Synthesis,Crystal Structure,Hirshfeld Surface Analysis,DFT, and DNA-Binding Studies of (E)-2-(3-Hydroxy-4-Methoxybenzylidene)Hydrazinecarbothioamide

Applied Biochemistry and Biotechnology - (E)-2-(3-Hydroxy-4-methoxybenzylidene)hydrazinecarbothioamide 3 was synthesized by reacting thiosemicarbazide with 2-hydorxy-3-methoxybenzaldehyde in dry...     

新型含2-噁唑啉基三角架配体-银(I)一维配位聚合物的合成与结构

通过含2-噁唑啉基三角架配体1,3,5-三(2-噁唑啉基)苯(L)与三氟醋酸银反应合成了配合物[Ag₄(L)₂(CH₃CN)₂(CF₃CO₂)₄]_n (1), 并利用元素分析、电喷雾质谱、X射线单晶衍射等方法对其进行了表征. 晶体结构解析结果显示配合物1属三斜晶系, 空间群P-1, a＝0.83731(6) nm, b＝1.22828(9) nm, c＝1.33997(10) nm, α＝102.9760(10)°, β＝107.3050(10)°, γ＝93.8600(10)°, Z＝1, R＝0.0365, wR₂＝0.0929. 该配合物是由[Ag₄(L)₂(CF₃CO₂)₂]^2＋笼状结构单元通过另外两个三氟醋酸根双桥连形成的一维链状结构. 相邻的链间通过C—H…O氢键进一步扩展为二维网状结构. 电喷雾质谱研究结果显示在实验条件下, 溶液中配合物1是以聚合状态存在的.     

一维链状锰配位聚合物的合成、晶体结构与性能研究

本文合成了1个新的一维链状锰的配位聚合物{[Mn(HL)(phen)(H2O)2].1.5H2O}n,(H3L=2-羟基-5-羧基苯磺酸),并且进行了元素分析、红外、热重、荧光、紫外、粉末XRD及单晶X射线衍射等表征及研究。标题化合物属于单斜晶系,C2/c空间群,a=0.840 57(17)nm,b=1.757 5(4)nm,c=2.873 4(6)nm,β=92.54(3)°,V=4.240 7(16)nm 3,Z=4,R=0.027 0。每个Mn(Ⅱ)离子与邻菲咯啉配体的2个N原子、磺酸配体中的1个磺酸基O原子和羧基O原子以及2个配位水分子配位,展示出扭曲的八面体几何构型。2个相邻的Mn(Ⅱ)八面体单元通过1个磺酸基氧原子和1个羧基氧原子连接形成一维链状结构,该一维链进一步通过氢键作用构筑成三维网状结构。     

铀-钾异核配位聚合物的合成及晶体结构

在水热反应条件下合成了1种新颖的U(Ⅵ)-K异核配位聚合物[UO2K2(pdc)2(H2O)3]n(H2pdc=吡啶-2,6-二羧酸),通过元素分析、红外、紫外光谱及热重对该配合物进行了表征。单晶结构表明:配合物属于单斜晶系,C2/c空间群;晶胞参数分别为a=1.888 5(6)nm,b=1.490 0(5)nm,c=0.740 2(2)nm,β=111.104(10)°。中心铀及钾原子通过2个氮原子和6个氧原子与吡啶-2,6-二羧酸配体结合。不同的[UO2K2(pdc)2].3H2O单元通过氧原子桥联组成三维链状配位聚合物。配位聚合物中存在π…π相互作用及氢键作用。     

(Z)-2-羟基-3-苯甲酰丙烯酸甲酯的合成及晶体结构

标题化合物C11H10O4的晶体结构用X-射线单晶衍射法测定。晶体属单斜晶系, P21/c空间群, 晶胞参数a = 12.136(1), b = 5.559(1), c = 14.615(2) ? b = 96.758(3), V = 979.1(3) ?, Z = 4, Mr = 206.19, Dc = 1.399 g/cm3, F(000) = 432, m(MoKa) = 0.107 mm-1。晶体结构用直接法解出, 经全矩阵最小二乘法对原子参数进行修正, 最终的偏离因子为R = 0.0453, wR = 0.0990。标题化合物形成了1个大的共轭体系, 含有1个稳定的烯醇结构。结构测定表明还存在着1个分子内氢键的结构, 它使烯醇结构更加稳定。     

Synthesis and Crystal Structure of Zn(II) Complex with Tridentate Ligand N-(2-Hydroxy-1-naphthylidene)-L-serine

1 INTRODUCTION As the basic building blocks of proteins or enzy- mes, amino acids are versatile ligands showing flexi- ble coordination modes[1]. Recently, researchers have synthesized some metal complexes with amino acids and their derivatives[2～6]. Considerable efforts have been devoted to the preparation and structure of amino acid Schiff base complexes with transition metals[6～11]. In such cases, some Zn(II) complexes have been reported. However, most of them have been carried out…     

2-(3-羟基-2-吡啶基)-苯并咪唑的合成、晶体结构及光谱研究

在合成2-(3-羟基-2-吡啶基)-苯并咪唑的基础上, 利用NMR (1H, 13C, COSY, HSQC 和HMBC), MS, IR 和UV 进
行了详细表征; 通过X-ray 单晶衍射测定该化合物的晶体结构, 实验结果表明该晶体属于单斜晶系{空间群为P21/c,
a＝14.289(3) Å, b＝10.618(2) Å, c＝12.783(3) Å, β＝93.51(3)°, V＝1935.8(7) Å3, Z＝8}, 很好支持了波谱表征的结果.
2-(3-羟基-2-吡啶基)-苯并咪唑的荧光光谱表明, 该化合物在激发态下存在双质子转移现象, 密度泛函计算结果合理解
释了实验现象.     

三维配位聚合物[Zn（HCO2）2（4,4＇-bipy）]∞的合成、晶体结构及性质研究

以ZnO,HCO2H及4,4-bipy（摩尔比1：3：1.25）溶于H2O和DMF（体积比13：1）,并在60℃反应,合成了标题化合物[Zn（HCO2）2（4,4＇-bipy）∞,对其进行了元素分析、红外光谱等表征,并测定了晶体结构.该化合物晶体属四方晶系,P43212空间群,a=b=0.79675（5）nm,c=1.7627（2）nm,V=1.1190（3）nm^3,Z=4,Dc=1.850 g/cm^3,Mr=311.60,F（000）=632,μ=22.07 cm^-1,最终偏离因子R1=0.0183和wR2=0.0483.该化合物中Zn原子和两个4,4＇-bipy的N原子和四个甲酸根的O原子配位,形成的ZnN2O4八面体通过4,4＇-bipy和甲酸根桥联,组成一种新颖的3D网络结构.同时,研究了该化合物的热性质和荧光性质.     

三维配位聚合物[Zn(HCO2)2(4,4''''-bipy)]∞的合成、晶体结构及性质研究

以ZnO,HCO_2H及4,4'-bipy(摩尔比1∶3∶1.25)溶于H_2O和DMF(体积比13∶1),并在60℃反应,合成了标题化合物[Zn(HCO_2)_2(4,4'-bipy)]_∞,对其进行了元素分析、红外光谱等表征,并测定了晶体结构.该化合物晶体属四方晶系,P4_32_12空间群,a=b=0.79675(5)nm,c=1.7627(2)nm,V=1.1190(3)nm~3,Z=4,Dc=1.850g/cm3,M_r=311.60,F(000)=632,μ=22.07cm-1,最终偏离因子R1=0.0183和wR_2=0.0483.该化合物中Zn原子和两个4,4'-bipy的N原子和四个甲酸根的O原子配位,形成的ZnN_2O_4八面体通过4,4'-bipy和甲酸根桥联,组成一种新颖的3D网络结构.同时,研究了该化合物的热性质和荧光性质.     

Synthesis and Crystal Structure of a Puckered Rhombus Grid-like Coordination Polymer with Bridging Ligand Containing Sulfanyl Linker

Introduction The design and construction of metal-organic frameworks (MOFs), obtained by metal-directed self-assembly from labile metal centers and multidentate bridging ligands, is a rapidly developing area of su-pramolecular chemistry.1-3 Besides the aesthetic struc-tural and fascinating functional motifs, they are of in-terest both for understanding the mechanisms of the assembly process and for the host-guest chemistry asso-ciated with their large central cavities.4-13 It has been documen…     

Synthesis,Crystal Structure and Fluorescence of A 1-D Polymeric Zinc(Ii) Complex with Pyrazine-2-Carboxylate as a Bridging Ligand

A one-dimensional chain complex {[Zn(pyz)(SCN)(H₂O)₂]·H₂O}_∞ (pyz = pyrazine-2-carboxylic anion) has been synthesized and its crystal structure determined by X-ray crystallography. The complex crystallizes in an orthorhombic system and the space group is P2 ₁2₁2₁ with a = 6.873(3), b = 9.847(4), c = 16.466(7) Å. The Zn(II) ion is located in a distorted octahedral environment with two oxygen atoms O(3) and O(4) from terminal ligands of two water molecules, another oxygen atom O(1) from the carboxylate group of pyz, and three nitrogen atoms, N(1), and N(2A) from two different pyz and N(3) from a terminal thiocyanate anion, in which a chelated five-membered ring is formed by coordination of O(1) and N(1) to the Zn(1) atom. Therefore, an infinite zigzag chain consisting of Zn(II) ions and pyz anions is constructed and the chains are linked together with hydrogen bonding from coordinated and uncoordinated water molecules. The fluorescence spectra for the bridging ligand Na(pyz) and the complex were measured at room temperature in aqueous solution and in the solid state.     

一维链状配位聚合物[Cd{5-(NO2)sal}2(2,2'-bipy)]n的合成与晶体结构

A coordination polymer of [Cd{5-(NO2)sal}2(2,2'-bipy)]n (5-(NO2)sal=5-nitrosalicylate, 2,2'-bipy=2,2'-bipyridine) was synthesized by hydrothermal reaction and characterized by elemental analysis, IR and X-raydiffraction single crystal structure analysis. The title complex crystallizes in monoelinic with space group C2/c, a=2.730 8(16) nm, b=1.272 3(5) nm, c=0.674 5(3) nm,β=96.73(2)°, V=2.327(2) nm3, Z=4, R=0.022 2, wR=0.057.The 5-nitrosalicylate anions doubly bridge the Cd(Ⅱ) atoms to form one-dimensional polymeric chain with therepeated eight-membered ring units (Cd-O-C-O)2. The crystal structure is stabilized by intra- and interchainhydrogen bonds interactions.     

Synthesis,Crystal Structure and Magnetism of A 1-D Polymeric Manganese(II) Complex with 2-Hydroxyl-2-Hydroxylate-Malonate as Bridging Ligand

A one-dimensional chain complex {Na[MnL(H₂O)₂]} _n (L = 2-hydroxyl-2-hydroxylate-malonate trivalent anion) has been synthesized and its crystal structure determined by X-ray crystallography. In the complex each Mn ion is located in a distorted octahedral environment with two oxygen atoms O(7) and O(8) from terminal ligands of two H₂O molecules, and four other coordinating oxygen atoms O(1), O(5), O(3A) and O(6A) from two bridging ligands, respectively. Each bridging ligand provides four coordinating oxygen atoms, in which O(6) comes from the hydroxylate, O(5) from the hydroxyl, and O(1) and O(3) from two carboxylate groups, respectively. The O(1) and O(5) atoms coordinate to one Mn ion and the O(3) and O(6) atoms coordinate to another Mn ion; a one-dimensional chain is thereby constructed. The variable-temperature magnetic susceptibility of the complex was measured in the 4–300 K range. The magnetic coupling parameter is consistent with an antiferromagnetic exchange and generates the antiferromagnetic coupling parameter, 2J=–0.0544 cm^–1.     

铜配位聚合物[Cu(C5H6S5)(SCN)]∞的合成和结构研究(英)

The Copper(Ⅰ) supramolecular complexes of 4,5-bis(methylthio)-1,3-dithiole-2-thione (C₅H₆S₅), [Cu(C₅H₆S₅)(SCN)]_∞ 1 and [Cu(C₅H₆S₅)I]_∞ 2, have been prepared and characterized. X-ray structure analysis for complex 1 reveals that the infinite chain structure with polymeric stairs of different lengths is formed through the coordination mode (μ₃) of the thiocyanate bridges. The shorter interchain S…S contacts give rise to a three-dimensional network structure. CCDC: 215668.     

含有药物配体依诺沙星的二维配位聚合物的合成、晶体结构和光致发光性质研究

Two new 2D coordination polymers of[M(Enox)_2]·C_2H_5OH(M=Zn,1 and Co,2;HEnox=1,4-dihydro-1-ethyl-6-fluoro-4-oxo-7-piperazine-1,8-naphtyridine-3-carboxylic acid)were synthesized under hydrothermal con-ditions.The single crystal X-ray diffraction analyses showed that 1 and 2 are isostructural.The Zn(Ⅱ)in 1 and Co(Ⅱ)ions in 2 are six-coordinated in an octahedral environment with an equatorial plane composed of four oxygen atoms:two of them from the 4-oxo and the other two from 3-carboxylate of two coordinated Enox ligands,forming a stablesix-membered chelating ring with the apical positions occupied by two N atoms of the piperazinyl rings.Thus,themolecules were self-assembled into a 2D neutral square grid with cavity dimensions of 1.3399 nm×1.3399 nm for1 and 1.3389 nm×1.3389 nm for 2,respectively.Compound 1 emits strong blue fluorescence on irradiation by UVlight in the solid state at room temperature.     

含硫磷桥基的两核铁羰基簇合物的合成和晶体结构

Fe3(CO)12与杂环二硫代次膦酸盐SP(C6H4OR)(S)N(C6H5)NC(Me)(R=Me,Et)反应,得到两个新的含硫磷桥基的双核铁羰基簇合物Fe2(CO)6[μ-η2-SC(Me)NN(C6H5)P(C6H4OMe)](Ⅰ)和Fe2(CO)6[μ-η2-SC(Me)NN(C6H5)P(C6H4OEt)](Ⅱ),以及簇合物Fe3(CO)9(μ3-S)2(已知).对它们进行了元素分析,IR,1HNMR和MS等谱学表征,并用X-ray衍射技术测定了(Ⅰ)的晶体结构.该晶体属单斜晶系,P2(1)/n空间群,晶胞参数a=11.192(2)A,b=14.272(3)A,c=16.281(3)A,β=108.22(3).,V=2470.2(8)A3,Z=4.两核簇合物中含有两个桥基Fe-S-Fe和Fe-P-Fe,而且-C(7)-N(2)-N(1)-链连结在S、P原子间,形成了两个六员螯环Fe(1)SCNNP和Fe(2)PNNCS,增强了簇合物的稳定性.     

Synthesis and Crystal Structure of (E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl Propionate

(E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl propionate (C22H27O6N, Mr = 401.45) has been synthesized by a condensation reaction of paeonol with tyrosin methyl ester hydrochloride, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 11.91291(15), b = 9.49947(12), c = 19.8727(3) , β = 106.1104(15)°, V = 2160.60(5)3, Z = 4, Dc = 1.234 g/cm3, μ = 0.739 mm-1, F(000) = 856, R = 0.0466 and wR = 0.1461 for 3859 observed reflections with (Ⅰ> 2σ(Ⅰ)). In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking enantiomers, and such units are linked by intermolecular O(5)-H(5)…O(1) and intramolecular N(1)-H(1)…O(1) hydrogen bonds.     

Synthesis,Crystal Structure and Spectral Property of a Water-bridged Co(Ⅱ) Coordination Polymer with 3-Flavonoxylacetic Acid Ligand

A new cobalt complex with flavonoid carboxylate ligand was synthesized and characterized. X-ray diffraction data revealed that the compound crystallizes in the monoclinic crystal system, space group P2_1/c with a = 7.936(3), b = 21.475(7), c = 20.010(7) ?, β = 102.856(14)o, V = 3325(2) ?~3, Z = 4, C_(34)H_(32)CoO_(15), M_r = 739.53, D_c = 1.477 g/cm~3, F(000) = 1532, μ = 0.591 mm~(-1), R = 0.1123 and w R = 0.1419. In the crystal structure, the Co(Ⅱ) shows 6 coordination geometry, and the flavonoid ligand coordinated with the Co(Ⅱ) ion in a monodentate mode. Hydrogen bonding interactions and π-π stacking interactions lead to the three-dimensional stacking of crystal and increase its stability. Moreover, the thermal stability and luminescent properties of the complex are also investigated. The fluorescence of the complex shows a great reduction of the intensity than that of the ligand.     

Synthesis and Crystal Structure of a Tetravalent Cerium Complex with a Bridging Triphenolate Ligand

Reaction of(NH4)2 Ce(NO3)6 first with NaOtBu in a 1:6 molar ratio in THF, then with an equivalent of 2-bis(salicylidieneamino)methylphenol(H3 salmp) affords the(salmp)2 Ce2-(O)Na4(OtBu)4(THF)4 ·2C6 H6 complex. It crystallizes in monoclinic, space group C2/c with a = 16.5218(14), b = 23.992(2), c = 21.9454(18), β = 97.470(1)°, V = 8625.1(12)3, Z = 4, Mr = 1811.96, Dc = 1.395 g/cm3, μ = 1.126 mm-1, F(000) = 3736, S = 1.061, R = 0.0405 and wR = 0.0932(I 2σ(I)).