Synthesis and Crystal Structure of 1D Chloride Bridged Cadmium(Ⅱ) Chain

Hydrothermal reaction of 1,10-phenanthroline with CdCl2·2.5H2O in aqueous solution leads to the complex of [Cd(μ-Cl)2(phen)]n (phen=1-10-phenanthroline).The crystal structure has been determined by X-ray analysis.It crystallizes in monoclinic with space group C2/c,a=16.947(3),b=10.529(1)(A),β110.795(3),V=1208.8(3)(A)3,Z=4,Dc=1.997g,cm-3, μ=2.22mm-1,F(000)=704,R=0.0231,Rw=0.626 for 1194 reflections with with I＞2δ(I).In the crystal structure ,the [Cd(phen)]2+ units are bridged by chloride ions to form 1D chain. The 1D chains combine through π…π interactions of phen groups to form 2D infinite molecular zipper.     

Synthesis of Novel Ionic Liquid （[C4CNmim]^＋PF6^-） and Application to Preparation of Polyketone

N-valeronitrile-N’-methylimidazolium hexafluorophosphate ([C 4 CNmim]+ PF 6),as a novel ionic liquid with polar nitrile functional group,was prepared.The structure of the ionic liquid was characterized by using IR and 1 H NMR.As a medium,the ionic liquid plays an important role in copolymerization of carbon monoxide (CO) with styrene (St).Some synthetic conditions were determined,including the usage of ionic liquid,palladium composite catalyst and methanol,CO pressure,reaction time and reaction temperature.The influence of these factors on catalytic activity was analyzed.The results show that the catalytic activity has reached 1 724.1 gStCO/(gPd·h) and the catalyst could be reused 5 times under the optimal condition:composite catalyst 0.015 mmol,ionic liquid 3 mL,methanol 0.75 mL,CO pressure 2MPa,reaction time 2 h and reaction temperature 70℃.This CO/St copolymerization within [C 4 CNmim]+ PF 6 system could facilitate ionic liquids with efficient and economical applications to polymeric materials.     

Synthesis and Characterization of Novel Copolymers Based on 3 （S）-Methyl-Morpholine-2,5-Dione

A series of novel copolymers were successfully synthesized by ring-opening polymerization(ROP) of 3(S)-methyl-morpholine-2,5-dione(MMD) and 5-methyl-5-benzyloxycarbonyl-1,3-dioxan-2-one(MBC) using stannous octoate as catalyst.The copolymers were characterized by means of 1 H-NMR and FT-IR spectroscopy.Gel permeation chromatography(GPC) test shows that the average-number relative molecular mass and average-weight relative molecular mass slightly increase with the increase of MBC content in feed.The results of differential scanning calorimetry(DSC) demonstrate that the glass transition temperature of copolymers increases with the increase of MBC content in copolymers.The copolymers of MMD and MBC are amorphous copolymers,as indicated by DSC results,while the homopolymer of MMD is semicrystalline.     

Synthesis of Schiff bases of naphtha[1,2-d]thiazol-2-amine and metal complexes of 2-（2＇-hydroxy）benzylideneaminonaphthothiazole as potential antimicrobial agents

Objective： A series of 2-benzylideneaminonaphthothiazoles were designed and synthesized incorporating the lipophilic naphthalene ring to render them more capable of penetrating various biomembranes. Methods： Schiff bases were synthesized by the reaction of naphtha[1,2-d]thiazol-2-amine with various substituted aromatic aldehydes. 2-（2＇-Hydroxy）ben- zylideneaminonaphthothiazole was converted to its Co（Ⅱ）, Ni（Ⅱ） and Cu（Ⅱ） metal complexes upon treatment with metal salts in ethanol. All the compounds were evaluated for their antibacterial activities by paper disc diffusion method with Gram positive Staphylococcus aureus and Staphylococcus epidermidis and Gram negative Escherichia coli and Pseudomonas aeruginosa bacteria. The minimum inhibitory concentrations of all the Schiff bases and metal complexes were determined by agar streak dilution method. Results： All the compounds moderately inhibited the growth of Cram positive and Gram negative bacteria. In the present study among all Schiff bases 2-（2＇-hydroxy）benzylideneaminonaphthothiazole showed maximum inhibitory activity and among metal complexes Cu（Ⅱ） metal complex was found to be most potent. Conclusion： The results obtained validate the hypothesis that Schiff bases having substitution with halogens, hydroxyl group and nitro group at phenyl ring are required for the antibacterial activity while methoxy group at different positions in the aromatic ring has minimal role in the inhibitory activity. The results also indicated that the metal complexes are better antibacterial agents as compared to the Schiff bases.     

[Cu~(2+)(phen)(SCN~-)_2]_n配合物的合成及晶体结构

以1,10-邻菲咯啉为配体,合成了标题配合物,该化合物的分子式Cu2+(phen)(SCN-)2,分子量359.90,采用经单色化的Mo ka(λ=0.71073)射线测定,共收集3850个衍射点,其中独立衍射点1555个,[Ι>2ó(I)]可观测点数1233个。结果表明该化合物属单斜晶系,C2/c空间群,其晶胞参数:a=1.4067(3)nm,b=1.03281(18)nm,c=1.02975(18)nm,β=111.104(2)o,V=1.3957(4)nm3,z=4,Dc=1.713g.cm-3,μ=1.859 mm-1,F(000)=724,s=1.024,(Δρ)max=0.307e-3和(Δρ)m in=-0.305e-3。该配合物是四配位的平面四边形结构。     

配合物[Cd_2(bipy)_4(NO_3)_3(H_2O)]NO_3的水热合成与晶体结构

水热合成了配合物[Cd2(bipy)4(NO3)3(H2O)]NO3(bipy=2,2’-联吡啶),并用单晶X-射线衍射测定了其晶体结构.配合物晶体属正交晶系,Pbca空间群,a=1.4361(3)nm,b=1.7215(2)nm,c=3.5099(5)nm,Z=8,Dc=1.708g/cm3,R1=0.0352,ωR2=0.0504.配合物中每一个镉离子均由两个2,2’-联吡啶的四个氮原子和两个氧原子配位构成变形八面体结构.     

三维杂核Ni（II）－Sm（III）配合物的合成、晶体结构及性质研究

利用过渡金属镍盐、稀土盐与5-异烟酰胺吡啶基异酞酸水热合成了杂核化合物{[NiSm2(INAIP)4(H 2 O)4]?2 H 2 O}n (1)(INAIP2－＝异烟酰胺吡啶基异酞酸根),并对其进行了元素分析、IR 及 X-射线衍射法表征。晶体结构研究表明：配合物1属于三斜晶系,P－1空间群。配合物1是由配体异烟酰胺吡啶基异酞酸连接稀土钐离子形成二维层状结构,该二维层通过 Ni-O 和 Ni-N 键连接成三维非贯穿网络结构。配合物1脱水分子后具有稳定微孔结构,对二氧化碳具有一定吸附而对氮气无吸附作用。此外,配合物1还具有典型的稀土钐离子红色荧光性能。     

混配双核铜配合物[Cu（C12H8N2）（C7H5O2）（NO3）]2的合成及晶体结构表征

采用传统溶液法合成了二聚体配合物[Cu（C12H8N2）（C7H5O2）（NO3）]2,其晶体属三斜晶系,P1空间群;晶胞参数为：a=0．87921（10）nm,b=0．91004（10）nm,c=1．16484（13）nm,α=95．7980（10）°,β=111．0080（10）°,γ=95．7870（10）°,V=0．85613（17）nm^2,Z=2,Dc=1．656g／cm^3．铜离子周围有2个氮原子和4个氧原子与之配位形成畸变的八面体配位构型,其中,2个氮原子由邻菲罗啉提供,4个氧原子中3个由配体水扬醛提供,1个由硝酸根提供．两个配位单元通过水杨醛的酚羟基氧原子相连．     

烟酸锌配合物的合成及结构表征

应用水热合成法合成了烟酸锌配合物,通过X-射线单晶衍射对其进行了结构表征,并通过XRD对其纯度进行了分析.X-射线单晶衍射表明,该配合物属正交晶系,空间群为Pbca,晶胞参数为a=1.4229(3)nm,b=0.69191(12)nm,c=0.85012(15)nm,α=90°,β=118.2020(10)°,γ=90°,Z=2,V=737.6(2)3,Mr=381.64,Dc=1.718 mg/m3,μ=1.710 mm-1,F(000)=392,最终R1=0.0189,wR2=0.0532.晶体结构表明,该配合物中中心锌原子是六配位,形成了一个稍微畸变的正八面体构型,通过氢键的作用,标题化合物形成了复杂的三维的网状结构.     

镨与β-丙氨酸配合物的合成及晶体结构

报道了稀土金属Pr与β-丙氨酸配合物的合成、分子结构和晶体结构的测定,具体结果如下:化学式C_(18)H_(50)C_(16)Pr_2 N_6 O_(41),分子式{[Pr_2(β-ala)_6(H_2O)_4](ClO_4)_6·H_2O}_n(β-ala=β-丙氨酸),三斜晶系,Pi空间群,晶胞参数:a=9.388(1)A,b=12.906(2)A,c=21.690(4)A,α=76.90(1)°,β=81.04(1)°,γ=83.23(1)°,Z=2,Mr=1503.18,D_c=1.982g/cm~3.配合物为无限链状分子,Pr(Ⅲ)离子为九配位的单帽四方反棱柱配位多面体.     

新型二价铕配合物的合成及晶体结构研究

通过还原剂保护法合成了二价稀土铕的邻菲咯啉配合物并进行了元素分析、红外等表征,测定了配合物的晶体结构:配合物组成为[Eu(Phen)_2·cl_2],单斜晶系,P2(1)/c空间群,晶胞参数α=9.6039(9)■,b=15.1374(14)■,c=14.6339(14)■,β=99.6170 (10)°,Z=4,Mr=583.27,D_c=1.848 Mg.m~(-3),R_1=0.0629,wR_2=0.2014。铕为6配位,两个邻菲咯啉作为螯合配体参与配位,另两个配位点被Cl原子占有。     

配合物Ni(CSH)_2(EtOH)_2的合成与晶体结构

合成了一个新的含有肉桂醛缩水杨酰腙(CSH)的单核镍配合物Ni(CSH)2(EtOH)2。配合物晶体属于正交晶系,空间群为Pbca,a=18.587(7),b=7.914(3),c=23.395(9),V=3441(2)3,Z=4,F(000)=1432,GOF=1.074,R1=0.0621。配合物分子呈中心对称,中心镍(Ⅱ)形成扭魡曲的八面体构型。     

一例镉双氰胺化合物的合成结构及荧光性质

硝酸镉、双氰胺钠(Na Dca)以及N,N–二甲基乙二胺(Dmda)在水溶液中混合反应得到一个新型配位聚合物[Cd(Dca)2(Dmda)](1).单晶结构分析表明该配位聚合物结晶于P21/c空间群,晶胞参数a=7.446 5(2),b=14.028 3(5),c=12.365 2(4),β=91.476(1)°.该配位聚合物中镉离子通过两种晶体学独立的双氰胺配体的双端配位作用形成了一维双链状结构.进一步地,通过这种双链状结构单元的链内氢键作用以及相邻链单元之间的氢键作用,堆积组装形成了一个结构相对紧凑的三维超分子结构.荧光测试表明,该配位聚合物的荧光发射主要来自于双氰胺配体内部的跃迁.