在室温下表现出绿色的荧光性质．     

无机-有机杂化化合物[Zn（4,4′-bipy）（2,2′-dpa）]_n的合成和晶体结构

利用中温水热技术合成了一种新型的三维无机-有机杂化化合物[Zn（4,4′-bipy）（2,2′-dpa）]n（4,4′-bipy=4,4′-联吡啶,2,2′-dpa=2,2′联苯二甲酸）,并测定了该化合物晶体结构.结果表明：该化合物属于单斜晶系,C2/c空间群;晶胞参数a=2.0178（4）nm,b=0.95049（19）nm,c=1.1421（2）nm,α=90°,β=117.11（3）°,γ=90°,V=1.9498（7）nm3,Z=8,R1=0.0439,wR2=0.1307.     

N-[(2-羟基-5-甲基苯)(苯基)]亚甲基邻苯二胺的晶体结构及电极反应

合成了N-［(2-羟基-5-甲基苯)（苯基）］亚甲基邻苯二胺,晶体属单斜晶系,空 间群P21/c. 晶胞参数 a = 1.034 0(6) nm, b =1.092 0(3) nm, c =1.472 0(4) nm, β = 107.89(3)°, 化学式C20H18N2O, M r =302.36, Z =4, V =1.581 7(10) nm3 , D c = 1.268 g/cm3, F （000）= 160,最终偏离因子 R1 = 0.054 1. 结构分析表明,分子间以氢键形成二聚体,二聚体 的分子间互为中心对称. 循环伏安法表明标题化合物的电极反应是一个不可逆的单电子传荷 过程.     

离子液体中5-(4-氟苯基)-7,8-二氢化-7,7-二甲基-10-(4-甲苯基)-5H-茚并[1,2-b]喹啉-9,11(6H,10H)二酮的合成及其晶体结构

在离子液体中,由4-氟苯甲醛、5,5-二甲基-3-（4-甲苯氨基）环己-2-烯酮和1,3-茚二酮首次合成标题化合物C34H33FN2O3．其结构通过单晶X射线衍射分析确定．晶体属于单斜晶系,空间群P2,／n,a=1．30147（18）nm,b=0．95006（12）nm,c=2．2985（3）nm,β=102．850（3）°,Mr=536．62,V=2．7709（6）nm^3,Dc=1．286g／cm^3,Z=4,u（MoKa）=0．087mm^-1,F（000）=1136．X衍射分析表明,新形成的吡啶环采用半椅式构象．另外,在晶体结构中还存在非常规分子间氢键C—H…O,连接相邻的分子沿b轴方向形成多聚体．     

5-苄基-4-叔丁基-2-苄亚氨基噻唑的合成及其对环氧合酶-2的抑制活性

5-苄基-4-叔丁基-2-氨基噻唑与芳香醛缩合制备了11 种5-苄基-4-叔丁基-2-苄亚氨基噻唑.结构经1H NMR和元素分析确证, 并用单晶 X-射线衍射测定了化合物Ⅰc的晶体结构.化合物Ⅰc晶体属单斜晶系, 空间群为 P21/n,晶胞参数为:a= 1.437 53(11) nm,b= 0.986 65(8) nm,c=1.465 65(12) nm,β=114.256 0(10)°;Z＝4,V＝1.895 3(3) nm3, Dc＝1.349 g/cm3, F(000)＝808, R1＝0.050 7, wR2＝0.116 3,S＝1.03.体外筛选结果表明,化合物Ⅰb, Ⅰk 在10 μmol/L 浓度下对COX-2的抑制率超过50%.     

2-(2-氮氧化吡啶基)苯并噻唑的合成与晶体结构

通过N-氧化吡啶-2-甲醛与邻氨基苯巯酚反应得2-(2-氮氧化吡啶基)苯并噻唑,并测定单晶结构,化合物分子式为C12H8N2OS.晶体属单斜晶系,空间群P21/c,晶胞参数:a=1.1938(2)nm,b=0.48630(10)nm,c=1.8533(4)nm,β=106.09(1)°,V=1.0338(4)nm3,Z=4,Dc=1.467g/cm3,μ=0.289mm-1,F(000)=472,结构偏离因子R1=0.0446,wR2=0.1035.化合物分子间通过非常规氢键和π-π堆积作用而成二维网状结构.     

反-环己二醇二（吡咯-2-）羧酸酯的合成与晶体结构

合成了反式环己二醇二（吡咯-2-）羧酸酯,利用X-射线单晶衍射技术在室温下测定了该化合物的晶体结构。结果表明,标题化合物处于单斜晶系,C2／c空间群,晶胞参数为：α=1．8327（18）nm,b=0．8553（9）nm,c=1．0122（10）nm,a=γ=90°,β=106．037（12）°,V=1．525（3）nm^3,Z=4。在晶体结构中,环己烷部分采用了椅式构像,同时标题化舍物是G对称的;整个分子通过N—H…O氢键形成一维柱状结构,在C-H…π弱相互作用的帮助下进一步形成二维层状结构;化合物的红外光谱也进一步表明分子间存在N-H…0氢键相互作用。     

Synthesis and crystal structure of new supramolecular adducts of [PtCl6]2− with cucurbit [7] uril: [(H3O)2 (PtCl6)]3 (C42H42N28O14)2·H2O

A novel supramolecular adduct [(H₃O)₂ (PtCl₆)]₃ (C₄₂H₄₂N₂₈O₁₄)₂·H₂O (1) was synthesized by mixing [PtCl₆]²⁻ and cucurbit [7] uril in solution of hydrochloric acid. The crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to orthorhombic system and space group F dd2 with cell dimensions:a=4. 705 33 (5) nm,b=7. 153 80 (6) nm,c=1. 894 61 (2) nm,Z=16,V=63, 7744 (11) nm³,D _c =1.534 g/cm³, μ=3. 007 mm⁻¹,F(000)=29 120,R ₁=0.070 7,wR ₂=0. 169 2. In crystal, the cucurb [7] uril molecules from two zig-zag chains. Foundation item: Supported by the National Natural Science Foundation of China (20172040) Biography: Yan kun (1977-), female, Master, research direction: macrocyclic chemistry.     

二苯环丙烷衍生物的晶体结构与分子结构

用Ｘ射线单晶衍射法测定二苯环丙烷衍生物Ｃ１６Ｈ１２ＮＣｌ晶体结构和分子结构,晶体属正交晶系空间群Ｐｚ１ｚ１ｚ１,晶胞参数ａ＝０．７６８１７（３）ｎｍ,ｂ＝１．１６３０７（４）ｎｍ,ｃ＝１．４２０５７（５）ｎｍ,ｖ＝１．２６９２（７）ｎｍ３,Ｚ＝４．Ｄｅ＝１．３２８ｇｃｍ－３,Ｒ＝０．０４７,ＲＷ＝０．０５０。并讨论了分子结构。     

Synthesis and Characterization of Polyamide-Containing 2, 6- （Substituded） pyridine Derivatives

0 IntroductionPayrriodminaetiics hoenteer oofc ythcleics m .os tC oambupnoduanndts a cnodn tbaeisntin kgno twhnepyridine ring are widely distributedin nature,principally asenzymes and alkaloids . Pyridine enzymes have been foundintissues of all plants and ani mals examined thus far ,andare derivedfromeither nicotinic acid or Vitamin B6[1].Pyr-idine derivatives are also the building block of many phar-maceuticals with a wide range of functionalities that includeantitubercular compounds ,antivi…     

1-甲基海因的合成及其晶体结构分析

以甲胺、 氯乙酸钠、 氰酸钠等为原料, 用“一锅法”合成1-甲基海因, 合成总收率为62.9%.单晶经X射线衍射方法解析, 其晶体属于单斜 晶系, P2₁空间群, 其中a=0.558 9(3) nm, b=1.217 6(6) nm, c=0.809 0(4) nm;β=105.330(7)°;V=0.531 0(5) nm³;Z=4, D_c=1.427 mg/m³, μ=0.116 mm^-1, F(000)=240.     

Synthesis, crystal structure and thermal behavior of Rb(NTO) · H2O

The Rb(NTO)·H₂O crystal has been synthesized by reaction of 3-nitro-1,2,4-triazole-5-one (NTO) with Rb₂CO₃ in aqueous solution. Its crystal structure has been determined. The crystal belongs to monoclinic system. Crystal structure data: space group P2₁ / n; a = 0.633 0(1), b = 0.824 1(2), c =1.296 4(3) nm; β= 97.90(1)°; V = 0.669 9 (2) nm³ , Z = 4, D_c = 2.306 g/cm³, μ= 7.365 nm^-1, F (000) = 448. An eight coordinated compound is formed between Rb⁺ with oxygen atoms and nitrogen atoms. A layer structure is formed by coordination bonds and hydrogen bonds. The thermal decomposition mechanism of this coordination compound is discussed .     

Preparation,crystal structure and quantum chemical investigation of [Li(NTO) (H2O)]

[Li(NTO)(H₂O)₂] was prepared by mixing the aqueous solution of 3-nitro-1,2,4-triazol-5-one (NTO) and lithium hydroxide. The crystal structure of [Li(NTO)(H₂O)₂] was determined by single crystal diffraction analysis. The crystal is monoclinic, space group P2₁/n with crystal parameters of a = 0.742 0(2) nm, b = 0.344 9(1) nm,c = 2.490 6(3) nm, β= 94.89(1)°, Z = 4,D _c , = 1.799 g cm⁻³,V = 0.635 nm³, μ = 1.591 cm⁻¹, F(000) = 392. The finalR is 0.051. The MNDO MO calculation shows that the coordinate bonds of title compound possess certain extent of covalent character. O₂ atom of NTO anion is bonded to Li atom; the nitro group will be lost first when NTO is decomposed.     

K4Sn3Se8的固相合成、晶体结构和反射光谱研究

采用反应性熔盐法，通过中温固相反应在500℃下合成晶体K₄Sn₃Se₈。该晶体属正交晶系，空间群Ccca，晶胞参数：a=0.82115(6)nm，b=2.7790(2)nm，c=0.81865(6)nm，V=1.8682(2)nm³，Z=4。K₄Sn₃Se₈由[Sn₃Se₈]₄三聚体负离子和K⁺正离子组成。漫反射光谱研究表明该材料能隙(Eg)为2.6eV，属于半导体，对太阳能具有选择吸收的特性。     

Hydrothermal synthesis and crystal structure of copper （Ⅱ） coordination polymer composed of helix-like chains： [Cu（NIeH）（bpy）]

Hydrothermal reactions of Cu （Ⅱ） acetate, 2,2＇-bipyridyl （bpy） with 5-nitroisophthalic acid （H2NIPH） resulted in a new coordination polymer [Cu（NIPH）（bpy）] 1. Single crystal X-ray diffraction experiment indicates that 1 possesses a single helixlike chains, of which Cu atoms are coordinated by NIPH ligands and bpy ligands. Compound 1 crystallizes in the space group P2（ 1）/c, a = 0.955（19） nm, b = 1.259（3） nm, c = 1.3737（3） nm, ,6= 95.13（3）°, V= 1.6455（6） nm^3 and Z = 4. The TGA analysis shows that 1 has no remarkable weight loss up to 284℃, as a result of its high thermal stability. Magnetic measurements indicate an antiferromagnetic behavior of compound 1.     

Molecule modification and mass deposition induced by the implantation of low energy Fe+ ion beams into amino acids

Fe⁺ ion beams with the energy of 110 keV were implanted into films of L(+)-cysteine (HSCH₂CH(NH₂)COOH). One of the single crystals grown in hydrochloric acid solution with the implanted samples through slow evaporation was structurally characterized by the X-ray crystallography. The crystal is monoclinic, space group C2, with a = 1.8534(4) nm, b = 0.5234(1) nm, c = 0.7212(1) nm, β= 103.72°, V = 0.67965(3) nm³, Z = 4, F(000) = 144.0, D{clac} = 1.763 g · cm⁻³, μ(MoK _a = 1.06 mm⁻¹, T = 293(2) K. R = 0.0379, wR = 0.0835 for 660 observed reflections (I > 2σ(I)). The structural formula of the crystal compound is (CH₂CH(NH₂)NO₂)ClFe (M _r = 180.38 u). Products of heavy ion beam irradiation were purified and it was directly confirmed that the implanted Fe⁺ ions had been deposited in the novel molecules. The same doses of Fe⁺ ion beams of the same energy were implanted into films of L(+)-cysteine hydrochloride monohydrate. FTIR spectroscopy of the implanted samples proved that some of the original molecules were seriously damaged and significant modifications were induced.     

Chenguodaite （Ag9FeTe2S4）： a new tellurosulfide mineral from the gold district of East Shandong Peninsula,China

Chenguodaite, approved by IMA-CNMMN （2004-042a）, was discovered in the Bunan quartz vein-type gold deposit in the gold district of East Shandong Peninsula. The mineral occurs in high grade Au-Ag-Cu ores, coexisting with galena, chalcopyrite, hessite, electrum, unnamed Ag6TeS2 and AglsFeBiTe3Se, enclosed and replaced by native silver and acanthite. In the reflected light microscope, the mineral has light gray color, indistinguishable anistropism and hardness around 2-3. The color indices of chenguodaite relative to ICE C illuminator are： x=0.3027, y=0.3076, Y=25.78%,λd=474 nm, Pe=3.68%, similar to those of canfieldite. The average chemical composition from 16 microprobe analyses is Ag8.97Fe1.00Te1.99S4.04, idealized to AggFeTe2S4. The polycrystalline X-ray diffraction of chenguodaite by Gandolfi camera and synchrotron oscillation photography results in 67 reflections with the 12 strongest being （relative intensity in bracket）： 6.742（69）, 6.416（39）, 5.951（33）, 3.265（100）, 2.981（24）, 2.649（22）, 2.25（24）, 2.188（71）, 2.142（22）, 2.123（31）, 2.044（23）, 1.949（33）, which are indexed to a primitive orthorhombic cell with a=12.769 （2） A, b= 14.814（2） A, c= 16.233 （1） A, V= 3070.6 A^3, Z= 9, Dcal.=6.85 g/cm^3. The name is for the late Prof. Chen Guoda, a famous Chinese geologist and the founder of Diwa-Geodepression theory of tectonics.