Synthesis,Photo-physical Properties and Cell Imaging of Meso-2,6-dichlorophenyl Boron-dipyrromethene Derivatives

The meso-2,6-dichlorophenyl boron-dipyrromethene(BODIPY) derivative 1 was synthesized and characterized by single-crystal X-ray diffraction analysis, 1 H NMR and Esi-HRMS. Compound 1 crystallizes in monoclinic, space group P21/n with a = 8.717(4), b = 20.938(9), c = 12.402(6) ?, β = 98.660(7)°, V = 2237.7(17) ?3, D3 c = 1.333 Mg/cm, F(000) = 936, μ = 0.319 –mm1, Z = 4, the final R = 0.0537 and wR = 0.1556 for 5064 observed reflections with I 2ζ(I). Its photophysical properties were investigated by fluorescence and UV-Vis spectrum. 1 shows high fluorescence quantum yield in different solvents and poor solvent effect. In addition, compound 1 has high values of initial decomposition temperature(298 ℃). Moreover, cell imaging experiments showed 1 is promising for further bioimaging applications.     

基于L-苹果酸铜锌配位聚合物的合成和结构表征

以L-苹果酸为配体,并分别以2,2′-联吡啶和菲咯啉为辅助配体,合成了3个过渡金属配位聚合物{[Zn(mal)(2,2′-bipy)]_2·5H2O}_n(1)、{[Zn(mal)(Phen)(H_2O)]_2·3H_2O}_n(2)和{[Cu(mal)(Phen)]_2·4H_2O}_n(3)(H_2mal=L-苹果酸,2,2′-bipy=2,2′-联吡啶,Phen=菲咯啉),采用X射线衍射技术分别测定了3个配合物的单晶结构,并进行了元素分析、粉末XRD衍射、红外光谱等研究。结果表明配合物1和2均属于正交晶系,空间群均为P2_12_12_1,通过L-苹果酸根桥联金属中心形成一维链结构,2条平行链之间以面对面的方式重叠及通过吡啶环或菲咯啉环之间的π-π弱相互作用形成梯状双链结构;而配合物3属于单斜晶系,空间群为P21,并通过L-苹果酸根桥联Cu(Ⅱ)金属中心及菲咯啉π-π弱相互作用形成双链二维层状结构。     

K2SO4晶体枝状形貌及结晶学模型

生长了具有枝状形貌的K2SO4晶体.基于单偏光显微镜下的形貌观察和背散射电子衍射分析,测定了枝晶的生长方向,建立了K2SO4晶体枝状形貌的结晶学模型.研究表明,K2SO4晶体的生长方向为[111]方向和[(1)-(1)1]方向,且两者夹角为114.4°;发育的晶面为(1(1)0)面,是由[111]晶向和[(1)-(1)-1]晶向组成的晶面.K2SO4枝晶具有两种生长模型,当其作为单枝生长时,一个< 111>方向的枝体连续发育做主枝,另一个<111>方向的枝体不连续发育作为侧枝;当其多枝同时生长时,<111>方向既可作为一个主枝,又可以作为其它主枝的一个侧枝.两种模型均指示出了K2SO4枝晶生长的不对称性.该研究揭示了结晶学方向在枝晶形成过程中的控制作用.     

硫酸钾枝状晶的生长与EBSD测定

采用单玻片溶液蒸发法、双玻片溶液蒸发法以及凝胶法,在不同条件下分别获得了硫酸钾枝晶和枝蔓晶,并利用EBSD技术对硫酸钾枝晶和枝蔓晶的结晶学取向进行了测试和分析.研究表明:硫酸钾(K2SO4)枝晶的主干主要沿着＜ 111＞方向生长;而硫酸钾(K2SO4)枝蔓晶中,组成枝蔓晶的相邻枝晶(晶粒)之间存在典型的双晶关系,其双晶轴为＜011＞,双晶面为(053).     

利用EBSD研究C3S的结构及其纳米结构表征计算

通过X射线粉晶衍射测试及计算得出了C3S的精确晶胞参数和原子坐标,建立了C3S的三维晶体结构模型及准确的C3S晶体的EBSD晶体学数据库文件.经过EBSD测试分析检验证明,该数据库文件可以很好地标定C3S晶体的EBSP图像,并进行其初步的EBSD相测定,测试结果与X射线粉晶衍射得出的结果一致,均为α0=0.7078nm,b0=0.7078 nm,c0=2.4940 nm;α=β=90°,γ=120°,V=1.08205 nm3.根据C3S的三维晶体结构模型,假设C3S纳米微粒具有最小尺度,理论上确定了其最佳纳米尺度,粒径在110 nm左右,厚度值约为387.60 nm.     

双核Cd(Ⅱ)配合物[Cd2(C22H14N4)2Cl2(N3)2]2·H2O的合成与晶体结构

A dinuclear Cd(Ⅱ) complex [Cdz (N3)2LzCl2]2·H2O (1) [L=4'-(4-eyanophenyl)-2,2':6',2"-terpyridine]was synthesized by reaction of ligand L with CdCl2 and NaN3 using solvothermal method and its structure was determined by X-ray crystal structure analysis. The structure indicates that the complex crystallizes in monoclinic, space group C2/c with a=1.644 5(16) nm, b=1.441 9(12) nm, c=1.9181(18) nm,β=100.349(11)°. V=4474(7) nm3, Z=2, Dc=1.570Mg·m-3,μ=1.120 mm-l, F(000)=2 100, and final R1=0.039 3, wR2=0.0811. The result shows a Cd(Ⅱ) ion was sixcoordinated by a tridentate 4'-(4-cyanophenyl)-2,2' :6',2"-terpyridine ligand and one bridging nitrogen atom of the azide group in the basal position and an chloride atom and the other bridging nitrogen atom of the azide group in the axialone, to form a distorted octahedral-pyramidal geometry. CCDC: 673291.     

N,N-二(2-吡啶甲基)胺基三聚茚衍生物的合成及对铜离子、镍离子的选择性识别

以二(2-吡啶甲基)胺(DPA)和三聚茚为原料,设计合成了一种"turn-off"型荧光探针化合物6,表征了其结构,研究了它对不同金属离子的识别作用.结果表明,化合物6对Cu2+和Ni2+具有较高的灵敏性和选择性,在N,N-二甲基甲酰胺(DMF)/H2O(V/V=8/2,p H=7.0)溶液中对Cu2+、Ni2+显示出荧光淬灭效应,且对Cu2+检测几乎不受其他金属离子的干扰;高分辨质谱证明化合物6与Cu2+、Ni2+结合计量比为1∶1;化合物6对Cu2+的检测极限可低至28 nmol/L,对Ni2+的检测极限可低至41nmol/L,检测极限均低于世界卫生组织(WHO)规定的饮用水中两种离子最大含量,有潜在的应用价值.     

化合物[2，6-bis(benzo[1，2-d：4，5-d′]diimidazole-2′-yl)pyridine]的合成、晶体结构和光物理性质(英)

A new tridentate benzimidazole derivative, 2,6-bis (benzo[1,2-d:4,5-d′]diimidazole-2′-yl) -pyridine (Bzdiimpy), was prepared from o-phenylenediamine in five steps with improved methods according to the literature in good yield. The crystal structure was determined by X-ray diffraction analysis. It crystallized in monoclinic, space group P2₁/c, with a=1.170 8(4) nm, b=2.479 6(9) nm, c=1.215 9(4) nm, β=114.641(7)°, Z=1, R=0.035 0, wR₂=0.089 0. The bzdiimp molecule displayed an almost planar structure and formed a zig-zag chain through weak interactions between imidazole-N and [SnCl₆]^2--Cl. Its electronic absorption and emission spectra were measured and compared with the reported analogue 2,6-bis (benz[1,2-d:4,5-d′]imidazole-2′-yl)-pyridine (Bzp). CCDC: 239203.     

Meso位单取代卟啉及其配合物的合成、表征和光谱性质

设计合成了一系列新型的meso位N,N-二甲氨基苯基或N-苯基咔唑基单取代卟啉（5a~c）及其锌配合物（6a~c）,用高分辨质谱、¹H NMR、紫外-可见光谱及X射线单晶衍射方法等对结构进行了表征;研究了卟啉化合物及其配合物的热稳定性及荧光性质。结果表明,这些卟啉化合物及其锌配合物在400~410 nm之间具有强的吸收且具有很好的热稳定性,荧光量子产率在0.05~0.09;另外还分析了meso位不同取代基对光谱性质的影响。