[K2(TNR)(H2O)]n的制备、分子结构和热分解机理

2,4,6-三硝基间苯二酚(斯蒂芬酸)及其盐类,如斯蒂芬酸铅、斯蒂芬酸钡等是常用的含能材料[1],但斯蒂芬酸铅盐及钡盐在爆炸后产生重金属污染,对使用人员的健康及环境都产生危害.     

{[Cd(NTO)_2(CHZ)]·2H_2O}_n的合成、分子结构和热分解机理

通过3-硝基-1,2,4-三唑-5-酮(NTO)镉与碳酰肼(NH2NHCONHNH2,CHZ)反应制备出了新型配合物狖犤Cd(NTO)2(CHZ)犦·2H2O狚n,研究了其分子结构和热分解机理。该配合物的晶体属正交晶系,Pbca空间群,晶体学参数:a=0.8623(1)nm,b=1.8259(4)nm,c=1.9997(3)nm,Z=8。晶体结构经全矩阵最小二乘法修正,最终偏离因子R1=0.0517,wR2=0.0655。中心Cd离子为六配位、畸变的八面体构型,NTO-作为二齿配体同时与2个镉离子形成配位键,三齿配体CHZ的2个配位原子与一个镉离子形成五元螯合环、另1个配位原子与第二个镉离子形成配位键,依次无限延伸,形成三维网状结构的配合物。     

M(TNR)·H2O的热分解机理

本文用TG—DTA、DSC、IR和X光衍射分析考察了三硝基间苯二酚金属盐M(TNR)·H_2O(M=Pb、1/4Pb3/4Ba、Ba)的热行为及其热分解机理。结果表明,M(TNR)·H_2O晶体的热分解过程均分三个阶段进行。即脱水阶段;脱硝逸出NO_2伴随苯环碎裂成凝聚相产物的阶段和凝聚相产物分别生成PbO和少量碳;BaCO_3、PbO和少量碳;BaCO_3的阶段。     

[Pb2(TNR)2(CHZ)2(H2O)2]4H2O的结构及热分解机理

The coordination compound of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O was prepared by using the aqueous solution of carbohydrazide, lead nitrate and sodium styphnate. The molecular structure of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O(C 7H 13 N 7O 12 Pb, Mr=594.43) was determined by using a single crystal diffraction analysis .The thermal decomposition mechanism of the title compound was studied by TGDTG, DSC and IR techniques. The crystal belongs to monoclinic with space group P2 1/n.The unit cell parameters are as follows: a=0.64700(10)nm, b=1.6074(3)nm, c=1.4883(3)nm,β=97.42(2)°,V=1.5349(5)nm3, Z=2, DC=2.572g•cm -3 ,μ(Mo, Kα)=11.080cm -1 , F(000)=1128. R=0.0422, Rw=0.0735. The binuclear lead coordination compound is bridged by two carbohydrazide molecules. The molecule has a symmetrical center. TNR 2- ,CHZ and H 2O coordinate with the central ions simultaneously.     

[Pb2(TNR)2(CHZ)2(H2O)2]·4H2O的结构及热分解机理

用碳酰肼 (CHZ ,NH2 NHCONHNH2 )、硝酸铅和三硝基间苯二酚 (TNR ,斯蒂酚酸 )的水溶液制备 [Pb2 (TNR) 2 (CHZ) 2 (H2 O) 2 ]·4H2 O .采用单晶分析的方法测定它的分子结构 ,并用TG DTG、DSC和　IR相结合的技术研究它的热分解机理 .所得晶体属单斜晶系 ,P2 1/n空间群 .晶体学参数为 :a=0 .6470 0 ( 10 )nm ,b =1.60 74 ( 3)nm ,c=1.4 883( 3)nm ,β =97.4 2 ( 2 )° ,V =1.534 9( 5)n ,Z =2 ,DC=2 .572 g·cm- 3,μ(Mo ,Kα) =11.0 80cm- 1,F( 0 0 0 ) =112 8.最终偏离因子R =0 .0 4 2 2 ,Rw=0 .0 735.该配合物分子呈中心对称 ,两个羰基O原子形成两个氧桥 ,TNR2 - ,CHZ和H2 O同时参与了与中心离子的配位     

[K(HTNR)(H_2O)]_n的制备、晶体结构和热分解机理

通过2，4，6－三硝基间苯二酚（斯蒂芬酸，TNR）与氢氧化钾在乙醇溶液中反 应，首次合成出配位聚合物[K(HINR)-(H_2O)]_n，并测定了其晶体结构。该晶体属 单斜晶系, P2_1/c空间群；晶胞参数： a = 0.7888(1)nm, b = 1.38002(2) nm, c = 0.9520(1) nm, β=8.91(1)°；V = 1.0238(2) nm~3; D_c = 1.954 g/cm~3; Z = 4; F(000) = 608; μ(MoKα) = 0.575 mm~(-1)。用DSC，TG－DTG及FT－IR 等分析方法研究了该配位聚合物的热分解机理。在线性升温条件下，该配合物的热 分解包含两个重叠的弱吸热过程和两个强放热分解过程。分解残渣的红外分析表明 ，在271.9 ℃时，分解残渣中有KNCO与羧酸钾，357.1 ℃时，残渣中只有KNC存在 。     

[Co(mcz)3](NO3)2·H2O的制备、分子结构和热分解机理

由硝酸钴水溶液和肼基甲酸甲酯(NH2NHCOOCH3, mcz)的水溶液反应, 首次制备出了配合物[Co(mcz)3](NO3)2H2O, Mr = 471.23, 测定了其晶体结构。晶体属单斜晶系, P21/n空间群。晶体学参数为: a = 13.648(3), b = 8.234(1), c = 16.144(4) ? b=91.96(2), V=1813.1(5) ?, Z=4, Dc = 1.726 g/cm3, m(MoKa ) = 1.030 mm1, F(000)=972, R=0.0359, wR = 0.0935。在该配合物中, 肼基甲酸甲酯作为双齿配体, 由羰基氧原子和1位氮原子与钴原子配位, 形成五员平面螯合环, 配合物分子中共有3个这样的螯合环, 中心离子为六配位八面体构型。配合物的外界为2个硝酸根离子, 并含有1个结晶水分子, 通过库仑力与内界结合在一起, 相邻分子间以氢键作用连接。采用TG、DTG, DSC和IR技术研究了标题化合物热分解机理。在程序升温条件下, 该配合物有2个吸热峰和3个放热峰, 由TG-DTG分析和IR分析结果表明, 300 ℃时的最终分解产物为CoO。     

斯蒂芬酸氢铷的制备，晶体结构和热分解机理

A new compound,[RbHTNR]_∞[HTNR:C_6H(NO_2)_3(OH)O],was synthesized by the reaction of rubidium ni-trate and styphnic acid.The molecular structure was characterized using X-ray diffraction analysis,elementalanalysis and FTIR spectroscopy.The crystalline is monoclinic with space group P2_1/n and the empirical formulaC_6H_2N_3O_8Rb.The unit cell parameters are:a=0.4525 nm,b=1.0777 nm,c=1.9834 nm,β=90.47(2)°,V=0.96725 nm~3,Z=4,D_c=2.263 g/cm~3,Mr=329.58,F(000)=640,μ(Mo Kα)=5.165 mm~(-1).The thermal decompo-sition mechanism of the complex was studied by differential scanning calorimetry(DSC),thermogravimetry-derivative thermogravimetry(TG-DTG)and FTIR techniques.At the linear rate of 10 ℃/min,the thermaldecomposition of the complex showed three mass reducing processes between 60 and 500 ℃,and finally evolvedRbCN and some gaseous products.     

[Sr(CHZ)(TNR)(H2O)(OH)]2·2H2O的晶体结构和热分解机理

The coordination compound of [Sr(CHZ)(TNR)(H₂O)(OH)]₂·2H₂O (TNR: 2,4,6-trinitroesorcinol, CHZ: carbohydrazide) was prepared by reacting CHZ solution and strontium styphnate solution (obtained through the reaction of strontium carbonate and styphnic acid). The molecular structure was characterized by using X-ray diffraction analysis, element analysis and FTIR analysis. The crystal belongs to triclinic with space group P1. The unit cell parameters were as follows: a=0.725 2(2) nm, b=1.021 2(2) nm, c=1.144 0(2) nm, α=69.50(3)°, β=78.82(3)°, γ=84.64(3)° and Z=2. The thermal decomposition of the compound is studied using differential scanning calorimetry (DSC) and thermogravimetry thermogravimetry-derivative (TG-DTG) techniques. CCDC: 269310.     

{[Cd(NTO)2(CHZ)]·2H2O}n的合成、分子结构和热分解机理

通过3-硝基-1,2,4-三唑-5-酮(NTO)镉与碳酰肼(NH₂NHCONHNH₂,CHZ)反应制备出了新型配合物{[Cd(NTO)₂(CHZ)]·2H₂O}_n,研究了其分子结构和热分解机理。该配合物的晶体属正交晶系,Pbca空间群,晶体学参数:a=0.8623(1)nm,b=1.8259(4)nm,c=1.9997(3)nm     

Crystal Structure and Thermal Decomposition Mechanism of [K（DNP）（H2O）0.5]n

Introduction As developing high-energy, low toxicity and envi-ronment friendly primary explosive has been becoming a new and important investigation field, much attention has been paid to nitrogen-rich potassium coordination compounds for the sake of their low toxicity and little pollutions.1-11 In order to make good use of potassium compounds, the reaction of 2,4-dinitrophenol (DNP) and potassium hydroxide was designed, and the title compound potassium 2,4-dinitrophenate (KDNP) was obtained…     

Crystal Structure,Thermal Behavior and Luminescence of a One-dimensional Coordination Polymer [Zn（4-CPOA）（Phen）（H2O）]n

A novel coordination polymer of [Zn（4-CPOA）（Phen）（H2O）]n （C21H16N2O6Zn,1,4-CPOA = 4-carboxylato-phenoxyacetate dianion and Phen = 1,10-phenanthroline） has been synthesized and characterized by elemental analysis,IR,TG,PL and single-crystal X-ray diffraction. The crystal crystallizes in the triclinic system,space group of P1 with a = 9.622（3）,b = 9.631（3）,c = 11.526（4）A,α = 67.719（5）,β = 71.203（5）,γ = 83.552（6）o,V = 935.5（5） A^3,Z = 2,Dc = 1.625 g/cm^3,μ = 1.357 mm^-1 and F（000） = 468. The Zn（II） ion is surrounded by three carboxylate O atoms from two different 4-CPOA groups,two N atoms from the Phen ligand and one water molecule,forming a distorted octahedral coordination configuration. The Zn（II） ions were alternately interlinked by carboxylate groups of 4-CPOA with chelating bisbidentate and monodentate modes into a one-dimensional zigzag chain having an intrachain distance of ca. 9.631（1） . Under the direction of supramolecular recognition and attraction,the adjacent chains yield a double-stranded chain through π-π stacking between the phen ligands,which was further expanded into a 2-D framework via strong C–H–π interaction （ca. 2.95（1） ） between the 4-CPOA ligands and into a 3-D supramolecular network by strong hydrogen bond between terminal water molecule and carboxyl group. TG/DTG shows that its chain skeleton is thermally stable up to 419 oC and the blue fluorescent emission of the complex was determined at 471 nm in a solid state with its long decay lifetime of 1.83 ns.     

3,3′-偶氮-二(6-羟基苯甲酸)镉和钴的配合物:[Cd(OSA)(Phen)(H_2O)]_n和[Co(OSA)(Phen)(H_2O)]_n的合成、表征及晶体结构(英文)

利用药物奥沙拉秦钠,邻菲罗啉与Cd(ClO4)2·6H2O或Co(NO3)2·6H2O水热反应分别得到其配合物的晶体[Cd(OSA)(Phen)(H2O)]n(1)(OSA=3,3′-偶氮-二(6-羟基苯甲酸))和[Co(OSA)(Phen)(H2O)]n(2)。单晶结构分析表明两化合物均为一维链状聚合结构,两者的晶体的空间群皆为C2/c。两化合物中,中心金属的配位几何构型均为五配位的五角双锥。3,3′-偶氮-二(6-羟基苯甲酸)通过羧基桥连金属离子形成一维链状聚合物结构。     

Preparation and Thermal Decomposition of [Cr (salen) (H_2O)_2] Cl

Chromium(III)isanessentialtraceelement.Inanactiveform.chronlium(III)asacomponentofglucosetolerancefactor(GTF)canimproveinsulinbiologicalactivity.CrsupplementationinhumansandanimalsreducessymptomsofTypeIIdiabetesandhypoglycemia.Forabetterunderstandingofthenatureofbiologicallyactivechromium(ill)complex,manyGTFmodelcomplexeshavebeenstudiedpreviously'.Here,oneGTFmodelcomplexofN,N'-ethylenebis(salicylideneiminato)diaquochromium(ill)chloride,[Cr(salen)(H,O)=]CIwaspreparedandcharacterized.a…     

Cu(Ⅱ)-牛磺酸缩水杨醛席夫碱-邻菲咯林三元配合物的合成、晶体结构及性质

The title complex was synthesized by reaction of taurine salicylic schiff base(TSSB), O-phenanthroline(phen) and cupric acetate in water-ethanol solution. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 498.00. The crystal structure of the title complex belongs to orthorhombic system with space group Pbcn and cell parameters: a=3.107 2(4) nm, b=1.289 09(18) nm, c= 1.034 78(14) nm; and V=4.144 7(10) nm³, Z=8, D_c=1.596 g·cm^-3, μ=1.197 mm^-1, F(000)=2 048. The compound is an one-dimensional chain complex of infinite length which are connected with hydrogen bonds. The Cu(Ⅱ) was coordinated by two oxygen atoms and three nitrogen while the o atoms of Ac- groups did not participate in the coordination. The Cu(Ⅱ) formed a distorted tetragonal pyramid and the capacities of coordination to Cu(Ⅱ) of atoms was discussed. Besides, the TG-IR of the complex was analyzed. The kinetics of the thermal decomposition reaction of the complex was studied under a non isothermal condition by TG-IR. TG and DTG curves indicate that the complex decomposed in three stages: (?) The kinetic parameters were obtained from the analysis of TG,DTG cures by OZAWA-Flynn-Wall method, and the activation energy and the value of A of the three stages are 74.98 kJ·mol^-1, 286.65 kJ·mol^-1, 87.55 kJ·mol^-1; 9.66×10⁸ s^-1,1.82×10²⁸ s^-1, 3.09×10³s^-1, respectively.     

配合物[Eu(4-MOBA)3(terpy)(H2O)]2的合成、表征、热分解机理及性质

合成了一个新的配合物[Eu(4-MOBA)₃(terpy)(H₂O)]₂ (4-MOBA:4-甲氧基苯甲酸根, terpy:2, 2':6', 2"-三联吡啶)。采用傅里叶变换红外(FTIR)光谱、元素分析和X射线粉末衍射(XRD)技术对标题配合物进行了表征,用X射线单晶衍射仪测定了配合物的晶体结构,在配合物中每个Eu³⁺离子与一个三联吡啶分子、一个水分子和三个羧酸分子结合,配位数为9,羧酸基团的配位模式包含三种:双齿螯合,桥连双齿,单齿。根据热重-差示扫描量热/傅里叶变换红外(TG-DSC/FTIR)联用技术,研究了配合物的热分解机理。配合物的发射光谱显示出Eu³⁺离子的特征荧光发射,表明三联吡啶和4-甲氧基苯甲酸在该体系中可作为敏化集团。另外,文中还讨论了配合物对白色念珠菌和大肠杆菌的抑菌活性。