三维超分子化合物[Zn(C6H4O2N)2·(H2O)4]n的水热合成及晶体结构

用2-羧基吡啶和六水合氯化锌反应制备了一种新的三维氢键超分子配合物,经X-射线衍射分析确定了单晶结构。该晶体属单斜晶系,P2(1)/n空间群,晶胞参数为:a=9.836(2),b=5.2256(10),c=14.611(3),Mr=381.64,β=90.01(3)°,V=751.0(3)3,Z=2,Dc=1.688Mg.m-3,F(000)=392,μ=1.680mm-1,R=0.0258,wR=0.0612。共收集2159个衍射数据,其中1273个为独立衍射点(Rint=0.0332),可观测点数1139个(I>2σ(I))。结果表明,在组成该超分子体系的基本结构单元[Zn(C6H4O2N)2.(H2O)4]中,Zn(Ⅱ)离子形成六配位的畸变的八面体构型,配合物单元之间通过氢键OH…O相互连接,形成了无限延伸的具有网状结构的三维超分子体系。     

三维超分子化合物[Zn(C6H4O2N)2·(H2O)4]n的水热合成及晶体结构

用2-羧基吡啶和六水合氯化锌反应制备了一种新的三维氢键超分子配合物,经X-射线衍射分析确定了单晶结构.该晶体属单斜晶系,P2(1)/n空间群,晶胞参数为a=9.836(2)(A),b=5.2256(10)(A),c=14.611(3)(A),Mr=381.64,β=90.01(3)°,V=751.0(3)(A)3,Z=2,Dc=1.688Mg·m-3,F(000)=392,μ=1.680mm-1,R=0.0258,wR=0.0612.共收集2159个衍射数据,其中1273个为独立衍射点(Rint=0.0332),可观测点数1139个(I＞2σ(I)).结果表明,在组成该超分子体系的基本结构单元[Zn(C6H4O2N)2·(H2O)4]中,Zn(Ⅱ)离子形成六配位的畸变的八面体构型,配合物单元之间通过氢键OH…O相互连接,形成了无限延伸的具有网状结构的三维超分子体系.     

A 2D Cu(I) triazolate coordination polymer: Synthesis and characterization of [Cu4Br4(C8H8N4)2]·H2O

The title compound, [Cu₄Br₄L₂]·H₂O (1), (L = C₈H₈N₄, 4-(4-aminophenyl)-4H-1,2,4-triazole) was synthesized from a hydrothermal reaction and characterized by single-crystal X-ray diffraction analysis, IR, and fluorescent spectroscopy. The structure of 1 shows a two-dimensional rectangular grid layer, which is formed by the interconnection of Cu₄Br₄ step-like and the tris(monodentate) L bridges, with guest water molecules filling in the grid. Compound 1 in the solid state exhibits deep green emission with maximum at 538 nm.     

配合物[Cu（L）2]ECu’（L）2]·CH3OH·3H2O的合成和结构表征

以邻氯蜷苯磺酸与吡啶-2-甲醛进行缩合得到席夫碱配体（KL）,然后与Cu（AeO）2．H20进行配位反应,得到了席夫碱配合物[Cu（L）2][Cu’（L】2】’CH3OH·3H2O,用面素分析、FT—IR和X-射线单晶衍射进行r表征。结果表明t配合物属]i单斜晶系,P21／c空间群。配合物的一一个独立单元由置个品格水分子、一个晶格甲醇分子和两个不同的单核铜单元构成。有趣的是,这两个荤核铜单元的组成完全相同但配位模式不同,它们均由一个铜离子和两个脱质子的席夫碱配体组成,其中一个瞥核铜单元中的两个磺酸基均参与了配位,另一个则只有一个磺酸基配位。     

A new open-framework zinc arsenate [C4N3H16]2[Zn5(AsO4)4(HAsO4)2]

A three-dimensional zinc arsenate with an interrupted zeolitic framework (?IIO), [C₄N₃H₁₆]₂[Zn₅(AsO₄)₄(HAsO₄)₂], I has been synthesized solvothermally. The structure is built up from ZnO₄, AsO₄ and HAsO₄ tetrahedral units connected alternatively through their vertices forming the 3-D structure possessing one-dimensional channels bound by 10 T-atoms (T = Zn, As). The framework density of the structure is 10.4 T-atoms which indicates considerable openness in its structure.     

配合物[Cd(IA)_2(H_2O)_4]的合成及晶体结构

以硝酸镉与吡啶-4-甲酸(HIA)为原料在水热条件下合成了配合物[Cd(IA)2(H2O)4],并用红外光谱、元素分析和X射线单晶衍射进行了表征。该配合物属三斜晶系,P-1空间群,晶胞参数为:a=6.4400(5)nm,b=6.9489(6)nm,c=9.4051(8)nm,α=95.2600(10)°,β=104.580(2)°,γ=111.570(2)°,V=0.037079(5)nm3。配合物中Cd(Ⅱ)位于变形八面体环境中,与分属于两个吡啶-4-甲酸根的2个N原子以及来自于四个配位水分子的O原子配位。     

Synthesis and structure of a mixed valence metal carbitoxide complex: Eu3[O(CH2CH2O)2CH2CH3]4(OC6H3iPr2-2,6)3

The direct reaction of europium metal with HO(CH₂CH₂O)₂CH₂CH₃ followed by treatment with 2,6-ⁱPr₂C₆H₃OH leads to the crystallographically-characterizable, mixed valent carbitoxide product Eu₃[O(CH₂CH₂O)₂CH₂CH₃]₄(OC₆H₃ⁱPr₂-2,6)₃ (1), which contains bridging alkoxide ligands and both terminal and bridging aryloxide ligands.     

两种基于DMBA原位分解的配位聚合物{[Y(C_2O_4)_(1.5)(H_2O)_2]·H_2O}_n和{[Y(C_2O_4)_(1.5)(H_2O)_3]·2H_2O}_n的合成及结构研究

以DMBA(1,3-二甲基巴比妥酸)为底物,通过其原位分解产物H2C2O4(草酸)的自组装,分别制备了两种新颖的由压力调控的二维层状配位聚合物{[Y(C2O4)1.5(H2O)2]·H2O}n(1)和{[Y(C2O4)1.5(H2O)3]·2H2O}n(2)。在水热合成条件下,考察了不同阳离子、阴离子及溶剂对终产物分离的影响。结果显示,配合物(1)的构筑需在Y(Ⅲ)离子及去离子水同时存在的条件下完成。在此基础上,对反应机理进行了初步探究,发现氧化反应、亲核加成反应及消除反应等多种有机转化过程或可诱导原位开环产物的形成。     

Synthesis,characterizations, and crystal structure of a novel 2D metal phosphonate: Na2[Cd2(H2O)3(O3PCH(OH)CO2)2] · 2H2O

A novel cadmium phosphonate compound Na₂[Cd₂(H₂O)₃(O₃PCH(OH)CO₂)₂] · 2H₂O (1) has been synthesized by hydrothermal reaction at 120 °C and characterized by single-crystal X-ray diffraction as well as with infrared spectroscopy, elemental analysis and thermogravimetric analysis. The structure of compound 1 comprises CdO₆ octahedra and CdO₇ pentagonal bipyramid connected by [O₃PCH(OH)CO₂]³⁻ to form a 2D layered structure with a one-dimensional channel system and the charge-compensating Na⁺ cations being located between two adjacent layers.     

Synthesis and characterization of strontium 1,3,5-benzenetricarboxylate, [Sr3(1,3,5-BTC)2(H2O)4]·H2O

A three-dimensional strontium-based metal-organic framework was constructed using 1,3,5-benzenetricarboxylic acid, [Sr₃((OOC)₃C₆H₃)₂(H₂O)₄]·H₂O. This new compound was synthesized hydrothermally and is a rare example of a strontium metal-organic network. The compound network contains three distinct Sr centers, one of which is seven-coordinate and the other two are nine-coordinate geometry. The benzene rings form a herring-bone type of arrangement down the a-axis. The material is thermally stable to ca. 230 °C and transforms to an unknown material before finally decomposing to phase-pure SrCO₃ at 650 °C. The synthesis, structure, morphology and materials properties are discussed.     

新型配位聚合物[Co(C_5H_5N)_2(H_2O)_2(O_2CC_2H_4CO_2)]_n的水热合成和晶体结构

以CoCl2.6 H2O和丁二酸(CH2COOH)2、三乙胺为原料,在中温水热反应条件下,合成了一种新型配位聚合物[Co(C5H5N)2(H2O)2(O2CC2H4CO2)]n,并对其进行了X射线单晶衍射和红外光谱测定。晶体数据如下:正交晶系,Pbca空间群,a=11.91940(12)nm;b=8.91440(10)nm;c=15.1025(2)nm;α=90.00;β=90.00;γ=90.00;V=1604.71(3)nm3;Z=4;Dc=1.528 g/cm3;μ=1.101 mm-1;F(000)=764;R1=0.0492,wR2=0.0831。该晶体通过分子间氢键和相互作用的π-π键形成一维的链状结构。     

Synthesis and structure of the n = 4 member of the framework aluminium alkylenediphosphonate series Al2[O3PC n H2n PO3](H2O)2F2

We report here the solvothermal synthesis and crystal structure of the hybrid inorganic-organic framework material Al₂[O₃PC₄H₈PO₃](H₂O)₂F₂?2H₂O (monoclinic, 1P2₁ /m, a = 4.961(2) Å, b = 11.930(5) Å, c = 10.727(5) Å, β = 93.972(6)^°, Z = 2, R(F, F ² > 2σ) = 0.094, R _w(F ², all data) = 0.262), the third member of the Al₂[O₃PC _n H_{2 n} PO₃](H₂O)₂F₂ framework series. The structure is formed from corrugated chains of corner-sharing AlO₄F₂ octahedra in which alternating AlO₄F₂ octahedra contain two fluorine atoms in a trans or a cis configuration. The diphosphonate groups link the chains together through Al-O-P-O-Al bridges and through the butyl groups to form a three-dimensional framework structure containing a one-dimensional channel system consisting of one type of channel only. The channels contain four extra-framework water molecules per unit cell. The formation of this member of the series shows that the form of the alkyl chain can successfully define the number of channel types and the channel length in this hybrid framework system.     

[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]。     

配位聚合物[Zn(phen)(H_2O)_2SO_4]_n的合成与晶体结构

通过扩散法得到了一个新的配位聚合物[Zn(phen)(H2O)2SO4]n[phen=邻菲啰啉]。通过X-ray单晶衍射对配合物的结构进行了表征。配合物属单斜晶系,Cc空间群,晶胞参数:a=15.1399(10),b=14.1420(10),c=6.6994(5),α=90°,β=103.458(1)°,γ=90°,V=1395.01(17)3,Z=2,μ=0.752 mm-1,R1=0.0214,wR2=0.0602。     

Synthesis and structure of a high-nuclearity oxomolybdenum(V) complex, [Mo12O28(OC2H5)4(C6H7N)8]

(PyH)[MoOBr₄(H₂O)]·2/3PyHBr (PyH⁺=pyridinium cation, C₅H₅NH⁺) yielded upon the solvothermal reaction with ethanol and 4-methylpyridine (4-MePy, C₆H₇N) a novel oxoethoxomolybdenum(V) cluster, [Mo₁₂O₂₈(OC₂H₅)₄(4-MePy)₈] 1. Molybdenum atoms are grouped into six Mo^V₂ pairs linked by single metal–metal bonds. Three crystallographically independent Mo–Mo distances are 2.5578(14), 2.5981(14) and 2.6489(16) Å.     

A novel coordination polymer with double chains structure: hydrothermal syntheses,structures and magnetic properties of [Cu(phen)(H2O)2SO4]n (phen=1,10-phenanthroline)

A coordination polymer [Cu(phen)(H₂O)₂(SO₄)]_n (1) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, thermogravimetric analysis, and single crystal X-ray diffraction. This compound displays a novel double chains structure, in which each one-dimensional chain is constituted by the distorted octahedral complex of copper(II) bridged through bidentate sulfate ligands. Magnetic susceptibility measurement of 1 has been performed down to 2 K. Although paramagnetic behavior is dominantly manifested, compound 1 shows a weak antiferromagnetic interaction on cooling from room temperature to 2 K.     

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。     

Dielectric dispersion in [N(C2H5)4]2ZnCl4 single crystal

Temperature dependence of the complex dielectric permittivity of [N(C₂H₅)₄]₂ZnCl₄ crystal was measured in the frequency range 300 Hz / MHz. Jump-wise changes in the real and imaginary components of ε* were observed for the three crystallographic directions at the phase transition temperature. The dielectric dispersion clearly apparent in the high-temperature phase, rapidly disappears at the phase transition. The anomalous changes in the dielectric permittivity are related to vibrations of the tetraethylammonium ion. The activation energy of these vibrations amounts to 40 kJ/mol.