氧钒配合物[VO2(C10H8N2)2]·NH4HSO4的合成、晶体结构和荧光性能

在80℃下合成了1个新的标题化合物,通过元素分析、红外和单晶X-射线进行了表征。标题化合物属于三斜晶系,P-1空间群,a=0.671 14(9)nm,b=1.165 88(14)nm,c=1.401 83(18)nm,α=96.410 0(10)°,β=94.825 0(10)°,γ=97.901(2)°,V=1.074 2(2)nm3,Z=2。配合物由1个VO2、两个2,2’-联吡啶分子和1个NH4HSO4构成,NH4HSO4分子通过氢键在a方向形成一维超分子链状结构,通过荧光光谱研究了该化合物的荧光性质。     

一维梯状配位聚合物[ZnL（bbi）0.5（H2O）]n的结构及性质研究

一种新的配位聚合物[ZnL(bbi)0.5(H2O)]n(1)(L=3-羧甲基苯甲酸,bbi=1,4-二咪唑丁烷)被合成出来。结构分析表明化合物1结晶于单斜晶系,P21/n空间群,a=0.9674(3)nm,b=0.6294(2)nm,c=2.4918(7)nm,β=96.91(1)°。两种配体与金属离子连接形成一维梯状链,链间通过分子间相互作用形成二维网络结构。化合物1的元素分析,红外光谱,热重分析和荧光性质被表征。     

[Cd2（PIEA）2（μ-Cl）2Cl2]配合物的合成及晶体结构

以[2-(2-吡啶基)咪唑-1-基]乙酸乙酯为配体合成了配合物[Cd2(PIEA)2(μ-Cl)2Cl2],测定了其X-射线单晶结构。晶体学数据:P–l空间群,a=0.8978(3)nm,b=0.5462(3)nm,c=1.0719(3)nm,α=84.335(3)°,β=71.245(3)°,γ=62.323(3)°,V=0.7622(3)nm3,Z=1,s=1.069,最终残余因子(I>2σ(I)),Rl=0.0249,wR2=0.0712;对于全部数据Rl=0.0271,wR1=0.0726。     

一价铜配合物[Cu（pyz）（NO3）]n的水热合成及结构表征

利用H3PO3的还原性,合成了一个一价铜配合物[Cu(pyz)(NO3)]n(1)(pyz:吡嗪),并利用元素分析、红外光谱、单晶X-射线衍射对配合物(1)进行了表征。单晶结构分析表明,配合物(1)中的一价铜离子通过硝酸根和吡嗪的桥连作用,连接成二维层状结构。     

超分子化合物(C10H10N2)Co（SCN）4的合成、晶体结构和热稳定性

在室温下合成了一个新的超分子配合物(C10H10N2)Co(SCN)4,通过元素分析、红外和单晶X-射线进行了表征。标题化合物属于正交晶系,P 21 21 2空间群,a=1.283 32(11)nm、b=1.297 53(12)nm、c=0.544 12(5)nm、V=0.906 04(14)nm3、Z=2。在化合物中,每个Co2+离子与4个SCN-的4个N原子形成变形的四面体几何构型、4,4’-联吡啶的两个氮原子双质子化,并与SCN-的S原子形成N—H…S氢键,构成一维氢键超分子链。通过热重分析研究该化合物的热稳定性。     

{CdI4[（C4H6N2）2+C2H4]}n的合成与晶体结构

用溶液挥发法合成了一个新的有机-无机杂化聚合物{Cd I4[(C4H6N2)2+C2H4]}n,并通过X-射线单晶衍射仪对其进行结构表征。化合物1属于单斜晶系,C2/c空间群,a=34.383(7)?,b=8.1299(16)?,c=15.199(3)?,β=112.47(3)°,V=3926.0(13)?3,Z=8。化合物1由有机阳离子[(C4H6N2)2+C2H4]和无机[Cd I4]2-阴离子组成一个零维簇结构,相邻的簇与簇之间通过氢键作用形成三维超分子网状结构。     

超分子化合物[（4,4′-联吡啶）3H5][PMo10V2O40]·3H2O水热合成与表征

利用水热合成法合成了一个新的杂多（Keggin）基超分子化合物[（4,4′-联吡啶）₃H₅][PMo₁₀V₂O₄₀]·3H₂O,并且通过元素分析、红外光谱和X射线单晶衍射的方法确定了该化合物的晶体结构。结构分析表明,该化合物属于单斜晶系,C2/c空间群,晶胞参数a=1.534 9（9）nm,b=1.813（1）nm,c=2.097（8）nm,α=90°,β=101.36°,γ=90°,V=5.725（2）nm3,Z=4,R1=0.050 7,wR2=0.163 8。     

2-甲基-4-(4-(吡啶-4-乙炔基)苯基)-3-丁炔-2-醇的合成及结构表征

由1,4-二碘代苯出发,经过两步Sonogashira偶联反应合成标题化合物2-甲基-4-(4-(吡啶-4-乙炔基)苯基)-3-丁炔-2-醇。通过1 H NMR、13 C NMR核磁共振、X射线单晶衍射等手段对化合物的结构进行了表征。结果表明,该化合物属于单斜晶系,空间群为P2(1)2(1)2(1)。晶体学参数:a=0.060754(15)nm,b=0.081700(19)nm,c=0.32073(7)nm,α=90.00°,β=90.00°,γ=90.00°,V=15.920(7)nm3,Z=8。     

4-甲基水杨酸铜(Ⅱ)配合物的合成与表征

采用溶剂热法合成了一个配合物[Cu(4-Me-SA)(Phen)]·2H2O(Phen=1,10-邻菲啰啉,4-Me-SA=4-甲基水杨酸),用X射线单晶衍射仪测定了该化合物的晶体结构,通过元素分析(EA),红外光谱(FTIR),紫外-可见光谱(UV-Vis),热分析(DSC-TGA)和荧光光谱(FS)对其结构和性质进行了分析与表征。结果表明:晶体属于单斜晶系,P2(1)/c空间群,晶胞参数a=0.8324(3)nm,b=1.2644(5)nm,c=1.7493(7)nm,α=90.00°,β=100.404(7)°,γ=90.00°,V=1 810.8(12)nm3,Z=4。配位原子分别来自于1个4-甲基水杨酸配体的2个氧原子和1个邻菲啰啉配体的2个氮原子,形成配位数为4的稳定结构。配合物中的氢键和π-π堆积作用使其自组装成1个稳定的三维立体结构。发光性能测试表明,该配合物具有荧光性质。     

类金刚烷型配合物[Cd（C6H5O2N）2（H2O）]n的水热合成及其晶体结构研究

以Cd(CH3COO)2和烟酸(C6H5O2N)为原料,采用水热法合成了类金刚烷型配位聚合物[Cd(C6H5O2N)2-(H2O)]n,利用元素分析、X射线单晶衍射对其结构进行了表征。该配合物属于正交晶系,Pbca空间群,a=1.144 9(5)nm,b=1.208 3(5)nm,c=1.742 8(5)nm,α=β=γ=90°,V=2.411(16)nm3,Z=8,dc=2.064 g/cm3,μ=1.834 mm-1,F(000)=1 472,R1=0.022 6,wR2=0.041 8。     

新型含α-Keggin结构超分子化合物（C6H10N2）2[SiW12O40]的合成、结构表征及性质研究

利用水热合成法合成了目标化合物（C6H10N2）2[SiW12O40]通过X射线单晶衍射仪确定了晶体结构,晶体属单斜晶系,空间群C2／m。通过红外、热重分析和循环伏安曲线对晶体进行了结构表征、晶体的热稳定性和氧化还原性研究。晶体中的α-Keggin阴离子、有机配体通过氢键相互作用,形成超分子化合物。     

Preparation and characterization of H4SiW12O40@MIL-100 (Fe) and its catalytic performance for synthesis of 4,4'-MDA

The catalytic performance of commonly used heteropoly acids(H_3 PW_(12)O_(40). H_4 SiW_(12)O_(40) and H_3 PMo_(12)O_(40)) for the synthesis of 4,4'-methylenedianiline(4.4'-MDA) from aniline and formaldehyde was evaluated and the result showed that H_4 SiW_(12)O_(40) with moderate acid strength exhibited the best catalytic performance. Then H_4 SiW_(12)O_(40)@MIL-100(Fe) was prepared by encapsulating H_4 SiW_(12)O_(40) within the pores of MIL-100(Fe) to facilitate its recovery and reuse. The prepared H_4 SiW_(12)O_(40)@MIL-100(Fe) was characterized by means of FT-IR, N_2 adsorption-desorption, XRD, TG and then the catalytic performance was evaluated. The result showed that H_4 SiW_(12)O_(40) was highly dispersed in the pores of MIL-100(Fe), and both the Keggin structure of H_4 SiW_(12)O_(40)and the crystal skeleton structure of MIL-100(Fe) could be effectively preserved. Furthermore. H_4 SiW_(12)O_(40)@MIL-100(Fe) showed excellent catalytic performance under the following reaction conditions: a molar ratio of aniline to formaldehyde = 5, a mass ratio of catalyst to formaldehyde = 1.2, a reaction temperature of 120 ℃and a reaction time of 6 h. Under the above reaction conditions, the conversion of aniline was 41.1%, and the yield and selectivity of 4.4'-MDA were 81.6% and 79.2%, respectively. Unfortunately, an appreciable loss in the catalytic activity of the recovered H_4 SiW_(12)O_(40)@MIL-100(Fe) was observed because of the blocking of the pores and the change of the acidity resulted from the adsorption of alkaline organics such as aniline and 4,4'-MDA.The adsorbed alkaline organics could be cleaned up when the recovered catalyst was washed by methanol and DMF. Then the catalyst was effectively reused up to three cycles without much loss in its activity.     

[Pb(DNI)_2(H_2O)_4]的制备和晶体结构

通过2,4-二硝基咪唑(2,4-DNI)的钠盐水溶液与硝酸铅的水溶液反应,制备出了2,4-二硝基咪唑铅配合物;采用自然挥发法培养出了适于X光结构测定的单晶,X射线衍射测定结果为,晶体属单斜晶系,空间群为Cc,晶体学参数为:a=6.517(3)×10-1nm,b=17.131(6)×10-1nm,c=14.082(7)×10-1nm,α=90.00(3)°,β=97.80(4)°,γ=90.00(4)°,V=1 557.5(12)×10-3nm3,Z=4,Dc=2.531 g/cm3,μ=11.001 mm-1,F(000)=1 120,最后偏离因子R为0.022 6。根据红外光谱、元素分析和X射线衍射分析结果,确定了2,4-二硝基咪唑铅配合物的化学组成为C6H10O12N8Pb,分子结构式为[Pb(DNI)2(H2O)4]。     

三维配位聚合物[Cu_2(pda)_2(bpp)]的合成和结构

利用间苯二乙酸,1,3-二(4-吡啶)丙烷和硝酸铜在水热条件下反应制备了一种新型三维配位聚合物[Cu2(pda)2(bpp)](1)(H2pda=间苯二乙酸,bpp=1,3-二(4-吡啶基)丙烷)。通过X单晶衍射测定了晶体结构,并用元素分析、红外光谱、热重分析等技术对其进行表征。配合物属单斜晶系,空间群为P2(1)/c,a=24.412(1)nm,b=12.632(5)nmc,=10.076(4)nm,β=95.134(4)°,Z=4。晶体结构分析表明:在配合物1中,铜离子均形成六配位微扭曲八面体,较为特殊的是在双核结构单元中存在着轮浆[Cu2(CH2COO)4]次级单元。这些次级单元通过顺式桥连双齿间苯二已酸的连接形成(4,4)网格二维波浪面。毗邻的波浪网面又通过1,3-二(4-吡啶基)丙烷配体的连接支撑,拓展为复杂的三维网络结构。     

Supramolecular Architectures in Three Metal(II) Coordination Polymers with 2,5-Dichloroterephthalate and Flexible Bis(Benzimidazole) Ligands

Three supramolecular coordination polymers, namely [Ni(L1)(DCTP)(H₂O)] _n (1), [Cu(L2)(DCTP)] _n (2), [Co(L3)(DCTP)] _n (3) (L1?=?1,5-bis(5,6-dimethylbenzimidazole)pentane, L2?=?1,4-bis(5,6-dimethylbenzimidazole)butane, L3?=?1,4-bis(benzimidazole)-2-butylene) have been hydrothermally synthesized and characterized by single crystal X-ray structure determination, FT-IR, elemental analysis, X-ray powder diffraction (XPD), and thermogravimetric analysis (TGA). CP 1 exhibits 2D 6³ honeycombed network structure, which is further extended into a 3D Moganite (mog) supramolecular framework by classical O–H?O hydrogen-bonding interaction. CPs 2 –3 present 2D (4,4) layers, and 3D supramolecular frameworks that are formed by π–π stacking interactions. Furthermore, the catalytic activities of CPs 1–3 for the degradation of methyl orange in a Fenton-like process has been investigated, and CPs 1–3 show strong photoluminescence properties at room temperature in solid state.     

Ternary Copper(II) Complexes With Indomethacin, a Potent Non-Steroidal Antiinflammatory Drug. Crystal Structure of Bis (Dimethylformamide)-Tetrakis[1-(4-Chlorobenzoyl)-5-Methoxy-2-Methyl-1-H-Indole-3-Acetato]Dicopper(II). Antiinflammatory Properties and Prevention of Gastrointestinal Side Effects by Nanocapsules

Two ternary copper(ll) complexes of indomethacin [1-(4-chlorobenzoyl)-5-methoxy-2- methyl-1-H-indole-3-acetic acid] called hereafter lndo, were prepared and characterized by single crystal X-ray diffraction. The first complex Cu(2)(Indo)(4)(DMF)(2) I crystallizes in space group P-1 (a = 10.829(2), b = 13.379(2), c = 16.491(3) A; alpha = 105.58(2), beta = 101.06(2), gamma = 106.96(2) degrees ; V= 2104.6(6) A(3), Z= 1). The title molecule is a centrosymmetric binuclear complex, with Cu atoms bridged by the carboxylate moieties of four indomethacinate ligands. The four nearest O atoms around each Cu atom form a square planar arrangement with the square pyramidal coordination completed by the O atom of N,N'-dimethylformamide. Daily administration for seven days of 1 mg/kg of indomethacin, I and I encapsulated into liposomes induces a weak inflammation of rat gastrointestinal tract. I was less inflammatory than indomethacin but the better protection was brought by encapsulation of the compound. This might be of interest in sustained therapies of chronic inflammatory diseases.     

Synthesis and Anti-Candida Activity of Cobalt(II) Complexes of Benzene-1,2-Dioxyacetic Acid (bdoaH(2)). X-Ray Crystal Structures of [Co(bdoa)(H(2)O)(3)] 3.5H(2)O and {[CO(phen)(3)](bdoa)}(2)24H(2)O (phen = 1,10-Phenanthroline)

Co(CH(3)CO(2))(2)4H(2)O reacts with benzene-1,2-dioxyacetic acid (bdoaH(2)) to give the Co(2+) complexes [Co(bdoa)(H(2)O)(3)]H(2)O (1a) and [Co(bdoa)(H(2)O)(3)] 3.5H(2)O (1b). Subsequent reaction of 1a with 1,10- phenanthroline produces [CO(phen)(3)] bdoa10H(2)O (2a) and {[CO(phen)(3)](bdoa)}(2)24H(2)O (2b). Molecular structures of 1b and 2b were determined crystallographically. In 1b the bdoa(2-)- ligates the metal by two carboxylate oxygens and two ethereal oxygens, whereas in 2b the bdoa(2-) is uncoordinated. The Mn(2+) and Cu(2+) complexes [Mn(bdoa)(phen)(2)]H(2)O (3) and [Cu(pdoa)(imid)(2)] (4) were also synthesised, 1a-4 and other metal complexes of bdoa H(2) (metal = Mn(2+), Co(2+) ,Cu(2+), Cu(+) ) were screened for their ability to inhibit the growth ofhe yeast Candida albicans. Complexes incorporating the 1,10-phenanthroline ligand were the most active.     

水热合成阻燃剂Zn[B_3O_4(OH)_3]及其结构的探讨

在水热的条件下合成了硼酸锌Zn[B3O4(OH)3],用组装合成的思想来描述该化合物的结构。该化合物系三硼氧聚阴离子B3O5(OH)3通过共享环外氧原子形成一维无限链,三硼氧聚阴离子链通过与ZnO4或氢键作用连接起来的网状结构。使用红外光谱、热重分析及X射线单晶衍射分析手段对该化合物结构进行了表征。该化合物属单斜晶系,P21/n空间群,晶胞参数a=6.8482(4),b=9.7967(6),c=7.7014(4),β=107.0290(10),V=494.03(5)3,Z=4。     

超分子化合物（C12N2H9）2（C12N2H8）[SW12O40]的合成与结构表征

利用水热法合成了超分子化合物（C12N2H9）2（C12N2H8）[SW12O40],通过元素分析和X射线单晶衍射确定了其晶体结构,该晶体为正交晶系,P2（1）2（1）2（1）空间群,晶胞参数为a=12．0168（3）A^。,b=21．0534（6）A^。,c=22．5820（6）A^。,V=5713．1（3）A^。^3,α=β=γ=90°,Z=4,Dc=3．977mg·m^-3,并通过IR和XRD进行了结构表征,采用热重分析研究了晶体的热稳定性。该化合物由邻菲罗林和Keggin结构[SW12O40]^2-阴离子组成,以氢键自组装成超分子结构化合物。