Preparation and Crystal Structure of KFeCl3 and KFeBr3

The preparation and crystal structures of anhydrous KFeCl₃ and KFeBr₃ are described. X-ray diffraction data obtained at room temperature indicate that the two compounds belong to the orthorhombic system, space group Pnma and z = 4. Unit cell parameters are a = 8.712 Å, b = 3.845 Å, c = 14.15 Å for KFeCl₃ and a = 9.220 Å, b = 4.026 Å, c = 14.899 Å for KFeBr₃. Atomic positions were determined.     

碘化苯乙烯吡啶盐的制备与晶体结构

通过碘化1, 4-二甲基吡啶盐与3-甲氧基苯甲醛反应,得到了一种碘化苯乙烯吡啶盐,即碘化4-[3′-(甲氧基)苯乙烯基]-N-甲基吡啶盐,并通过红外、元素分析、氢谱、电喷雾质谱和X单晶衍射仪对其进行分析与表征,结果表明,该化合物属单斜晶系,空间群P21/c,晶胞参数a=6.848 5(16) nm,b=19.707(4) nm,c=10.831(3) nm,α=90°,β=91.069(9)°,γ=90°,Z=4,Dc=1.605 g/cm3,V=1461.5(6) nm3,μ=2.180 mm-1,F(000)=696。     

双缩合螺吡喃的制备与晶体结构

通过过量Fischer碱与3,5-二氯水杨醛反应,得到了一种新型的双缩合螺吡喃(1),即4-(2-亚甲基-1-乙基-3,3-二甲基吲哚啉-2′-基)-6,8-二氯-1′-乙基-3′,3′-二甲基-螺[3,4-二氢-2 H-l-苯并吡喃-2,2′-吲哚啉],并通过熔点、元素分析、IR和X-单晶衍射仪进行表征,确定了该化合物的结构。结果表明:a属单斜晶系,空间群P21/n,晶胞参数a=1.2889(3),b=1.2395(3),c=1.9362(4)nm,β=106.86(3)°,V=2.9603(13)nm3,Z=4,F(000)=1160,Dc=1.228g/cm3,μ=0.247mm-1。     

R-依福地平单晶的制备和结构表征

依福地平外消旋体采用丙酮重结晶,加热溶解澄清后,室温避光静置可顺利获得标题化合物,该纯光学异构体结构经单晶衍射表征。晶胞参数a=9.957 1(3),b=13.187 9(3),c=24.611 7(7),α=β=γ=90°,正交晶系,P2_12_12_1手性空间群,绝对构型参数-0.04(2)。     

Preparation,Crystal Structure,Thermal Decomposition,and Explosive Properties of [Cd(en)(N3)2]n

A new multi‐ligand coordination polymer of cadmium(II) ethylenediamine azide, [Cd(en)(N₃)₂]_n (en=ethylenediamine), was synthesized and characterized by using elemental analysis and FT‐IR spectrum. Its crystal structure was determined by means of X‐ray single crystal diffraction. The obtained results show that this crystal belongs to monoclinic, P2₁/n space group, a=0.6548(1) nm, b=1.0170(2) nm, c=1.2246(2) nm, β=90.23(1)°, V=0.8156(2) nm³, D_c=2.090 g⋅cm⁻³, Z=4, R₁=0.024, wR₂ (I>2σ(I))=0.0416 and S=0.998. The Cd(II) ion is six‐coordinated with four azido ligands by μ‐1, 1 azido bridges, and two ethylenediamine molecules which serve as bidentate ligands through the nitrogen atoms. The thermal decomposition mechanism of the title complex was studied by using differential scanning calorimetry (DSC) and thermogravimetry‐differential thermogravimetry (TG–DTG) techniques. Under nitrogen atmosphere with a heating rate of 10 K⋅min⁻¹, the thermal decomposition of the complex contains two main successive exothermic processes between 519 and 701 K in the DSC curve, and the final decomposed residue at 725 K is Cd. The non‐isothermal kinetics parameters were calculated by using the Kissinger's method, Ozawa–Doyle's method, pervasive integration method, and differential method, respectively. The sensitivity properties of [Cd(en)(N₃)₂]_n were also determined with standard methods.     

混晶结构纳米TiO2粉体的制备与性能表征

以钛酸丁酯为前驱体,采用溶胶-凝胶法制备了具有混晶结构的二氧化钛纳米粉体材料.研究了煅烧温度、pH值对二氧化钛晶型的影响,并用X射线衍射(XRD)、场发射扫描电镜(SEM)、分光光度计等对其进行测试表征.光催化降解性能测试表明:同一pH值下,随着温度的升高,金红石型TiO2的含量增加,锐钛矿型TiO2的含量减少.随着溶胶pH值的减小,TiO2由锐钛矿相向金红石相的转变温度也随之降低.光催化降解亚甲基兰实验表明,锐钛矿含量为76.12%、金红石含量为23.88%时1h内光降解率达98%.     

孔道层状己二酸多聚体的制备及晶体结构

采用水热法,以己二酸和水为原料,在碱性条件下,制备了一种新型的具有孔道二维层状己二酸多聚体。利用X-射线单晶衍射对其结构进行了测定,结果表明:该晶体属于单斜晶系,P1 21/c空间群,a=7.195(4),b=5.150(3),c=10.022(6),α=90.00°,β=111.019(9)°,γ=90.00°,V=346.65(30)3,Z=2,Dc=1.40002 g·cm3,F(000)=156,R gt(F)=0.0371,w R ref(F2)=0.0908。     

1,5-二氨基-3-硝基-1,2,4-三唑的合成及晶体结构

以3,5-二硝基-1,2,4三唑铵盐为原料,经还原、氨化合成出1,5-二氨基-3-硝基-1,2,4-三唑(BANT),总收率为64%,采用红外光谱、核磁共振光谱、质谱以及元素分析等进行了结构表征。培养了BANT单晶,四圆衍射分析表明,BANT晶体属于单斜晶系,晶体空间群为C2/c,晶包参数为:a=11.672(4)nm,b=3.7395(13)nm,β=1.463°,c=13.365(5)nm,V=564.5(3)nm3,Dc=1.696g/cm3。     

The Crystal and Molecular Structure of Dianhydrogossypol

Dianhydrogossypol (4,4′-dihydroxy-5,5′-diisopropyl-7,7′-dimethyl-bis(3H-naphtho[1,8-bc]furan-3-one)) was made by refluxing gossypol in m-xylene. Proton NMR spectroscopy was used to confirm that complete conversion was achieved over a time period of several hours. Single crystals of the compound were obtained by slow evaporation from dichloromethane. Diffraction studies indicate that this crystal form is tetragonal with a I4₁/a space group and with cell dimensions of a = b = 33.8265(4) Å, c = 9.1497(2) Å, V = 10469.4(3) Å³ at 100 K. The structure was solved by direct methods and was refined to an R1 value of 0.0415 on 6,408 independent reflections. Dianhydrogossypol exists as a pair of enantiomers within this structure. The two fused planar ring systems are oriented at a 117° angle to each other (i.e., close to perpendicular), and the isopropyl groups are oriented with the ternary carbon hydrogen atoms pointed inward toward the center of the molecule. Repeating groups of four molecules (of the same chirality) pack to form a helical structure that is supported by intermolecular hydrogen bonds. Each helix is surrounded by four neighboring helices that are composed of molecules of the opposite chirality. The helices form the walls of empty channels that are 5–6 Å wide. As has been found for some gossypol crystal forms, the open-channel structure of dianhydrogossypol might be useful for scavenging or carrying small molecules. Additional NMR studies confirm that dianhydrogossypol can be converted directly to gossypol lactol ethers in the presence of anhydrous alcohols.     

CuO对C3S亚晶尺寸及晶型的影响

以Ca(OH)2、SiO2化学纯为原料,分别掺入不同质量分数的CuO制备不同晶型组成的C3S,运用相图分析、XRD、IR测试方法及MDI jade5.0软件对C3S亚晶生长、晶型转变过程进行研究。结果表明:由CaO-CuO、CuO-SiO2二元相图分析,CuO促进CaO-SiO2固相反应效应明显;C3S经CuO掺杂后,其晶型转变和亚晶成长均受到影响。当CuO掺量小于1.5%时,C3S亚晶尺寸减小趋势明显,大于1.5%时,减小趋势减缓。且C3S晶型随掺量变化先由T型向R型转换,但掺量大于2.0%时,R型又逐步转换为MⅠ型。同时IR分析表明,818 cm-1、999 cm-1谱带处的先减弱后增强及497 cm-1伸缩振动平移先增大后减小,均说明C3S晶体对称性先增大后减小的变化趋势。     

Sr_(1-x)Ca_xRuO_3系列的制备、结构与磁性

固相反应法制备了Sr1-xCaxRuO3 系列 ,X射线衍射确定样品的相结构为正交畸变钙钛矿结构。随Ca替代量x的增加 ,晶格常数a基本保持不变 ,而b和c随之减少 ,晶格畸变更加明显。利用物理性质测量系统 (PPMS)测量了样品的零场冷却 (ZFC)和加场冷却 (FC)磁化强度随温度的变化规律 ,对此规律给出了合理解释。     

SrRuO_3的制备及其结构与磁性

利用固相反应法制备了多晶SrRuO3固体。利用X射线衍射确定样品的相结构为正交畸变钙钛矿结构,空间群为Pbnm。利用最小二乘法求得晶格常数为a=0.5548nm,b=0.5551nm,c=0.7830nm。利用物理性质测量系统(PPMS)测量样品在不同偏磁场下的交流磁化率、零场冷却(ZFC)和加场冷却(FC)磁化强度随温度的变化规律,对此规律给出了合理解释。     

A 3D 3d-4f Heterometallic Coordination Polymer: Synthesis,Crystal Structure and Properties

Abstract  A three-dimensional heterometallic coordination polymer formulated as Sm₂Zn₂(BIPA)₅(H₂O)₂ (1) (H₂BIPA = 5-bromoisophthalic acid) was synthesized by hydrothermal reaction of H₂BIPA with Sm₂O₃ and Zn(NO₃)₂. Complex 1 shows an 8-connected (3⁶.4¹⁸.5³.6) topological network. The thermal analysis of complex 1 has been measured and discussed. Additionally, the photoluminescent property of complex 1 was investigated. Graphical Abstract  An intriguing feature of complex 1 is a 3D eight-connected framework of 3⁶.4¹⁸.5³.6 topology.      

一种三维配位聚合物的水热合成和晶体结构

通过水热合成法获得了La2（H20）4（PDC）2（XO）·2H2O,X射线-单晶衍射结果表明,标题化合物属于单斜晶系,空间群为P2（1）／n,晶胞参数为a=0．77512（16）nm,b=0．9975（2）nm,c=1．5142（3）nm,β=98．50（3）°和Z：4。La（Ⅲ）呈现四方反棱柱体的配位模式,分别和2个来自同一个草酸配体的氧原子、4个来自4个PDC配体的氧原子以及2个来自2个配位水分子的氧原子配位。标题化合物的三维结构是通过草酸配体和水分子配体将二维[La（PDC）]^＋阳离子层连接而成。该三维网络结构中沿着a-轴形成孔道,标题化合物中的自由水分子占据了这些孔道。该化合物在250℃下保持热稳定。     

3-氨基吡嗪-2-羧酸镍配合物的合成与结构

以3-氨基吡嗪-2-羧酸(3-Hapzac)为配体合成了一个镍的配合物[Ni(3-apzac)_2(H_2O)_2],并利用元素分析、IR以及X射线单晶衍射等手段对配合物进行了表征。在配合物中,配位的水分子、羧基和与氨基都参与形成了氢键,通过强的氢键相互作用使配合物形成了三维超分子网络结构。     

The Crystal Structure of a Diacid Triglyceride

The x-ray structure analysis of a single crystal of the β-@#@ form of 2-11-bromoundecanoyl-l, 1- dicaprin has revealed an arrangement of carbon atom chains within a molecular layer that is identical to that found in the β-form monoacid triglycerides. However the packing of the molec-ular layers within the crystal lattice is sub-stantially different because of the unequal fatty acid chain-lengths in the symmetrical diacid triglyceride of this investigation. Insufficient diffraction data owing to difficulty in preparing crystals of adequate size prohibits computation of precise interatomic distances and angles for this triglyceride.     

二硝酰胺钾的合成、晶体结构及性能

以N-脒基脲二硝酰胺盐(GUDN)和氢氧化钾为原料合成了二硝酰胺钾(KDN),用元素分析、傅里叶红外光谱对其结构进行了表征。培养了KDN的单晶,并通过X射线单晶衍射仪测定了其晶体结构。采用差示扫描量热分析仪(DSC)研究了KDN的热分解行为,并测试了其感度。结果表明,KDN晶体属于单斜晶系,P2(1)/n空间群,晶胞参数为:a=0.661 0(11)nm,b=0.927 2(15)nm,c=0.719 4(12)nm,β=97.568(3)°,V=0.437 1(12)nm~3;Z=4;Dc=2.236g/cm~3;F(000)=288。KDN的熔点为128℃,撞击感度大于50cm,摩擦感度为0,静电感度为142.53mJ,感度低于RDX,是一种钝感的二硝酰胺类含能材料。     

The Crystal and Molecular Structure of Kinamycin C p-Bromobenzoate

The molecular structure of kinamycin C has been determined by means of an X-ray study of its p-bromobenzoate derivative, C₃₁H₂₃N₂O₁₁Br. The crystals are monoclinic, P2₁, with four molecules of the derivative and four molecules of benzene in a unit cell of dimensions: a = 18.404 ± 0.005, b = 21.299 ± 0.004, c = 9.049 ± 0.001 Å, and β = 90.07 ± 0.03°. Reflection intensities were measured visually from equi-inclination Weissenberg photographs taken with Cu Ka radiation. The structure was solved by the heavy-atom method, and was refined by the block-diagonal-matrix least-squares method using anisotropic temperature factors for all the atoms. The final R factor is 8.9%. The stereostructures of the two crystallographically independent molecules are almost identical. The skeleton of the molecule is made up of four fused rings: two of these form a 1,4-naphthoquinone system and the rest are a pyrrole and a cyclohexene ring. A cyano group is bonded to the nitrogen atom of the pyrrole ring, which is rather unusual in an antibiotic.     

硼砂的红外和晶体结构研究

通过X-ray单晶衍射和IR对硼砂的结构进行表征,该化合物属于单斜晶系,空间群C2/c,晶胞参数为:a=11.8795(6),b=10.6512(5),c=12.1963(6),α=90,β=106.604(2),γ=90°,V=1478.86(13)3,B4H20Na2O17,Mr=381.38,Z=4,Dc=1.713 g/cm3,μ=0.223 mm–1和F(000)=792。每个钠离子都处于晶体学上的反演对称中心,被来自六个水分子的氧给电子体所包围,形成了一个扭曲的八面体几何构型。晶体结构由水分子和四硼酸根阴离子的氧原子所形成的O-H-O氢键叠加成二维网状。