Hydrothermal Synthesis,Crystal Structure and Thermal Analysis of a Dinuclear Complex Cd_2(3,5-Dinitrobenzoate)_4(pyridine)_4

A dinuclear complex Cd2（dnba）4（pyridine）4 （dnba = 3,5-dinitrobenzoate） has been synthesized by hydrothermal method and characterized by X-ray single-crystal diffraction, elemental analysis, FT-IR spectroscopy, DSC and TG-DTG techniques. The complex with empirical formula C48H32Cd2NI2024 （Mr = 692.83） crystallizes in monoclinic, space group P21/n with a - 12.0344（14）, b = 10.5752（13）, c = 21.578（3） A, β = 104.150（2）°, V = 2662.8（6） A^3, Z = 2, D, = 1.728 g/cm^3,μ（MoKa） = 0.897 mm^-1, F（000） = 1384, S = 1.016 and （△/σ）max = 0.001. R = 0.0638 and wR = 0.0737 for all data; the final R = 0.0337 and wR = 0.0644. In this complex, four carboxylates are bidentate-or chelate-coordinated with the Cd（Ⅱ） centers to give the dinuclear structure. The other coordination positions of Cd（Ⅱ） are occupied by the lone pair electrons from N of four pyridines. Thermal analyses DSC and TG-DTG have been used to determine the thermal decomposition mechanism of the title complex.

Hydrothermal Synthesis,Crystal Structure and Thermal Stability of a Binuclear Copper(Ⅱ) Complex with 3-(Pyridin-2-yl)-1,2,4-triazole

One novel binuclear copper（Ⅱ） complex [Cu 2 （Hpt） 2 （CO 3） 2 （H 2 O） 2 ]·H 2 O with copper carbonate and 3-（pyridin-2-yl）-1,2,4-triazole （Hpt） was hydrothermally synthesized and characterized by IR and X-ray diffraction analysis.The complex crystallizes in triclinic,space group P2 1 /n with a=0.6862（1）,b=0.7805（1）,c=1.1983（2） nm,α=72.03（2）,β=107.72（3）,γ=75.28（2）o,V=0.5884 nm 3,D c=2.105 g/cm 3,Z=1,F（000）=357,GOOF=1.041,the final R=0.01859 and wR=0.04348.The whole molecule is composed of two cooper ions,two Hpt molecules,two carbonate and three water molecules,forming a binuclear structure.The crystal structure shows that the cooper ion is coordinated with three nitrogen atoms from two Hpt molecules,two oxygen atoms from one carbonic acid and one water molecule,forming a distorted square pyramidal geometry.The TG analysis result shows that the title complex is stable under 131.0 ℃.

Hydrothermal Synthesis,Crystal Structure and Thermal Properties of a Novel Samarium Complex with 1D Nano-chain Structure

1 Introduction The design and construction of metal-organic polymers has been a field of rapid growth in materials chemistry because of their intriguing topologies and potential applications as functional materials. In this regard, every effort has been devoted to the deliberate design and control of self-assembly infinite coordination networks via selecting the chemistry structures of ligands, Multidentate carboxylate ligands are widely adopted for construction of coordination frameworks due to their rich coordination modes.

Free-Interface Dual-Compatibility Modal Synthesis Substructure Method in Large-Scale Structures

Free-interface dual-compatibility modal synthesis method(compatibility of both force and displacement on interfaces)is introduced to large-scale civil engineering structure to enhance computation efficiency. The basic equations of the method are first set up, and then the mode cut-off principle and the dividing principle are proposed. MATLAB is used for simulation in different frame structures. The simulation results demonstrate the applicability of this substructure method to civil engineering structures and the correctness of the proposed mode cut-off principle. Studies are also conducted on how to divide the whole structure for better computation efficiency while maintaining better precision. It is observed that the geometry and material properties should be considered, and the synthesis results would be more precise when the inflection points of the mode shapes are taken into consideration. Furthermore, the simulation performed on a large-scale high-rise connected structure further proves the feasibility and efficiency of this modal synthesis method compared with the traditional global method. It is also concluded from the simulation results that the fewer number of DOFs in each substructure will result in better computation efficiency, but too many substructures will be time-consuming due to the tedious synthesis procedures. Moreover, the substructures with free interface will introduce errors and reduce the precision dramatically, which should be avoided.

Influence of Hydrothermal Synthesis Conditions on the Formation of Calcium Silicate Hydrates:from Amorphous to Crystalline Phases

Hydrothermal treatment has been widely applied in the synthesis of well crystalline calcium silicate hydrate（CSH）, such as tobermorite and xonotlite. However, both morphology and crystallinity of CSH are greatly affected by the conditions of hydrothermal treatment including siliceous materials, temperature increase rate and isothermal periods. In this study, the influence of hydrothermal conditions on the growth of nano-crystalline CSH was investigated based on XRD analysis. Results showed that siliceous materials with amorphous nature（i e, nano silica powder） are beneficial to synthesize pure amorphous CSH, while the use of more crystallized siliceous materials（i e, diatomite and quartz powder） leads to producing crystalline CSH. Results also indicate that the formation of tobermorite and xonotlite is greatly affected by the temperature rise rate during hydrothermal treatment.

A New Dinuclear Zinc Polymer Based on 3-Methoxy-2-hydroxybenzaldehyde:Synthesis,Structure,Spectral Characterization and Hirshfeld Surface Analysis

A highly efficient fluorescence material dinuclear zinc polymer [Zn2（mhbd）2（dca）2]n （1, Hmhbd is 3-methoxy-2-hydroxybenzaldehyde, dca is N（CN）2？） has been synthesized under room temperature and structurally characterized by elemental analysis, IR, and single-crystal X-ray diffraction. The structure belongs to the triclinic system, space group P with a = 8.475（1）, b = 9.595（1）, c = 15.001（1） A, α = 86.84（1）, β = 81.10（1）, γ = 68.78（1）°, Mr = 565.15, V = 1123.5（1） ？3, Dc = 1.671 g？cm–3, F（000） = 568, μ = 2.185 mm–1, R = 0.0451, and wR = 0.1297. 1 is a dinuclear zinc complex which further constructs a 1D chain through double μ1,5-dca bridge. Luminescent property and Hirshfeld surface analysis of 1 have been studied. The result indicates that the fluorescence intensity of complex 1 is forty-one times the fluorescence intensity of Hmhbd ligand.

Synthesis, Structure Analysis, and Antitumor Activity of （R）-2,4-Dioxo-5-fluoro-l-[1-（methoxycarbonyl） Ethylaminocarbonylmethyl]-1,2,3,4-tetrahydropyrimidine

A new dipeptide compound, （R）-2,4-dioxo-5-fluoro-1-[1-（methoxycarbonyl） ethylaminocarbonylmethyl]-1,2,3, 4-tetrahydropyrimidine （5-FUAPM）, has been synthesized and identified by means of elemental analysis, IR, ^1H NMR and ^13C NMR spectra. The single crystal of compound 5-FUAPMoDMF was also obtained and characterized by DSC-TGA techniques. The crystal belongs to orthorhombic space group P212121 with the cell parameters： a= 0.4740（7） nm, b= 1.923（3） nm, c= 1.9229 nm, a=β=y=90°, V= 1.753 nm^3, Z=4, Dc= 1.312 g/cm^3, Mr=346.32, F（000）=728 and u=0.111 mm^-1. The final R and wR are 0.1378 and 0.2862, respectively. The result of the biological test showed that the compound 5-FUAPM has certain antitumor activities.

Synthesis and Structural Analysis of LDH-SO4-CO3 Whisker

High-quality LDH-SO4-CO3 whiskers were synthesized via liquid precipitation method using MgSO4·7 H2 O and Al2(SO4)3·18 H2O as precursors and Na2CO3-NaHCO3 buffer solution as precipitant. The influence of buffer solution concentration on the characteristics of the samples was investigated. The asgrown whiskers were characterized by X-ray diffraction, transmission electron microscopy, and BrunauerEmmett-Teller N2 specific surface area measurements. The results show that the buffer solution concentration has significant impact on whiskers with intercalated structure. The LDH-SO4-CO3 whiskers with well-defined geometry, distinct intercalated structure, decent quality, and excellent dispersing capability can be obtained under the following conditions: buffer solution volume ratio of 45%, reaction temperature of 83°C, and reaction time of 182 h. The obtained whiskers are well-crystallized and exhibit homogeneous morphology consisting of fiber bars.

A novel one-dimensional organic-inorganic polymer: synthesis and crystal structure of[{Ca(DMF)_5}_2SiMo_(12)O_(40)]_n

A novel polyoxometalate-based organic-inorganic polymer [{Ca(DMF)5}2SiMo12O40]n has been synthesized and characterized by elemental analysis, IR, UV and X-ray single-crystal structural analysis. The title compound crystallizes in a monocline lattice, P21/n, with a =1.3379(3), b = 1.9796(4), c = 1.4574(3) nm, β= 92.24(3)(, V = 3.8568(13) nm3, Z = 2, R1 = 0.083 and Rw = 0.2065. The result of crystal structure analysis indicates that Ca2+ is surrounded by seven coordination oxygen atoms with pentagonal bipyramidal geometry and bridged with terminal oxygen atom of polyanion in the structure. The compound contains an unprecedented one-dimensional linear chain built by alternate polyanions and cationic units through Mo-Od-Ca-O-Ca links in crystal. The IR spectra and X-ray crystallography analysis exhibit that there is a strong interaction between the polyanion and organic group in solid state. The electronic spectra (λ = 200-500 nm) for the title compound dissolved in the mixed solvent of acetonitrile and water indicate that it is fully dissociated. The TGA/DTA study shows three stages of weight loss and that the thermal stability of polyanion is better than that of H4SiMo12O40@H2O.

Synthesis and structural analysis of ^(13)C-fatty acids

The 13C-labeled fatty acids octanoic-1-13C acid and palmitic-1-13C acid were synthetically prepared from Ba 13CO3. The yield of the former was more than 90% and that of the latter was above 85%. MS, IR, 1H-NMR and 13NMR were performed to analyze the structures of the two 13C-fatty acids, compared with their unlabeled fatty acids.

Syntheses,Crystal Structures,and Antimicrobial Activities of 3-Bromo-N'-(2- chloro-5-nitrobenzylidene)benzohydrazide and 3-Bromo-N'-(4-nitrobenzylidene)benzohydrazide

Two new hydrazone compounds, 3-bromo-N＇-（2-chloro-5-nitrobenzylidene）-ben- zohydrazide 1 and 3-bromo-N＇-（4-nitrobenzylidene）benzohydrazide 2, have been synthesized and characterized by elemental analysis, IR spectra, 1H NMR, and single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a=7.7924（10）, b=24.490（3）, c=7.8989（9） , β=94.987（6）°, V=1501.7（3） 3, Z=4, R=0.0345 and wR=0.0739. Compound 2 crystallizes in monoclinic, space group P21/c with a=7.4099（11）, b=24.868（4）, c=8.3255（12） , β=112.796（8）°, V=1414.3（4） 3, Z=4, R=0.0744 and wR=0.1912. Both compounds display E configurations with respect to the C=N double bonds. In the crystal structure of 1, molecules are linked through N-H…N and N-H…O hydrogen bonds, forming chains running along the c axis. In the crystal structure of 2, molecules are linked through N-H…O hydrogen bonds, forming chains running along the c axis. The preliminary antimicrobial activities were studied.

A high-throughput strategy for rapid synthesis and characterization of Ni-based superalloys

This study developed a new high-throughput strategy,designated as hot-isostatic-pres sing-based microsynthesis approach(HIP-MSA),to optimize high-performance nickel-based superalloys in a rapid,efficient,and cost-effective manner.A specific honeycomb-array structure containing 106 discrete cells was designed and optimized using finite element analysis(FEA)and then applied to create a combinatorial library consisting of 106 Ni-based superalloys with various Co,Nb and Ta concentrations.By integration with high-throughput characterization tools,extensive composition and phase structure data were collected quickly and efficiently.In the superalloys with higher amounts of Nb and Ta,the detrimentalηphase displaying needle-like morphology was observed,and its content(wt%)increased drastically with Ta and Nb contents increasing.However,the increase of Co addition in those alloys was confirmed to be surprisingly beneficial by significantly suppressing the formation ofηphase that was induced by high Nb and Ta contents.The zero-phasefraction(ZPF)line ofηphase was established,which is critical to design superalloy chemistry for superior micros tructural stability at high-temperature service conditions.

Experimental and simulation studies on similitude design method for shock responses of beam-plate coupled structure

The similitude theory helps to understand the physical behaviors of large structures through scaled models. Several papers have studied the similitude of shock issues. However, the dynamic similitude for shock responses of coupled structures is rarely incorporated in open studies. In this paper, scaling laws are derived for the shock responses and spectra of coupled structures. In the presented scaling laws, the geometric distortion and energy loss are considered. The ability of the proposed scaling laws is demonstrated in the simulation and experimental cases. In both cases, the similitude prediction for the prototype's time-domain waveform and spectrum is conducted with the scaled model and scaling laws. The simulation and experimental cases indicate that the predicted shock responses and spectra agree well with those of the prototype, which verifies the proposed scaling laws for predicting shock responses.

Structure Elucidation of Hydroxypropyl Cellulose Homogenously Prepared from NaOH/Urea Aqueous Solution

Hydroxypropyl celluloses(HPC) were homogenously synthesized by the reaction of cellulose with propylene oxide in NaOH/urea aqueous solution.Water-soluble HPC with molar degree of substitution(MSNMR) in the range of 0.52~0.78 was prepared from microcrystalline cellulose,cotton linters,and spruce sulfite pulp.The structure of the HPC samples was characterized by means of FT-IR,NMR,gas chromatography(GC),and size exclusion chromatography(SEC) analyses.Three types of cellulose samples with different molecular weights were found to dissolve well in the NaOH/urea solvent with no obvious differences in reactivity and regioselectivity.The relative reactivity of hydroxyl groups in the glycosyl unit was in the following order:O-6>O-2>O-3.In addition,the results of the study indicated that the tandem reaction during hydroxypropylation could be ignored.

Wittig反应实验的绿色化改进

传统的有机化学实验教学中,大多侧重实验技能的训练,设置实验内容时对实验安全性、经典性和可重复性等因素考虑较多,而对反应的绿色化、新方法和新技能等重视程度不够。为此,经典的有机反应也需要不断改进,本文将需要在大量有机溶剂中进行的传统Wittig反应改进为无溶剂的固相研磨反应,使得合成方法更加简单、绿色、安全和高效。设计合成了3个不同推拉型(D-π-A)二苯乙烯结构分子,优化了反应条件,测定了它们的光谱性质,并对其进行比较,讨论其构性关系,不仅引入绿色化学理念,而且对知识进行扩展,增加了实验的新颖性、探索性和趣味性,提升了学生创新能力。

一种基于图论理论的大尺度连续变形机构构型综合分析方法

针对航空航天领域大尺度连续变形机构构型问题,提出了一种基于图论理论的大尺度连续变形机构构型综合分析方法。首先,分析了大尺度连续变形机构的组成与基本功能,获得了满足机构拓扑结构、约束条件的要求,对变形机构运动链进行了分析,得到了符合条件的运动链,并对其进行了数学描述;其次,选择并分析了运动链的拓扑对称性,利用特征数组的方法得到了判别矩阵,对运动链进行了同构判别,从而得到了可行的多种运动链形式;再次,建立了各运动链的拓扑图,通过筛选得到了最终的拓扑图,去掉该拓扑图的各个构件,得到了拓扑变换子图和相对应的邻接矩阵,对拓扑图进行了同构判别,再通过改变机架与移动副的位置得到了满足要求的12种构型,画出了其相应的机构拓扑图和机构简图;最后,考虑了大尺度连续变形机构的整体稳定性,避免了尺寸过大等因素,对大尺度变形机构进行了构型优选,得到了符合要求的多种新构型。研究结果表明:该方法能够将大尺度连续变形机构抽象为图形式,获得了22种构型,可根据机构变形要求的不同,改变优选依据,从而得到符合不同要求的构型。

两个含5-溴水杨酸钠(Ⅰ)/镉(Ⅱ)配合物的合成、晶体结构、Hirshfeld表面分析与抑菌活性

由5-溴水杨酸(H_(2)BBA)合成了钠/镉配合物[Na(HBBA)]_(n) (1)和[Cd(HBBA)_(2)(4,4′-Bipy)]_(n) (2)(H_(2)BBA=5-溴水杨酸,4,4′-Bipy=4,4′-联吡啶)。通过元素分析、红外光谱、热重、粉末X射线衍射和单晶X射线衍射表征了其结构。配合物1的不对称单元中有1个钠离子和1个HBBA-。钠离子是六配位的三棱柱构型,HBBA-配体的3个氧原子分别与2个钠离子配位,连接相邻的钠离子形成了3条一维链结构,HBBA-配体连接相邻的3条一维链形成了二维网络结构。分子间氢键连接相邻的二维网络结构形成了三维氢键网络结构。配合物2中有1个镉离子、2个HBBA-和1个4,4′-Bipy。镉离子是六配位的扭曲八面体构型,4,4′-Bipy配体连接相邻的2个镉离子形成了一维链结构。分子间氢键连接相邻的一维链结构形成了三维氢键网络结构。通过Hirshfeld表面和指纹图分析了配合物晶体中的弱分子间作用力。详细研究了配合物1和2的热稳定性和抑菌活性。

金刚石/纳米氧化铝陶瓷复合材料高温高压合成物相结构分析

以正硅酸乙酯(TEOS)为反应前驱体,采用溶胶-凝胶法在金刚石微粉(粒度0.1~4μm)表面包覆一层非晶纳米氧化硅膜层,同时在覆膜层中加入纳米Si粉和纳米Al_(2)O_(3)粉,制备出金刚石/纳米SiO_(2)/纳米Al_(2)O_(3)复合包覆体。采用高温高压(HTHP)技术,将复合包覆材料置于六面顶压机中,以压力5 GPa、温度1100℃~1700℃、保温20 min的条件制备了金刚石-氧化铝陶瓷烧结体。在高温高压合成过程中,纳米SiO_(2)从非晶态转变为晶态,原料纳米Al_(2)O_(3)中的γ-相、θ-相转变为稳定的α-相,同时,SiO_(2)和Al_(2)O_(3)之间形成了Al_(2)SiO_(5)(莫来石)相,由此,通过高温高压下反应原料的结构转变与复合,可以获得致密度良好的金刚石-氧化铝复合材料。

结构参数对不锈钢织物透光与电磁屏蔽的影响

为实现不锈钢织物高透明与强电磁屏蔽性能相兼容的目标,文章采用数值计算与理论分析相结合的方法,在分析不锈钢织物主要结构参数(线径与线距)对其透光与电磁屏蔽性能影响的基础上,引入TOPSIS评价方法,探讨了线径与线距对不锈钢织物光学与电磁学综合性能的影响。结果表明,由于电磁衍射的存在,结构参数对透光与电磁屏蔽性能的影响呈现非线性规律。其中,不锈钢织物的线距变化对总体性能的影响最为密切。当线径在0.02~0.05 mm且线距在0.4~1.0 mm时,不锈钢织物在90%高透光率的前提下,可达到至少30 dB的屏蔽效能,为高透光电磁屏蔽材料的结构设计提供了理论指导。

2-萘甲酸/1,10-菲啰啉共同构筑Mn(II)配合物的合成及固态发光

在溶剂热条件下,以2-萘甲酸(HL)与1,10-菲啰啉(phen)为配体、碳酸锰为金属源合成了一例双核锰配合物[Mn_(2)(L)_(4)(phen)_(2)(H_(2)O)_(2)](1)。通过单晶X射线衍射、元素分析、傅里叶变换红外光谱、粉末X射线衍射和热重分析等对配合物1进行结构表征。单晶衍射分析表明配合物1属于三斜晶系,P1空间群,晶胞参数为a=0.76989(5)nm,b=1.17586(5)nm,c=1.66830(9)nm,α=107.074(5)°,β=96.167(5)°,γ=106.901(5)°。不对称单元由一个锰离子、两个2-萘甲酸根、一个1,10-菲啰啉和一个水分子组成,Mn(II)呈扭曲的八面体构型。两个不对称单元之间通过羧基氧原子桥接形成双核分子,双核结构之间通过π…π堆积作用形成2D超分子结构。荧光光谱分析结果表明:配合物1具有良好的荧光性能,最大发射波长为416 nm(λ_(ex)=302 nm)。热重分析表明配合物1能够稳定到117℃,之后开始失水(失水量为3.18%),脱水之后的结构能稳定到223℃,之后有机骨架开始坍塌。Hirshfeld表面分析研究了分子间的相互作用。