镍(Ⅱ)三元配合物的合成与晶体结构

利用溶剂热法合成得到一种新的镍配合物[Ni(pht)2(ba)2(H2O)2],通过元素分析、红外光谱、热重分析和X射线单晶结构分析等对配合物进行了表征。该晶体属三斜晶系,空间群为P墿,晶胞参数:a=1.0063(2)nm,b=1.0472(2)nm,c=1.0711(2)nm,α=77.205(3)°,β=74.947(2)°,γ=73.181(2)°,V=1.0302(4)nm3,F(000)=426,Z=1,Dc=1.308Mg.m-3,μ=0.526mm-1,R1=0.0540,wR2=0.1174。配合物分子中每个Ni(Ⅱ)离子以N4O2的六配位形式位于变形的八面体构型中。     

Cr:LiSrAlF_6 晶体生长及其性能表征(英文)

本文报道了布里奇曼法生长的高品质Cr:LiSrAlF6晶体及其激光特性。采用固相氟化反应除去原料中的氧化物和水。在较小的温度梯度和较慢的生长速率下生长出的Cr:LiSrAlF6晶体尺寸达到2 0mm× 130mm。均匀的Cr3 +掺杂浓度为 1～ 15mol%。从XRD谱图计算出的Cr:LiSAF晶体点阵参数为a =0 .5 0 2nm ,c =0 .96 7nm。测试了晶体的吸收曲线 ,并分析了其吸收与能带结构的关系。实现了闪光灯泵浦的Cr:LiSAF激光器运转 ,激光转换斜效率达到 5 .85 %。     

Nd∶NaY(WO4)2激光晶体生长

采用提拉法生长出了四方晶系白钨矿结构的Nd:NaY(WO4)2(简称Nd∶NYW)激光晶体,尺寸为20mm×30mm.通过TG-DTA差热分析得到晶体的熔点为1211℃,从XRD分析得到晶胞参数为a=b=0.5212nm ,c=1.1268nm ,晶胞体积V=0.3062nm3.讨论了Nd∶NYW晶体的生长工艺,给出了晶体生长的最佳工艺参数.通过比较Nd∶NaBi(WO4)2(简称Nd∶NBW)和Nd:NYW的XRD、红外光谱和拉曼光谱测试结果,认为二者结构基本相同,为四方晶系白钨矿结构、I(4)空间群.     

Ho3+掺杂Sc2SiO5激光晶体生长与光谱性能研究

采用提拉法分别生长了具有高光学质量的0.5at;和1.0at;的Ho∶ Sc2SiO5(Ho∶ SSO)激光晶体.研究表明晶体空间群为C2/c,晶胞参数为a=0.99723 nm,b=0.64261 nm,c=1.16843 nm,β=103.9°.Ho3+在SSO基质中的分凝系数为0.82.Ho∶ SSO晶体在2085nm处发射截面为1.12×10-20 cm2,发射光谱呈现一个1850～2150nm的宽发射带.当粒子数反转比率β=0.25时,增益截面σg即开始出现正增益.综合评估了晶体的激光性能,表明Ho∶SSO晶体是一种有潜力的2μm波段激光介质.     

一种新型双核Zn(Ⅱ)配合物的合成、表征及性质研究

选用溶剂热法,以邻羟基苯甲醛缩4-氨基安替比林和Zn(NO3)2·6H2O为原料,成功合成出了一种新型双核Zn(Ⅱ)配合物[Zn2(L-)2(NO3)2](HL为邻羟基苯甲醛缩4-氨基安替比林),并采用单晶X射线衍射、红外光谱、X-粉末衍射、元素分析、热重分析等对该配合物单晶结构进行表征.结果表明:该配合物晶体属于三斜晶系,空间群为P1,晶胞参数a=0.80724(11)nm,b=0.94547(13) nm,c=1.28831(18) nm,α =99.281 (2)°,β=103.814(2)°,y=107.373 (2)°,V=0.8821 (2) nm3,Z =2,Dc=1.633 Mg/m3,F(000) =444,μ=1.432 mm-1,R1=0.0449,wR2=0.1083[I＞2σ-(I)].室温下固态荧光测试显示,配合物具有强的荧光吸收在490 nm(λmax).     

Cr:iSrAlF6晶体生长及其性能表征

本文报道了布里奇曼法生长的高品质Cr:iSrAlF6 晶体及其激光特性.采用固相氟化反应除去原料中的氧化物和水.在较小的温度梯度和较慢的生长速率下生长出的Cr:iSrAlF6晶体尺寸达到φ20mm×130mm.均匀的Cr3+掺杂浓度为1～15mol;.从XRD谱图计算出的Cr:iSAF晶体点阵参数为a=0.502nm,c=0.967nm.测试了晶体的吸收曲线,并分析了其吸收与能带结构的关系.实现了闪光灯泵浦的Cr:iSAF激光器运转,激光转换斜效率达到5.85;.     

新型N-杂环卡宾咪唑盐的合成、表征与抑菌活性研究

以喹哪啶作为桥联基团,合成了五个新型N-杂环卡宾咪唑六氟磷酸盐化合物(5a～5e),其结构经1H NMR,13CNMR表征,用X-ray单晶衍射确定5b、5c和5e的晶体结构.单晶结构分析表明,晶体5b和5c均为三斜晶系、P1空间群;5e晶体为单斜晶系、Cc空间群.5b的晶胞参数:a=6.945 1(10)nm,b=12.0166(18) nm,c=14.791(2) nm,α=91.997(11)°,β=95.340(12)°,γ=105.845(8)°;5c的晶胞参数:a=9.975(3) nm,b=11.056(4) nm,c =12.382(4)nm,α=99.010(4)°,β=103.527(3)°,γ=112.734(3)°;5e的晶胞参数:a=18.058 9(18) nm,b=12.510 0(9) nm,c=13.365 9(12) nm,α=90.00°,β=124.522(7)°,γ=90.00°.抑菌实验结果表明,5a～5e对金黄色葡萄球菌和大肠杆菌有一定的抑制作用.     

Cr,Nd:GSAG晶体生长、光谱及LD泵浦激光性能研究

Cr,Nd:GSAG是一种性能优良的激光晶体,但是关于它的LD泵浦激光性能的研究很少.用提拉法生长了Cr,Nd:GSAG晶体,测定了它的化学成分、结构,初步测试了它的激光性能.晶体的(111)面X射线摇摆曲线半高全宽为0.055°.采用Rietveld方法精修X射线粉末衍射谱得到了Cr,Nd:GSAG晶体的原子结构参数、温度因子等.Cr,Nd:GSAG的最强吸收峰位于808.6nm处,吸收截面为3.38×10-20cm2.808nm光激发下,Cr,Nd:GSAG的最强发射峰位于1060nm,发射截面为6.04×10-20cm2,并测得激光上能级4F3/2的荧光寿命为274μs.利用808nm连续波LD泵浦实现了1060nm的激光输出,在输入功率为8.88W时,最大输出功率为0.513W,斜效率为6.73;,光-光转换效率为5.78;.此外还讨论了Cr,Nd:GSAG晶体中的Cr3+与Nd3+之间的能量传递机理.     

BiIO_4:一种新型红外非线性光学晶体

本文采用水热法,将两种含孤对电子的元素基团I(Ⅴ)与Bi(Ⅲ)复合到一起,合成出一种新型红外非线性光学晶体BiIO4,该晶体属正交晶系,空间群Pca21(29),晶胞参数为a=0.5645(2)nm,b=1.1036(4)nm,c=0.5731(2)nm,α=β=γ=90°。并对其进行了SEM-EDS、XRD、TG-DSC、FT-IR、UV-Vis-NIR、SHG等测试。结果表明,其二阶非线性光学效应(SHG)约为KDP的10倍,红外吸收边可以达到远红外波段(13μm)。     

硒代锡酸盐Cd(tren)SnSe3的溶剂热合成与晶体结构

采用溶剂热法合成了一种新的硒代锡酸盐Cd(tren)SnSe3(tren=三(2-氨乙基)胺).单晶X-射线衍射分析表明该化合物为三斜晶系,空间群为P-1,a=0.7752(3)nm,b=0.8128(2)nm,c=1.2467(4)nm,α=97.299(19)°,β=103.639(18)°,γ=107.325(17)°,V=0.7121(4)nm3,Z=2,Dc=2.865 Mg·m-3,Mr=614.21,F(000)=564.该化合物为零维簇状结构,是由[Sn2Se6]单元的反式末端Se原子连接两个[Cd(tren)]2+单元形成的.紫外-可见漫反射光谱研究结果表明,该化合物的禁带宽度为1.80 eV.     

Mesomorphic Properties of the 4-(4-n-Alkoxybenzoyloxy)-Benzylidene-4-n-Alkoxyanilines and 4-(4-n-Alkoxybenzoyloxy)-3-Methoxy-Benzylidene-4-n-Alkoxyanilines

Transition temperatures, transition enthalpies and X-ray results are reported for 4-(4-n-heptyloxybenzoyloxy)-benzylidene-4-n-alkoxyanilines, 4-(4-n-nonoxybenzoyloxy)-benzylidene-4-n-alkoxyanilines and their 3-methoxy-benzylidene substituted derivatives.     

Vibrational Studies of Gel Grown Ferroelectric RbHC4H4O6 and SrC4H4O6 4H2O Crystals

Single crystals of Rubidium Hydrogen Tartrate (RbHT) and Strontium Tartrate Tetrahydrate (SrTT) have been grown by a gel technique using a chemical reaction method. A controlled reaction has been employed between tartaric acid and feed solution (RbCl for RbHT and Sr(NO₃)₂) at room temperature. The laser Raman and FT-IR spectra of these crystals are recorded in the frequency range 100 - 4000 cm^-1. The presence of tartrate ion, monohydrogen tartrate ion, water molecules and external mode vibrational frequencies are identified and discused. The doublet and broad nature of tartrate ion vibrational frequencies have also been observed and analysed.     

Na+对制备Al4SiC4/Al4O4C复合耐火材料的影响

以焦宝石、活性炭和铝粉为原料,添加Na2CO3制备Al4SiC4/Al4O4C复合耐火材料.采用化学分析、XRD和SEM等测试技术,研究了Na+对材料物相组成和显微结构的影响.结果表明:添加Na2CO3加速了Al2O3和活性炭的反应,促进了Al4O4C的生成.未添加Na2CO3时生成的Al4SiC4晶粒表面光滑,添加Na2CO3后Al4SiC4晶粒粗糙、凹凸,缺陷明显增加.此外,未添加Na2CO3的试样中生成的Al4O4C呈短纤维状,添加Na2CO3后全部转变为细小颗粒.     

New Cluster Precursors—K5 Pyramids and K4 Tetrahedra—for Self-Assembly of Crystal Structures of Mn4(ThMn4)(Mn4)-tI26, Mn4(CeCo4)(Co4)-tI26, and MoNi4-tI10 Families

Crystallography Reports - A combinatorial and topological analysis has been performed, and the self-assembly of the crystal structures of the Mn4(ThMn4)(Mn4)-tI26 (sp. gr. I4/mmm),...     

The Synthesis of Deuteriated 4-n-Alkyl-4′-Cyanobiphenyls

A single synthetic route for chain-deuteriated, totally ring-deuteriated, or per-deuteriated 4-n-alkyl-4′-cyanobiphenyls has been developed. This new route gives better yields than the previously reported route for the synthesis of 4-cyano-4′-n-pentyl-d₁₁-biphenyl and also eliminates the main “impurity” present in the final product. The synthesis of 4-cyano-4′-n-pentyl-d₁₁-2′,3′,5′,6′-tetradeuteriobiphenyl is also reported.     

X-ray Studies on the Liquid Crystalline Phases of the 4-[4-n-Heptyloxy-Benzylidene-Amino]4'-cyanobiphenyl

By means of X-ray diffraction studies of oriented and non-oriented samples the lattice parameters of the orthorhombic cell of the S_E phase as well as of the hexagonal cell of the S_B phase were determined. By packing considerations a bimolecular building unit with oppositely arranged cyano-groups was assumed in the case of the S_E phase. The S_B phase is characterized by an ABAB sequence of the smectic layers in which the molecules are hexagonal arranged. The increasing mobility of the molecules at increasing temperature offers the possibility for a part of the molecules to slide in a more stable dimerized form. In the N_R and S_A phase the existence of monomers as well as of dimers is assumed. In this way a conception of the phase transitions S_E → S_B → N_R → S_A is given on the base of a decrease by steps of the dipole-dipole repulsion.     

The Crystal and Molecular Structure of 4'-Cyanophenyl-4-n-Pentylbenzoate

The crystal and molecular structure of the title compound with the formula C₅H¹¹—C₆H₄—COO—C₆H₄—CN (CPPB) has been determined by X-ray diffraction methods. CPPB crystallizes in the monoclinic space group P2₁/n with eight molecules in a unit cell of dimensions a = 15.268(2) Å, b = 9.165(1) Å, c = 24.031(3) Å, β = 94.67(1)°. The structure has been solved by direct methods and refined to an R value of 0.070.

The CPPB molecules adopt a stretched form and are packed in an approximate parallel imbricated mode, the molecular long axes making an angle of about 5° with the crystal c axis. The molecular geometry and packing are discussed in relation to the mesomorphic behavior of CPPB.     

A Doubly Interpenetrated Layer Structure: 4-Acetamidobenzaldehyde 4-Nitrophenylhydrazone

Abstract  

The title molecule, 4-acetamidobenzaldehyde 4-nitrophenylhydrazone, is essentially planar with the maximum deviations from the least-squares plane through the 22 non-hydrogen atoms being 0.176(1) ? (nitro-O) and −0.152(1) ? (amide-O). The dihedral angle between the benzene rings is 6.93(7)°. The conformation about the C=N bond is E. The presence of amide-H···O-nitro and hydrazine-H···O-amide hydrogen bonding leads to the formation of zigzag 2-D arrays with a pseudo three-connected brick-wall network when viewed normal to the plane of the layer. The layers are sustained by 38-membered {···OCNC₅N₂C₄NO···HNCO···HN₂C₅NH···ONC₄NH} synthons and the rather large voids defined by these are occupied by a centrosymmetrically related layer to result in the formation of a doubly interpenetrated network. These stack along the b direction being connected by C–H···O interactions. The compound crystallizes in the monoclinic space group P2₁/c with a = 10.8152(3) ?, b = 10.9469(2) ?, c = 12.9198(4) ?, β = 113.679(1)°, and Z = 4.