吡啶-2-甲醛酰腙镉配合物的合成、晶体结构与荧光性质

合成了3个不同结构的吡啶-2-甲醛缩对氯苯氧乙酰腙(HL)与镉的配合物.通过X射线单晶衍射、红外光谱、紫外光谱、荧光光谱以及热重等分析,对其进行晶体结构和性质的研究.单晶衍射结构解析表明:配合物1属单斜晶系,C2/c空间群,是一个通过氯离子桥联的二聚体,分子式为[Cd(HL)Cl2]2;配合物2属单斜晶系,P21/c空...     

The synthesis, vibrational spectroscopy, and crystal and molecular structure of [H3NCH2CH2NH3][PdBr6]

The complex [H₃NCH₂CH₂NH₃][PdBr₆] has been isolated as well-formed brown crystals. The Raman (single crystal) and FTIR (wax disc) spectra of the complex have been recorded but the band assignments are complicated by extensive factor group splitting and resonance effects. The crystal belongs to space group Pnnm, with Z = 2, each ion occupying sites of 2/m (C_2h) symmetry. The [PdBr₆]²⁻ ion is very close to octahedral, the two unique PdBr distances, 2.466(3) and 2.470(3) Å, being equal within experimental error and the BrPdBr angles being 90 ± 0.8°. The diammonium cation has an extended, planar, trans structure.     

三环己基锡吡咯啶二硫代氨基甲酸酯和三环己基锡邻苯二甲酰亚胺配合物的合成、结构和量子化学研究

三环己基氢氧化锡分别与吡咯啶二硫代氨基甲酸钠和邻苯二甲酰亚胺反应,合成了三环己基锡吡咯啶二硫代氨基甲酸酯(1)和三环己基锡邻苯二甲酰亚胺配合物(2)。化合物经IR、1H NMR、元素分析表征,用X射线衍射法测定了晶体结构,化合物1属正交晶系,空间群P212121,晶体学参数:a=1.228 06(3)nm,b=1.238 20(2)nm,c=1.662 54(3)nm,Z=4,V=2.528 03(9)nm3,Dc=1.351 g.cm-3,μ(Mo Kα)=1.184 mm-1,F(000)=1 072,R1=0.048 7,wR2=0.121 0;化合物2属正交晶系,空间群P212121,晶体学参数:a=1.244 70(19)nm,b=1.269 45(19)nm,c=1.587 7(2)nm,Z=4,V=2.508 7(6)nm3,Dc=1.362 g.cm-3,μ(Mo Kα)=1.039 mm-1,F(000)=1 064,R1=0.049 9,wR2=0.128 4,中心锡原子均为畸变四面体构型。对化合物进行了量子化学从头计算,探讨了化合物的稳定性、分子轨道能量以及前沿分子轨道的组成特征。     

1－苯基－3－甲基－4－（6－氢－4－氨基－5－硫杂－2，3－吡嗪）－吡唑啉酮光致变色超分子化合物的合成、结构与性能

通过1－苯基－3－甲基－4－氯乙酰基－吡唑啉酮－5（PMCP）和氨基硫脲（ TSC）缩合，形成了一种含NNS六元杂环的光致变色化合物（PMCP－TSC）。利用元 素分析，MS，”1H NMR，IR和UV光谱进行了表征。通过紫外可见光谱对它的光致 变色性质进行了研究，测出了光致变色反应的动力学常数。并用X线单晶衍射仪测 定了PMCP－TSC变色后的晶体结构，该晶体属单斜晶系，具有P2_1/c空间群，a = 0.105 10(2) nm, b = 0.150 61(3) nm, c = 0.993 70(10) nm, β = 107.890 (10)°, V = 1.496 9(4) nm~3, Z - 4, D_c = 1.417 Mg/m~3, μ = 0.232 mm~(- 1), F(000) = 672, R = 0.033 4, wR = 0.089 6。结构分析表明：其光致变色现 象是由于它在溶剂与光的共同作用下发生了从醇式到酮式的异构化。同时该化合物 经分子间氢键形成二聚体，又通过甲醇与本体分子之间的氢键使化合物形成具有三 维网络结构的超分子化合物。     

Polarized IR and Raman spectra and ab initio calculations for bis(guanidine) zirconium bis(nitrilotriacetate) hydrate single crystal [C(NH2)3]2[Zr[N(CH2COO)3]2](H2O)--the new laser Raman converter

Fourier transform polarized IR and Raman spectra of bis(guanidine) zirconium bis(nitrilotriacetate) hydrate single crystal [C(NH(2))(3)](2)[Zr[N(CH(2)COO)(3)](2)](H(2)O) have been measured in the regions 30-4000 and 80-4000 cm(-1) and correlated with X-ray structural data. The factor group analysis has been applied in the discussion of the dichroic dependence of the vibrational modes. The assignment of the internal vibrations for the [Zr(nitrilotriacetate)2]2- complex ion has been based on the ab initio quantum chemical calculations. The usefulness of the studied crystal as Raman laser converter was analyzed basing on the comparison of the spontaneous and stimulated Raman spectra.     

Crystal growth, structural and spectroscopic analysis of hypoxanthinium chloride monohydrate

Protonated form of hypoxanthinium chloride monohydrate single crystal has been grown from dilute hydrochloric acid. Single crystal X-ray analysis was carried out and the titled crystal belong to the monoclinic P2(1)/c space group. Hypoxanthine is protonated at N(1) with the hypoxanthine cations, linked to chlorine anion via weak bifurcated N-H...Cl hydrogen bonds and interconnected by hydrogen bonding contacts of the type N-H...O. Infrared, Raman and UV spectroscopic tools were applied to characterize hypoxanthinium chloride monohydrate. By applying group theoretical methods the internal and external modes of vibrations of the title crystal have been identified and discussed.     

含能配合物[Zn(DAT)_6](ClO_4)_2 (DAT=1,5-二氨基四唑)的合成、晶体结构及性质

采用直接法合成了新型高氮含能配合物[Zn(DAT)6](ClO4)2(DAT=1,5-二氨基四唑),并用元素分析、傅立叶变换红外光谱对其结构进行了表征.利用缓慢蒸发溶剂法培养出其单晶,采用X射线单晶衍射仪测定其晶体结构,结果表明该晶体属于三方晶系,P3空间群,a=b=1.18398(9)nm,c=0.65700(10)nm,γ=120°,V=0.79760(15)nm3,Z=1.在目标配合物的最小不对称单元中有1个Zn2+,6个DAT分子和2个ClO-4.来自6个DAT分子的6个N原子分别与中心Zn2+配位,形成一个六配位、非中心对称的畸变八面体结构.用差示扫描量热分析、热重-微分热重分析结合红外光谱研究了标题化合物的热分解机理以及分解反应动力学参数.测定了标题配合物的感度性能,结果表明标题配合物具有一定的摩擦感度.     

11-钨硼酸钾的结构和振动光谱研究

标题化合物K₈H(BW₁₁O₃₉)·13H₂O属立方晶系,空间群P43m,a=10.710(1)Å,V=1228.58ų,Z=1;D_O=4.39g·cm^-3,D_c=4.42g·cm^-3。(BW₁₁O₃₉^9-离子属于不饱和α-Keggin型结构,B原子位于O₂四面体的中心。测定并研究了化合物的IR和Raman光谱性质。     

Crystal structure, differential scanning calorimetry and vibrational low temperature investigation of C(NH2)3 x HSeO4

The first X-ray and vibrational spectroscopic analysis of a new molecular complex between guanidinium and selenic acid is reported. The crystal of guanidinium hydrogenselenate at room temperature belongs to P2(1)/n space group of the monoclinic system with Z=4, a=8.330A, b=5.109A, c=14.855A and beta=92.65 degrees . Room temperature powder infrared and Raman spectra for the titled complex (1:1) were measured. The observed IR and Raman spectra are in accordance with this crystallographic structure. The differential scanning calorimetric (DSC) experiment on powder samples indicates on continuous phase transition at ca. 160K. To explain in detail the behavior of the crystal during the phase transition the infrared and Raman powder spectra in low temperature range (10-300K) were measured. The temperature dependencies of bands position and intensities for obtained spectra are analysed.     

Synthesis and characterisation of the compound CoSbS

In the search for new intermetallic materials with high thermoelectric performances, the Co–Sb–S ternary system has been explored and polycrystalline CoSbS samples have been prepared by a vapour phase technique starting from the pure elements. The crystal cell of CoSbS belongs to the Pbca space group and shows an orthorhombic structural arrangement with the following lattice parameters: a = 5.8341(2) Å; b = 5.9477(2) Å, and c = 11.6540(4) Å. The structure belongs to the pyrite–marcasite family, as Co forms tilted corner- and edge-sharing octahedra with three Sb and three S atoms. Scanning electronic microscopy (SEM), electron-probe microanalysis (EPMA) and X-ray powder diffraction were used to investigate the microstructure and to carry out the structural analysis; the crystal structure was refined by the Rietveld method using the DBWS-9807 program. The thermal stability of CoSbS was investigated referring to the ternary Co–S–Sb phase diagram and by differential thermal analysis (DTA) measurements. Thermoelectric power measurements at room temperature were also performed by a home-made instrument.     

有机杂化含Te2^2-／Se3^2-过渡金属化合物的溶剂热合成及晶体结构

本文通过溶剂热法合成了2种新的有机杂化锌碲化物[Zn(dien)2](Te2)(1)和镍硒化物[Ni(dien)2](Se3)(2)(dien=二乙烯三胺),单晶X射线衍射分析结果表明,化合物1属于正交晶系,Cmca空间群,晶胞参数:a=9.212(2),b=10.854(3),c=15.723(4),Z=4。化合物2属于正交晶系,Pna21空间群,晶胞参数:a=18.047(4),b=9.8236(19),c=9.0079(19),Z=4。在两种化合物中,1的阳离子中Zn2 与2个dien螯合形成稍变形的八面体几何构型,阴离子为哑铃型的Te22-。2的阳离子中Ni2 离子与2个dien螯合形成稍变形的八面体几何构型,阴离子为‘V’字型的Se32-。     

Polarised IR and Raman spectra of non-centrosymmetric Na3Li(SeO4)2.6H2O crystal--a new Raman laser material

Polarised IR and Raman spectra of Na₃Li(SeO₄)₂·6H₂O single crystal have been recorded. Discussion of the results has been based on the factor group approach for the trigonal R3c (C_3v⁶) space group with Z = 2. The obtained results for the spontaneous Raman scattering have been used in the discussion of the stimulated Raman spectra of the material studied—a new Raman laser crystal.     

氨基乙氧基一价铼羰基配合物的合成、晶体结构与表征

详细研究了[Re2(CO)10]在氧化三甲胺(TMNO.2H2O)的作用下与配体H2NCH2CH2OH的反应,反应产物用丙酮-己烷混合溶剂重结晶,得到Re(Ⅰ)双核配合物[Re2(-μOCH2CH2NCMe2)2(CO)6].采用元素分析、红外光谱和1H NMR对配合物的结构进行了表征.用SMART CCD X射线衍射仪测定了晶体结构,结果表明该晶体属三斜晶系,Pī空间群.在此晶体结构中,2个铼离子被2个氧桥联形成二聚单元,每个Re(Ⅰ)是六配位的变形八面体构型.     

Preliminary crystallographic analysis of deshexapeptide (B25-B30) insulin

Satisfactory single crystals of deshexapeptide (B25-B30) insulin for X-ray crystal structure analysis have been grown in citrate buffer by the method of hanging-drop gas phase diffusion. The crystal belongs to the monoclinic system with space group C2. The unit cell constants are a = 42.6 A, b = 37.9 A, c = 27.2 A, beta = 125.4 degrees and there is only one molecule of deshexapeptide insulin in an asymmetric unit.     

含钒氧链阴离子的苯基三联吡啶钴配合物的合成、晶体结构及性质研究

利用水热反应合成一种新型含钒氧链阴离子的苯基三联吡啶钴配合物{[Co(PhTPY)2]V3O9.3H2O}n(PhTPY=4′-ph-2,2′∶6′,2″-terpyridine)。用元素分析、红外光谱和X-射线单晶衍射对其结构进行了表征,该配合物晶体属单斜晶系,C2/c空间群。同时测定了配合物的热稳定性、荧光性质和磁性质。     

Computational,structural, spectral,optical and Hirshfeld surface analysis of (E)-2-(3,4,5-trimethoxybenzylidene) hydrazinecarbothioamide (ETMBHC): Third order NLO single crystal

By using a slow evaporation solution growth technique, single crystals of (E)-2-(3,4,5-trimethoxybenzylidene) hydrazine carbothioamide (ETMBHC) have been produced. The crystalline compound has the following properties: a = 7.471 (3), b = 9.705 (4), c = 11.168 (4), = 73.200(11)°, = 70.633 (10)°, = 70.334 (10)°; it belongs to the triclinic system with space group P. The ETMBHC chemical is a member of the P-1 triclinic system. Fourier transformations and Fourier transform infrared (FT-IR) The functional groups have been identified by Raman spectrum research. To understand how charge transfer occurs inside molecules and to establish that the title crystal is appropriate for NLO applications, the HOMO and LUMO energies for the grown crystal were computed. TGA-DTG analysis was used to study the melting point and thermal stability. Z-scan analyses were used to determine the grown crystal's nonlinear absorption coefficient and third-order nonlinear refractive index.     

STUDY OF THE CRYSTAL STRUCTURE OF BIS(2,4-DIMETHYL-PENTADIENYL) MONOCARBONYL-VANADIUM USING A LOW TEMPERATURE X-RAY DIFFRACTION TECHNIQUE

<正> The single crystal X-ray diffraction data of (2,4-(CH3)2C5H5]2VCO have been collected under low temperature (-60℃) and the crystal structure has been solved by heavy atom method. It belongs to orthorhombic system, space group P212121, a =9.921(6), b =9.899(6), c=14.491(8) A, Z=4. Several cycles of block matrix least-squares refinement gave the final R=0.087.     

Investigations on the physicochemical properties of the nonlinear optical crystal for blue green laser generation

Bisglycinehydrogenchloride (BGHC) an intriguing material for frequency conversion has been grown by slow evaporation solution growth technique at room temperature. Their structural, optical and physicochemical properties were characterized by X-ray powder diffraction, FTIR, Raman and UV-vis spectra. The title crystal has found to crystallize into noncentrosymmetric orthorhombic P2(1)2(1)2(1) space group. The material has a wide transparency in the entire visible region. It is found that the cutoff wavelength lies in the UV region. The mechanical response of the crystal has been studied using Vickers microhardness technique. The Kurtz powder second harmonic generation test shows that the compound is a prospective crystalline material for second order nonlinear optical application.     

Raman and Brillouin scattering spectroscopy studies of atomic layer-deposited ZrO(2) and HfO(2) thin films

Atomic layer-deposited ZrO(2) (zirconia) and HfO(2) (hafnia) films with various thicknesses, ranging from 112 to 660 nm, have been studied by Raman scattering spectroscopy. Spectral analysis of the excellent quality Raman data obtained by using freestanding edges of the films has unambiguously demonstrated that a metastable tetragonal t-ZrO(2) is coexisting with the stable monoclinic phase in zirconia films. Even though the Raman spectrum signal-to-noise ratio was high, only the monoclinic phase was positively identified from the observed spectral patterns of hafnia films. X-ray diffraction patterns are used to define the structure of metastable phases. Complementary Brillouin light scattering measurements of the freestanding edges are also employed in constraining elastic properties of the 405 nm HfO(2) thin film.     

固氮酶活性中心元件化合物及其组合体的结构化学——[(FeCl_3)_2O]~2及其衍生物的合成与晶体结构

无水FeCl_3和格氏试剂在THF中反应,反应产物在DMF中重结晶,得到(Mg·6DMF)[(FeCl_3)_2O]的晶体,在NMF中重结晶,得到FeCl_3·3NMF。本文讨论了氧桥生成的条件。(Mg·6DMF)((FeCl_3)_2O]和(Et_4N)_2[MoFeS_4Cl_ 2)在DMSO中反应得到一非化学计量的笼状化合物,其分子式为[MoFeS_4Cl_2]。[Fe_2S_2Cl_4]_(1-a)(Fe·6DMSO)_b(Mg·6DMSO)_(1-b。) 分别测定了(Mg·6DMF)((FeCl_3)_2O]及其衍生物的晶体结构。首次发现了单氧桥二铁化合物的交错型四配位直线氧桥结构,它存在于(Mg·6DMF)~(2+)的笼状母体中。 (Fe·6DMSO)~(2+)统计分布于(Mg·6DMSO)~(2+)的笼状骨架上,而阴离子[MoFeS_4Cl_2]~(2-)和[Fe_2S_2Cl_4]~(2_)统计分布在这个笼状母体中。 在FeCl_3·3NMF中,可以看到Fe—Cl键的对位效应。