一个新颖镍配位阳离子修饰的还原型钼磷酸盐：Ni[Mo6O12(OH)3(PO4)(HPO4)3]2][Ni(H2O)2][Ni(H2O)(bipy)2]4·5H2O

水热合成并通过红外、热重、单晶X-射线衍射表征了一个新颖镍配位阳离子修饰的还原型钼磷酸盐,Ni[Mo₆O₁₂(OH)₃(PO₄)(HPO₄)₃]₂][Ni(H₂O)₂][Ni(H₂O)(bipy)₂]₄·5H₂O。单晶X-射线衍射研究表明,两个{Mo₆P₄}簇单元通过一个镍离子连接形成一个Ni[Mo₆P₄]₂二聚结构单元,其进一步和其他的镍配位阳离子连接成钼磷酸盐一维链状结构。在H₂O₂存在下的液－固体系中,使用该化合物催化氧化苯甲醛的探针反应结果表明,该化合物具有较高的催化氧化活性。     

[(2,2′-bipy)2VO2](H2BO3)·3H2O的水热合成和晶体结构

A hydrothermal reaction of NaVO₃, Ce(NO₃)₃, H₃BO₃, 2,2′-bipyridine and water in a molar of 1∶2∶3∶2∶333 gives a yellow crystal [(C₁₀H₈N₂)₂VO₂](H₂BO₃)·3H₂O. It crystallizes in a triclinic with space group P1 and unit cell parameters a=0.6643(1)nm, b=1.1794(2)nm, c=1.4822(3)nm, α=101.39(3)°, β=101.59(3)°, γ=97.15(3)°, Z=2, D_c=1.542g·cm^-3, μ=0.508mm^-1, F(000)=528, R₁=0.0736, wR₂=0.1998,Goof=1.071. X-ray crystallographic study showed that the VN₄O₂ octahedron unit is distorted, in which the V1 atom is coordinated by two terminal O1 and O₂ atoms, and N1, N2, N3 and N4 atoms from two 2,2′-bipy ligands. The hydrogen bonding are observed between 2,2′-bipy and adjacent terminal oxygen atom. It is noteworthy that π-π stacking interaction between adjacent 2,2′-bipy groups plays an significant role in stabilization of the structure of crystal. CCDC: 194327.     

[Ni(en)3]4[HVⅣ12VⅤ6O42(PO4)]复合物的合成及晶体结构

A new complex [Ni(en)₃]₄[HV^Ⅳ₁₂V^Ⅴ₆O₄₂(PO₄)] has been hydrothermally synthesized and characterized by X-Ray diffraction, IR and Elemental analysis. Single crystal X-ray analysis indicates that this compoud crystallizes in cubic system,space group Im 3m with a=17.4081(2)?, V=5275.38(10)?³, R=0.0420, wR=0.1055, Z=2, D_c=1.663g·cm^-3, μ=2.297mm^-1, F(000)=2636. The crystal structure consists of [Ni(en)₃]²⁺ cations and {HV₁₈O₄₂(PO₄)}^8- cluster anion which construct from 18 {VO₅} square pyramids. The VO₅ pyramids joined each other to form a {V₁₈O₄₂} cage hosting a tetrahedral {PO₄}^3- moiety with disordered oxygen atoms. CCDC: 185574.     

N，N′-(2-苯并咪唑基甲基)亚氨基甲基膦酸的双核镍化合物Ni2(bbimp)2(4，4′-bipy)(H2O)2·2H2O和Ni2(bbimp)2(H2O)2][Ni(bbimp)(H2O)2]2·4H2O

该文报道了N，N′-(2-苯并咪唑基甲基)亚氨基甲基膦酸{bbimpH₂，[(C₇H₅N₂)CH₂]₂NCH₂PO₃H₂}的2个镍化合物Ni₂(bbimp)₂(4，4′-bipy)(H₂O)₂·2H₂O (1)和[Ni₂(bbimp)₂(H₂O)₂][Ni(bbimp)(H₂O)₂]₂·4H₂O (2)。化合物1是4，4′-联吡啶作为桥连配体的中性双核结构。化合物2含有1个中性的[Ni₂(bbimp)₂(H₂O)₂]双核分子与2个中性的[Ni(bbimp)(H₂O)₂]单核分子。双核分子单元中的2个Ni(Ⅱ)离子被2个膦酸氧桥连。在化合物2中，膦酸氧桥连的2个Ni(Ⅱ)离子之间存在铁磁性相互作用。     

一个新颖敞开结构硼磷酸盐的合成、结构、热和磁学性质：NH4Mn(H2O)2BP2O8· H2O

利用新的模板剂在水热条件下合成结构新颖的硼磷酸盐化合物NH₄Mn(H₂O)₂BP₂O₈·H₂O,单晶X射线衍射分析证明化合物属六方晶系,空间群为P6₁22,a = 0.9652(2) nm,c = 1.5792(5) nm,V = 1.2740(5) nm³,Z = 6．化合物所具有的三维敞开结构由硼磷酸盐螺旋带{[BP₂O₈]^3-和八面体MnO₄(H₂O)₂所构成．突出的结构特点是,化合物结构中的氨离子位于螺纹的外侧并与周围的氧原子形成较强的氢键．实验结果表明,顺磁性的标题化合物在较低的温度下表现出微弱的反铁磁性（Ө = -7.3 K）．此外,化合物的IR、元素分析和热分析在文中也被讨论．     

一个新的夹心型杂多钨酸盐Na6(C5N2H7){[Na(H2O)2]3Co(H2O)5-[Co(H2O)]3(AsW9O33)2}•27H2O的晶体结构及性质

在pH＝7.5的水溶液中, Na₂WO₄•2H₂O, NaAsO₂, CoCl₂•6H₂O与对氨基吡啶反应, 得到了一种新的夹心型杂多钨酸盐Na₆(C₅H₇N₂){[Na(H₂O)₂]₃Co(H₂O)₅[Co(H₂O)]₃(AsW₉O₃₃)₂}•27H₂O单晶, 用X射线单晶衍射法及元素分析确定了其结构, 晶体属三斜晶系, P 空间群, 其晶胞参数为: a＝1.3276(8) nm, b＝1.7581(10) nm, c＝2.4381(14) nm, α＝70.954(9)°, β＝86.663(9)°, γ＝72.885(9)°, V＝5.136(5) nm³, Z＝2, R₁＝0.0608, wR₂＝0.0848 [I＞2σ(I)]. 在{[Na(H₂O)₂]₃Co(H₂O)₅[Co(H₂O)]₃(AsW₉O₃₃)₂}^7－阴离子中, 一个Co^2＋与聚阴离子{[Na(H₂O)₂]₃[Co(H₂O)]₃(AsW₉O₃₃)₂}^9－的一个端基氧共价连接, Co^2＋呈现出5和6两种配位数, 质子化的氨基吡啶正离子作为抗衡离子存在于晶体之中. 对标题化合物进行了IR, UV-Vis, TG-DSC表征. 对该化合物、Na₂WO₄•2H₂O及CoCl₂•6H₂O催化H₂O₂氧化乙醛的活性进行了比较研究, 该化合物的催化活性远优于简单化合物Na₂WO₄•2H₂O和CoCl₂•6H₂O.     

一个新的夹心型杂多钨酸盐Na6(C5N2H7){[Na(H2O)2]3Co(H2O)5-[Co(H2O)]3(AsW9O33)2}•27H2O的晶体结构及性质

在pH＝7.5的水溶液中, Na₂WO₄•2H₂O, NaAsO₂, CoCl₂•6H₂O与对氨基吡啶反应, 得到了一种新的夹心型杂多钨酸盐Na₆(C₅H₇N₂){[Na(H₂O)₂]₃Co(H₂O)₅[Co(H₂O)]₃(AsW₉O₃₃)₂}•27H₂O单晶, 用X射线单晶衍射法及元素分析确定了其结构, 晶体属三斜晶系, P 空间群, 其晶胞参数为: a＝1.3276(8) nm, b＝1.7581(10) nm, c＝2.4381(14) nm, α＝70.954(9)°, β＝86.663(9)°, γ＝72.885(9)°, V＝5.136(5) nm³, Z＝2, R₁＝0.0608, wR₂＝0.0848 [I＞2σ(I)]. 在{[Na(H₂O)₂]₃Co(H₂O)₅[Co(H₂O)]₃(AsW₉O₃₃)₂}^7－阴离子中, 一个Co^2＋与聚阴离子{[Na(H₂O)₂]₃[Co(H₂O)]₃(AsW₉O₃₃)₂}^9－的一个端基氧共价连接, Co^2＋呈现出5和6两种配位数, 质子化的氨基吡啶正离子作为抗衡离子存在于晶体之中. 对标题化合物进行了IR, UV-Vis, TG-DSC表征. 对该化合物、Na₂WO₄•2H₂O及CoCl₂•6H₂O催化H₂O₂氧化乙醛的活性进行了比较研究, 该化合物的催化活性远优于简单化合物Na₂WO₄•2H₂O和CoCl₂•6H₂O.     

新型水合稀土多硼酸盐Ln[B5O8(OH)2](Ln=Pr，Nd)的合成与结构

采用熔融硼酸法在200 ℃下合成了一种具有层状结构的新型水合稀土多硼酸盐，Ln[B₅O₈(OH)₂](Ln=Pr，Nd)，并利用粉末X射线衍射技术确定了它的结构。Ln[B₅O₈(OH)₂]晶体属于单斜晶系、P2₁/c空间群，它的基本构建单元(FBB)是由3个BO₄和2个BO₃组成的双三元环，[B₅O₁₂](2Δ+3T)。每一个FBB和邻近的4个FBB通过共用氧原子相连，形成了具有九元环窗口的层状硼酸根基团，稀土离子位于九元环中心附近。CSD：391317。     

配合物[Cu2(C4H2O6)(Phen)2(H2O)]·8H2O的合成、晶体结构和抗菌活性

在pH≈10的乙醇-水溶液中以硫酸铜、酒石酸和邻菲咯啉反应合成了分子式为[Cu₂(C₄H₂O₆)(Phen)₂(H₂O)]·8H₂O的配合物单晶。用X-射线单晶衍射测定了晶体结构，并研究了配合物对大肠杆菌、金黄色葡萄球菌、枯草杆菌的抗菌活性。晶体属单斜晶系，空间群P2₁。标题化合物为双核铜配合物，2个铜原子配位数不同。Cu(1)是五配位的，具有扭曲的四方锥结构，5个配位原子分别是酒石酸的去质子的羟基氧和羧基氧、邻菲咯啉的2个氮原子及1个水分子的氧原子。Cu(2)为四配位的，配位原子分别是酒石酸的去质子的羟基氧和羧基氧和邻菲咯啉的2个氮原子。分子中Cu(1)…Cu(2)间的距离为0.354 8 nm。存在分子内邻菲咯啉-邻菲咯啉的面—面π-π相互作用，面间距为0.381 3 nm。配合物对大肠杆菌、金黄色葡萄球菌、枯草杆菌具有较强的抗菌活性。     

B2O3/TiO2-ZrO2的结构表征及其与酸性和催化性能间的关系

采用XRD、N₂吸附、 ¹¹B MAS NMR、NH₃-TPD和催化性能评价等方法研究了B₂O₃/TiO₂-ZrO₂催化剂的结构、酸性及催化环己酮肟气相Beckmann重排反应性能间的关系。结果表明,催化剂中的B₂O₃同时以三配位的BO₃和四配位的BO₄结构单元存在;     

A new route to prepare the mixed oxo-ethylidyne-capped trinuclear tungsten(IV) cluster and the crystal structure of H2Na3[W3O(CCH3)-(O2CCH3)6(H2O)3][H2W12O40]·13.5H2O

The synthesis and the structural characterization of the title compound H₂Na₃[W₃O(CCH₃)-(O₂CCH₃)₆(H₂O)₃][H₂W₁₂O₄₀]·13.5H₂O are described. It is known that the mixed oxo-ethylidynecapped tritungsten cluster can be obtained by Zn dust reduction of Na₂WO₄·2H₂O in acetic anhydride. The title compound has been characterized by X-ray diffraction, UV/VIS and ¹H NMR spectra. The tungsten atoms in the cluster cation and anion are in the oxidation states of W(IV) and W(VI) respectively. The crystal is rhombohedral with the space group R32, a = 17.058 (3)Å, c = 49.665 (9)Å, γ=120°, V=12516(9)ų, Z=6, final R = 0.037 for 2071 reflections with I ≥3σ (I). Both the cluster cation and anion have a C₃ symmetry. The important interatomic distances in angstroms for the cluster cation are: W—W, 2.730(2); W—μ₃?O, 2.00; W—O (carboxy1), 2.12; W—O_t 2.18 (2).     

一个新颖的由Zn配合物修饰的Keggin型钴钨酸盐：[Zn(2,2’-bipy)3]3{[Zn(2,2’-bipy)2(H2O)]2 [HCoW12O40] 2 }.H2O

通过水热合成技术,一个新颖的基于Zn配合物修饰的Keggin型钴钨酸的有机-无机杂化化合物：[Zn(2,2’-bipy)3]3{[Zn(2,2’-bipy)2(H2O)]2 [HCoW12O40] 2 }.H2O已经被合成,化合物通过红外光谱、热重分析和单晶X-射线衍射进行了表征。单晶X-射线衍射的结果显示标题化合物是由一个单支撑的{[Zn(2,2’-bipy)2(H2O)]2 [HCoW12O40] 2}6-多阴离子,三个[Zn(2,2’-bipy)3]2+阳离子和一个水分子构成。有趣的是[Zn(1)(2,2’-bipy)3]2+阳离子通过氢键连接在一起形成螺旋链。另外标题化合物在空气中是稳定的,并且在室温下显示了强的荧光。     

Crystal Structure, Thermal Analysis and Theoretical Calculation of a One-dimensional Chain Complex [Zn（dafo）2（H2O）2]（NO3）2

Introduction Molecular recognition and molecular self-assemblycarried out by cooperation of the weak interactions(electrostatic reaction, hydrogen bonds, van der Waalsforce, short-range repulsive force, etc) are the commonphenomena in nature. In recent years, the research onsupramolecular complex has been a crossing focus ofseveral subjects such as chemistry, physics, biology,material and information.1 Supramolecular complex hasa wide application foreground in material, catalysis,conductor,…     

Kristallstruktur von Natrium‐Dihydrogencyamelurat‐Tetrahydrat Na[H2(C6N7)O3] · 4 H2O

Crystal Structure of Sodium Dihydrogencyamelurate Tetrahydrate Na[H₂(C₆N₇)O₃] · 4 H₂O Sodium dihydrogencyamelurate‐tetrahydrate Na[H₂(C₆N₇)O₃]·4 H₂O was obtained by neutralisation of an aqueous solution, previously prepared by hydrolysis of the polymer melon with sodium hydroxide. The crystal structure was solved by single‐crystal X‐ray diffraction ( a = 6.6345(13), b = 8.7107(17), c = 11.632(2) Å, α = 68.96(3), β = 87.57(3), γ = 68.24(3)°, V = 579.5(2) ų, Z = 2, R1 = 0.0535, 2095 observed reflections, 230 parameters). Both hydrogen atoms of the dihydrogencyamelurate anion are directly bound to nitrogen atoms of the cyameluric nucleus, thus proving the preference of the keto‐tautomere in salts of cyameluric acid in the solid‐state. The compound forms a layer‐like structure with an extensive hydrogen bonding network.     

One‐dimensional Cadmium(II) Coordination Polymers: Syntheses and Crystal Structures of [Cd(H2O)3(C5H6O4)]·2H2O,Cd(H2O)2(C6H8O4), and Cd(H2O)2(C8H12O4)

[Cd(H₂O)₃(C₅H₆O₄)]·2H₂O ( 1 ) and Cd(H₂O)₂(C₆H₈O₄) ( 2 ) were prepared from reactions of fresh CdCO₃ precipitate with aqueous solutions of glutaric acid and adipic acid, respectively, while Cd(H₂O)₂(C₈H₁₂O₄) ( 3 ) crystallized in a filtrate obtained from the hydrothermal reaction of CdCl₂·2.5H₂O, suberic acid and H₂O. Compound 1 consists of hydrogen bonded water molecules and linear {[Cd(H₂O)₃](C₅H₆O₄)_2/2} chains, which result from the pentagonal bipyramidally coordinated Cd atoms bridged by bis‐chelating glutarato ligands. In 2 and 3 , the six‐coordinate Cd atoms are bridged by bis‐chelating adipato and suberato ligands into zigzag chains according to {[Cd(H₂O)₃](C₅H₆O₄)_2/2} and {[Cd(H₂O)₂](C₈H₁₂O₄)_2/2}, respectively. The hydrogen bonds between water and the carboxylate oxygen atoms are responsible for the supramolecular assemblies of the zigzag chains into 3D networks. Crystallographic data: ( 1 ) P1¯ (no. 2), a = 8.012(1), b = 8.160(1), c = 8.939(1) Å, α = 82.29(1)°, β = 76.69(1)°, γ = 81.68(1)°, U = 559.6(1) ų, Z = 2; ( 2 ) C2/c (no. 15), a = 16.495(1), b = 5.578(1), c = 11.073(1) Å, β = 95.48(1)°, U = 1014.2(1) ų, Z = 4; ( 3 ) P2/c (no. 13), a = 9.407(2), b = 5.491(1), c = 11.317(2) Å, β = 95.93(3)°, U = 581.4(2) ų, Z = 2.     

Synthesis and Crystal Structure of a Novel Supramolecular Compound [Mg(H_2O)_6](C_(16)H_(11)O_4SO_3)_2·10H_2O

IntroductionMolecularpolymerwithonedimensionalormultidimen sionalstructureassemblingthroughhydrogenbondsisanim portantresearchcontentinthesupramolecularchemistryandcrystalenginnering .1,2 Withthedevelopmentofnewtypefunctionalmaterialssuchasmolecularmagnetic ,selectedcatalysis ,reversiblecatalysis ,reversiblehost guestmolecular(ion)exchangeetc.,3themoleculardesignandsynthesishavealreadyattractedconsiderableattentioninsupramolecu larsystem .Thesupramolecularcomplexesandorganiccom poundscontainin…     

Synthesis and structural investigation of a new cadmium cyclohexaphosphate Cd[3,4-(CH3)2C6H5NH3]4P6O18·6H2O

Single crystals of a new cyclohexaphosphate, are synthesised and investigated by X-ray diffraction. This compound crystallizes in the triclinic system with the space group P-1 and cell parameters a=7.773(4), b=9.238(3), c=18.532(7) Å, α=88.57(3), β=88.10(4), γ=67.35(4)°, Z=1 and V=1227(1) ų. The three-dimensional network is built up from parallel (0 0 1) layers of [CdP₆O₁₈(H₂O)₆]⁴⁻ between which the organic molecules are inserted. The Cd atoms, in 1(a) sites, adopt an octahedral coordination. The 3,4-xylidinium cations exercise an electrostatic interaction on the inorganic anion and establish strong H-bonds with their oxygen atoms.     

Synthesis,Crystal Structure and Characterization of a new Protonated Magnesium Borophosphate: (H3O)Mg(H2O)2[BP2O8]·H2O

A new protonated borophosphate (H₃O)Mg(H₂O)₂[BP₂O₈]·H₂O ( 1 ) was synthesized under mild hydrothermal conditions and characterized by single‐crystal X‐ray diffraction, FTIR spectroscopy and TG‐DTA. The compound crystallizes in the hexagonal system, space group P6(1)22 (No 178), a = 9.4462(7) Å, c = 15.759(2) Å, V = 1217.8(2) Å³, and Z = 6. There exist infinite helical $^1_\infty$ {[BP₂O₈]^3–} ribbons built up from corner‐sharing PO₄ and BO₄ tetrahedra, which are connected by MgO₄(H₂O)₂ leading to an infinite three‐dimensional open‐framework. The H₃O⁺ ions are located at the free thread of the helical ribbons, whereas crystallized water occupy the channels of the helical ribbons. The dehydration of the compound occurs at a higher temperature which is presumably due to the anisotropic hydrogen bonds in the crystal structure. The luminescent properties of the compound were studied.     

Assembly of a New Cyano‐bridged 4f‐3d Dimer Sm(DMSO)4‐ (H2O)3Cr(CN)6 and Crystal Structure of [K3(18‐crown‐6)3‐(H2O)4]Cr(CN)6·3H2O

A new cyano‐bridged binuclear 4f‐3d complex Sm(DMSO)₄‐(H₂O)₃Cr(CN)₆ was synthesized and characterized by single crystal structure analysis. It crystallizes in monoclinic, space group P2₁ with a=0.9367(2) nm, b = 1.3917(3) nm, c = 1.1212(2) run, β = 99.88(3)° and Z = 2. In this binuclear complex, Sm atom is eight coordinated and linked to the Cr atom by a cyano bridge. The molecules packs to form 3D structure due to the hydrogen bonds among them. [K₃(18‐C‐6)₃(H₂O)₄]Cr(CN)₆·3H₂O (18‐C‐6 represents 18‐crown‐6‐ether) that was synthesized as a byproduct in the preparation of a Gd—Cr complex is also structurally characterized. Crystal data: triclinic, space group P‐l with a = 1.0496(7) nm, b= 1.1567(14) nm, c = 1.3530(13) nm, a = 94.15(9)°, β = 96.04(8)°, γ = 95.25(9)° and Z = l. [K₃(18‐C‐6)₃(H₂O)₄]‐Cr(CN)₆·3H₂O consists of ionic [K₃(18‐C‐6)₃(H₂O)₄]³⁺ and [Cr(CN)₆]^3‐ pairs, of which the [K₃(18‐C‐6)₃(H₂O)₄]³⁺ ion is a trinuclear duster connected by water, and K atoms are eight coordinated by eight oxygen atoms of one 18‐C‐6 and two water molecules.     

The Cocrystallization of the Cubic [Ta6Br12(H2O)6][CuBr2X2]·10H2O and Triclinic [Ta6Br12(H2O)6]X2·trans‐[Ta6Br12(OH)4(H2O)2]·18H2O (X = Cl,Br, NO3) Phases with the Coexistence of [Ta6Br12]2+ and [Ta6Br12]4+ in the Latter

Cubic [Ta₆Br₁₂(H₂O)₆][CuBr₂X₂]·10H₂O and triclinic [Ta₆Br₁₂(H₂O)₆]X₂·trans‐[Ta₆Br₁₂(OH)₄(H₂O)₂]·18H₂O (X = Cl, Br, NO₃) cocrystallize in aqueous solutions of [Ta₆Br₁₂]²⁺ in the presence of Cu²⁺ ions. The crystal structures of [Ta₆Br₁₂(H₂O)₆]Cl₂·trans‐[Ta₆Br₁₂(OH)₄(H₂O)₂]·18H₂O ( 1 ) and [Ta₆Br₁₂(H₂O)₆]Br₂·trans‐[Ta₆Br₁₂(OH)₄(H₂O)₂]·18H₂O ( 3 )have been solved in the triclinic space group P&1macr; (No. 2). Crystal data: 1 , a = 9.3264(2) Å, b = 9.8272(2) Å, c = 19.0158(4) Å, α = 80.931(1)?, β = 81.772(2)?, γ = 80.691(1)?; 3 , a = 9.3399(2) Å, b = 9.8796(2) Å, c = 19.0494(4) Å; α = 81.037(1)?, β = 81.808(1)?, γ = 80.736(1)?. 1 and 3 consist of two octahedral differently charged cluster entities, [Ta₆Br₁₂]²⁺ in the [Ta₆Br₁₂(H₂O)₆]²⁺ cation and [Ta₆Br₁₂]⁴⁺ in trans‐[Ta₆Br₁₂(OH)₄(H₂O)₂]. Average bond distances in the [Ta₆Br₁₂(H₂O)₆]²⁺ cations: 1 , Ta‐Ta, 2.9243 Å; Ta‐Brⁱ , 2.607 Å; Ta‐O, 2.23 Å; 3 , Ta‐Ta, 2.9162 Å; Ta‐Brⁱ , 2.603 Å; Ta‐O, 2.24 Å. Average bond distances in trans‐[Ta₆‐Br₁₂(OH)₄(H₂O)₂]: 1 , Ta‐Ta, 3.0133 Å; Ta‐Brⁱ, 2.586 Å; Ta‐O(OH), 2.14 Å; Ta‐O(H₂O), 2.258(9) Å; 3 , Ta‐Ta, 3.0113 Å; Ta‐Brⁱ, 2.580 Å; Ta‐O(OH), 2.11 Å; Ta‐O(H₂O), 2.23(1) Å. The crystal packing results in short O···O contacts along the c axes. Under the same experimental conditions, [Ta₆Cl₁₂]²⁺ oxidized to [Ta₆Cl₁₂]⁴⁺ , whereas [Nb₆X₁₂]²⁺ clusters were not affected by the Cu²⁺ ion.