吡啶-2-甲酸镍的合成及其晶体结构

以吡啶 2 甲酸和Ni(ClO4)2·6H2O为原料反应制得配合物[Ni(C5H4NCOO)2(H2O)2]2H2O,并通过X 射线衍射法测定其晶体结构.该化合物属于单斜晶系,空间群P21/n,晶胞参数:a=0.97351(15)nm,b=0.52254(8)nm,c=1.4483(2)nm,β=90.119(3)°,V=0.7367(2)nm3,Z=2,Dc=1.690g/cm3,μ=1.362mm 1,F(000)=388,结构偏离因子R1=0.0316,wR2=0.0902,共收集到4771个强度数据,其中1700个独立衍射点,1489个(I>2σ(I))可观测点.X 射线分析表明晶体是由分子间氢键和π π弱相互作用堆积而成的二维层状结构.     

2-乙酰基-6-甲氧基萘的多相催化氢化

乙酰基溴甲基萘;甲氧基萘基;2-乙酰基-6-甲氧基萘的多相催化氢化     

2，6-（2-苯并咪唑基）吡啶与稀土苦味酸盐配合物的合成、晶体结构及荧光性质研究

合成了稀土苦味酸盐（pic）与配体2,6-二（2-苯并咪唑基）吡啶（L）的配合物，通过元素分析、红外光谱及电子光谱对配体及配合物进行了表征，并用X射线单晶衍射测定了配合物[CeL2（pic）2]（pic）·（CH3OH）3的晶体结构．配合物属于三斜晶系，空间群为P1^-，晶胞参数a=1．3795（3）nm，b=2．1292（5）nm，c=2．5651（6）nm，α=105．847（3）°，β=100．150（3）°，γ=107．893（3）°，Z=2，R=0．0519，wR=0．1255．晶体中一个不对称单元内有两个结晶学上独立的分子，这两个分子的构型基本相同，中心Ce^3＋均与两个三齿配位的配体及两个双齿配位的苦味酸根配位，配位数为10．中心Ce^3＋的配位多面体为变形双帽四方反棱柱，两个分子之间以π-π堆积连接，生成一个非中心对称的二聚体．整个晶体则是由这些二聚体以分子间氢键作用连接成三维网状超分子结构．室温下，在紫外光激发下Eu（Ⅲ）配合物固体和溶液均表现出中心离子的特征荧光发射．     

N-二茂铁甲基乙酰胺的合成及其晶体结构

标题化合物(C13H15FeNO)由二茂铁甲酰肟与乙酸乙酯经一锅煮方法制得,其结构通过元素分析,1HNMR,13CNMR,IR和单晶X-射线衍射法确定,化合物具有一维无限链状结构。其晶体属正交晶系,Pbca空间群,M r:257.11,a=9.6101(19),b=9.2313(18),c=25.869(5),v=2295.0(8)3,z=8,D c=1.488Mg.m-3,u=0.71073,F(000)=1072,最终偏离因子为R=0.0517,wR=0.0877。     

2，6－二烷基吡啶类化合物的合成

在金属钠的作用下，通过２，６－二甲基吡啶侧链的烃基化反应，合成了９个新的２，６－二烷基吡啶化合物。化合物的结构经元素分析、ＭＳ、ＩＲ、１ＨＮＭＲ及ＵＶ分析确证     

N，N′-双(4-甲基-2-苯并噻唑基)-2，6-吡啶二酰胺钴(Ⅱ)配合物的合成和晶体结构(英)

Treatment of deprotonated N，N′-bis(4-methyl-2-benzothiazolyl)-2, 6-pyridicarboxamide (L^2-) with CoCl2·6H2O yields the mononuclear complex, (Et₄N)₂[CoL₂]·0.5H₂O. Single crystal X-ray structural determination has been carried out for the complex, crystal system: Monoclinic, space group: P2₁/c, a=1.444(1) nm, b=1.969(1) nm, c=2.448(1) nm, β=118.02(1)°, V=6.143 0(15) nm³, Z=4. In this complex, the central Co(Ⅱ) atom is in an octahedron environment, with four deprotonated amide-N atoms in the equatorial plane and two pyridine-N atoms in the axial positions. CCDC: 252558.     

N,N''''-双(4-甲基-2-苯并噻唑基)-2,6-吡啶二酰胺钴(Ⅱ) 配合物的合成和晶体结构

0IntroductionCobaltcomplexeswithnonmacrocyclicchelatingligandscontainingtheamidefunctionalityhavere鄄ceivedmuchattentioninpastyears[1~3].Somestudieshaverevealedthatdeprotonatednitrogensoforganicamides,beinganionicinnature,arecapableofstabi鄄lizingthetriva…     

稀土胺羧酸配合物的研究 Ⅱ.吡啶-2,6-二甲酸镧配合物的合成及其晶体结构

合成了吡啶-2,6-二甲酸稀土配合物晶体。元素分析表明,化学式为((CH_3)_4N)_2Ln(H_2DPA)_2(DPA)Cl(Ln为La、Ce,Pr、Nd和Sm;DPA为吡啶-2,6-二甲酸根)。用X射线衍射法测定了镧配合物的单晶结构,其结构式为((CH_3)_4N)_2[La(H_2DPA)_2(DPA)]Cl,属正交晶系,空间群Pccn。晶胞参数:α=1.0321(1),b=1.4951(2),c=2.0766(6)nm;V=3.2044(9)nm~3;Z=4。吡啶-2,6-二甲酸以三齿配位,镧的配位数为9,其配位多面体为扭曲的三冠三角棱柱体。     

水杨醛缩2-芴胺席夫碱的合成、晶体结构及生物活性

芴在煤焦油中的含量为1%～2%,全国每年可从中提取1.4万吨芴.芴是一种带有荧光的片状化合物,作为一种新型的发光材料主要用于制备芴基金属化合物、有机光导体、树脂、染料、Ziegler-Natta催化剂的给电子体等.     

双2-乙酰基二茂铁合汞的合成及其晶体结构

标题化合物(C24H22Fe2HgO2)3是由2 氯汞基 1 乙酰基二茂铁与乙二胺反应得到的,其结构通过单晶X 射线衍射法确定。其晶体属三斜晶系,P 1空间群,Mr=1964 12,a=10 193(2),b=11 504(2),c=14 413(3) ,α=92 21(3),β=104 12(3),γ=102 67(3)°,V=1591 55(5) 3,Z=1,Dc=2 049mg/cm3,μ=8 583mm-1,F(000)=942,最终偏离因子为R=0 0859,wR=0 2617。该晶体中同时含有meso型及dl型分子,各分子中Hg原子的配位情况不一样。meso分子中的两个二茂铁是相互平行的,而另两分子dl型的二茂铁是相互垂直的。Hg原子以桥联形式连接两个二茂铁部分。meso型与dl型分子通过Hg O弱配位作用相连。     

5-芳亚甲基海因的微波合成和晶体结构

用芳醛、海因为原料在微波辐射下合成了一系列的 5 芳亚甲基海因 ,产物的结构经红外、核磁共振、单晶X射线衍射分析表征     

Microwave-Promoted Syntheses of Pyridine Carboxamides and tert-Carboximides from Novel 6-Acetylpyridine-2-carboxylic Acid

A novel 6-acetylpyridine-2-carboxylic acid (4) was obtained occasionally during the synthesis of asymmetric ethyl 6-acetylpyridine-2-carboxylate (3) from 2,6-dipiclinic acid (1). Compounds 3 and 4 could transform mutually under some specific conditions. Two reactions of distinctive types occurred when they reacted with the aromatic amines as precursors, due to different functional groups on the 2-position of pyridine in the molecules of 3 and 4: one was Schiff base condensation and the other was an amidation reaction. From the latter reaction, two series of new compounds, pyridine carboxamides (5a–d) and pyridine tert-carboximides (6a–h), resulted. The relevant reaction mechanism is discussed in detail.     

The Rapid Synthesis of Schiff-Base without Solvent under Microwave Irradiation

The chemistry of the carbon-nitrogen double bond plays a vital role in the progresses of chemistry science1. Schiff-base compounds have been used as fine chemicals and medical substrates. Recently multi-dentate complexes of iron and nickel showed high activities of ethylene oligomerization and polymerization2. In our efforts for ligands of polymerization catalysts, synthesis of Schiff-base through classical condensation of aldehydes (or ketones) and amines were pursued, however, the yield o…     

Synthesis and Crystal Structure of 6—Bromo—piperonal—dimethyl—acetal

1 INTRODUCTION 6-Bromo-piperonal-dimethyl-acetal is an intermediate used for the synthesis of natural products, such as podophyllotoxin[1] and the related compounds[2～6] due to the useful biological activities associated with some of its derivatives[7, 8]. In particular, glycoside derivatives of 4?dimethyl- 4-epipodophyllotoxin have been used in cancer chemotherapy[9, 10]. The title compound has been synthesized from raw material piperonal, after bromo substitution and acetal protection…     

6-氟-2,4-二苯基喹啉的合成与晶体结构

合成了一种新的喹啉衍生物6-氟-2,4-二苯基喹啉(FDPQ),并且测定了该化合物的晶体结构.该晶体属于单斜晶系,P2(1)/c空间群.     

Synthesis and Crystal Structure of Hg5Sb2I6

Mercury antimonide iodide, Hg₅Sb₂I₆, previously and erroneously reported as Hg₃Sb₂I₄ was synthesized using standard ampoule technique. A gas-phase transport reaction was applied for preparation of single crystals. Hg₅Sb₂I₆ crystallizes in the space group Pc2₁n (No. 33) with unit cell dimensions: a = 8.108(1), b = 10.702(1), c = 21.295(1) Å. Crystal structure solved using single crystal X-ray data is built of [HgSbI₃] tetrahedra and [HgSbI₂] triangles. All antimony atoms are joined into Sb₂^4? dumbbells. The structure is compared with ones containing similar Sb₂^4? dumbbells.     

Synthesis and Crystal Structure of Cd（tla）（NO_3）_2［TLA＝tris（6－methyl－2－pyridylmethyl） amine］

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＣｄ（ｔｌａ）（ＮＯ_３）_２［ＴＬＡ＝ｔｒｉｓ（６－ｍｅｔｈｙｌ－２－ｐｙｒｉｄｙｌｍｅｔｈｙｌ）ａｍｉｎｅ］ＢＵＸｉａｎ－Ｈｅ；ＺＨＡＮＧＺｈｉ－Ｈｕｉ；ＺＨＵＺｈｉ－Ａｎｇ；ＣＨＥＮＹｕ...     

Synthesis and Crystal Structure of 3，3－Diphenylnaphtho ［1，2－b］furan－2（3H）－one

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ３，３－Ｄｉｐｈｅｎｙｌｎａｐｈｔｈｏ［１，２－ｂ］ｆｕｒａｎ－２（３Ｈ）－ｏｎｅＭｅｎｇＪｉ－Ｂｅｎ；ＷｅｎＺｈｏｎｇ；ＷａｎｇＹｏｎｇ－Ｍｅｉ；ＷａｎｇＲｕ－Ｊｉ；ＷａｎｇＨｏｎｇ－Ｇｅ...     

Synthesis and Crystal Structure of 9-（ 4-M e tho xylphen yl ）-1,8-dioxo-3,4,5,6,7,9hexahydroxanthene under Microwave Irradiation

1INTRODUCTIONInthepastfewyears,potassiumchannelacti-vatorshavegainedincreasingattentionbecauseoftheirclinicalpotentialapplicationsinvariousdiseases.Oneofthemostpotentcompoundsamongthisnewclassofdrugsisthebenzopyranderivativecroma-kalim[1～4].Benzopyranaswellasitsderivativesex-hibitsextensivepharmacologicalandbiologicalacti-vities[5],suchasantibacterialactivities[6,,antitumor7]activity[8],hypotensiveeffect[9],antiproliferationef-fect[10],etc.Thetitlecompoundbearingabenzo-pyranstructuraluni…     

Synthesis and Crystal Structure of △~6－4－Amino－5，6－diphenyl－5－hydroxy－1，2，4－triaza－cyclohexene－3－thione－monohydrate

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ△~６－４－Ａｍｉｎｏ－５，６－ｄｉｐｈｅｎｙｌ－５－ｈｙｄｒｏｘｙ－１，２，４－ｔｒｉａｚａ－ｃｙｃｌｏｈｅｘｅｎｅ－３－ｔｈｉｏｎｅ－ｍｏｎｏｈｙｄｒａｔｅ￥ＬｉｎＺｈｅｎ－Ｇｕａｎｇ；?..