双(二苯基膦)烷烃的合成与表征

以三苯基膦为起始原料,四氢呋喃为溶剂,经过金属锂化与烷基化分别合成了1,1-双二苯基膦甲烷(DPPM)、1,2-双二苯基膦乙烷(DPPE)、1,3-双二苯基膦丙烷(DPPP)、1,4-双二苯基膦丁烷(DPPB)、1,5-双二苯基膦戊烷(DPPPe)和1,6-双二苯基膦己烷(DPPH),收率为75%~86%.通过1 H NMR、31 P NMR、MS和元素分析确证了目标化合物的结构.     

纳米ZnO的制备及其气敏性能

螯合物;微乳液;溶胶-凝胶;纳米粒子;纳米ZnO的制备及其气敏性能     

A New One-dimensional Dicyanamide Bridged Zinc(II) Complex Containing Nitronyl Nitroxide Radicals:Synthesis,Crystal Structure and Magnetic Properties

A new one-dimensional dicyanamide bridged zinc(II) complex containing nitronyl nitroxide radicals Zn(NO3)(NIT-1'-MeBzIm)(dca)n·(H2O)n(NIT-1'-MeBzIm = 2-{2'-(l'-me-thyl)benzimidazolyl}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, dca = dicyanamide anion) has been prepared and structurally characterized by single-crystal X-ray diffraction.The complex crystallizes in triclinic, space group P1, with a = 7.428(3), b = 9.839(3), c = 16.708(6), α = 93.270(4), β = 101.642(4), γ = 100.632(4)°, C17.5H21N8O5.5Zn, Mr = 496.79, V = 1169.7(7) 3, Dc = 1.411 g/cm3, μ(MoKα) = 1.096 mm-1, Z = 2, F(000) = 512, R = 0.0583 and wR = 0.1663 for 4295 observed reflections with I > 2σ(I).X-ray analysis reveals that the zinc(II) ion is six-coordinated with a distorted octahedral geometry.These units develop as 1D species where dicyanamide ligands bridge zinc(II) ions.In addition, molecules are linked by π-π piling interactions to form 1-D double-chains.Magnetic investigation indicates that the weak intramolecular interactions are antiferromagnetic with J =-0.27 cm?1, where the spin Hamitonian is defined as H =-2∑i,jJi,jSiS within the complex.     

β-二酮双核铜(I)配合物的合成、结构与性质

室温下,通过还原反应合成了双核铜(I)配合物[Cu(dppm)(ttfac)]2·(C4H8O)2(1),dppm=双二苯基膦甲烷,ttfac=2噻吩甲酰三氟丙酮,研究了配合物的物理化学和光谱性质,并经X射线单晶结构分析,确定了配合物(1)的分子结构,晶体属单斜晶系,空间群P2n,a=1.3000(3),b=1.3730(4),c=2.0372(9)nm,β=94.46(3)°,Dc=1.224gcm3,Z=2,V=3.625nm3,R=0.04493,中心铜离子分别由来自两个不同dppm的P原子和ttfac的两个氧原子形成四面体配位结构。     

Synthesis and Structure of a Cerium Coordination Polymer Templated by Double-Keggin-anion

A porous coordination polymer, {[Ce（dpdo）4（H2O）3]（PMo_12O_40）（dpdo）0.5（H2O）4}n 1 （dpdo = 4,4＇-bipyridine-N,N＇-dioxide）, templated by double-Keggin-type polyanions was synthesized and structurally characterized. The crystal structure was determined by single-crystal X- ray diffraction. The crystal is of triclinic, space group P1 with a = 13.368（4）, b = 16.503（4）, c = 18.506（5）А, α = 88.831（5）, β= 82.095（5）, γ = 83.578（5）°,V= 4018.6（18）А^3, Z=2, C45H50N9O56CeMo12P, Mr = 2935.31, Dc = 2.426 g/m^3, μ= 2.491 mm^-1, F（000） = 2816, the final R=0.0603 and wR = 0.1611 for 11977 observed reflections with I 〉 2σ（I）. Compound 1 exhibits a 3D non-interwoven framework with large cavities housing centrosymmetrically related shoulder-by-shoulder double-Keggin anions as guests.     

溶胶-凝胶法制备小颗粒(Y,Gd)BO_3∶Eu及其表征

用溶胶 凝胶方法制备了平均粒径为 1～ 2 μm的小颗粒、高发射效率的 (Y ,Gd)BO3 ∶Eu红色发射荧光体。用XRD、SEM、粒度分析和PL光谱对荧光体作了表征和研究。常规固相反应合成 (Y ,Gd)BO3 ∶Eu需在 1 2 0 0℃以上才能形成均一的固溶体。而溶胶 凝胶法制取稀土正硼酸盐 80 0℃灼烧已可形成均一的单相 (Y ,Gd)BO3 ∶Eu,在 1 1 0 0℃可得到发光亮度最高的荧光体。它的亮度是常规固相反应于 1 2 0 0℃制得的荧光体的 1 2 0 %。采用溶胶 凝胶法制取 (Y ,Gd)BO3 ∶Eu荧光体 ,可在相当宽的实验条件范围内得到小粒径、窄分布和高亮度的荧光体 ,且有良好的颗粒形貌。     

N,N’-二苯基-N,N’-二(9,9-二甲基芴-2-基)-9-己基-(4,4’-二胺基苯基)咔唑的合成方法及表征

以2,7-二溴咔唑为原料经过N-烷基化、Suzuki偶联反应、Buchwald-Hartwig偶联反应合成了有机发光二极管(OLED)空穴传输材料N,N’-二苯基-N,N’-二(9,9-二甲基芴-2-基)-9-己基-(4,4’-二胺基苯基)咔唑,利用NMR、IR和熔点等分析方法对产物结构进行了表征,并通过TG、UV-Vis及荧光光谱研究了物质的热稳定性和光学性能。     

稀土硝酸盐与苯并15—冠—5和4—皮考林氮氧化物的三元配合物

本文首次合成了稀土硝酸盐与苯并-15-冠-5和4-皮考林氮氧化物的三元配合物。由元素分析确定其化学组成为Ln(NO_3)_3·2(4-picNO)·3H_2O·1/2(B-15-C-5)(Ln=La～Tm)。通过电导、热谱及红外光谱研究,对其物理与化学性质进行了讨论。     

单核零价过渡金属配合物的研究——Ⅱ.含有π-键合醌及双齿氮配体的混配零价钯配合物的合成与表征

本工作合成了一系列十个新的零价钯混配配合物,并对这些配合物进行了表征.研究了配体的立体效应和电子效应的差别,讨论了配体间的相互作用.一.配合物的合成与组成据文献合成dba(PhCH=CHCOCH=CHPh)和Pd_2(dba)_3(CHCl_3).其余试剂及溶剂均为市售商品,用前经无水无氧处理.