一种新颖的二维4f-3d-5d多金属-异烟酸配合物的合成、晶体结构和磁性研究

通过水热方法合成了一种新颖的异金属金属-异烟酸无机-有机杂化体[Zn0.5(H2O)]{(Hg2Cl5)[Er(C6NO2H4)3(H2O)2]}(HgCl2)·0.5CH3OH·0.5H2O (1)并对其进行了单晶X-射线衍射结构表征。该化合物是首例4f-3d-5d多金属-异烟酸配合物。化合物1属于单斜晶系C2/c空间群,每个单胞中有8个分子,晶体学参数为：a = 34.165(4) Å,b = 9.4692(8) Å,c = 24.575(3) Å,β = 115.090(5)°,V = 7200(1) Å3,C18.50H21Cl7ErHg3N3O10Zn0.50,Mr = 1495.25,Dc = 2.759 g/cm3,T = 293(2) K,μ(MoKα) = 15.954 mm-1,F(000) = 5400, R1/wR2 = 0.0561/0.0909,共有6468个独立衍射点,其中[I > 2σ(I)]的有3157个。该化合物具有新颖的二维{(Hg2Cl5)[Er(C6NO2H4)3(H2O)2]}层状结构,由Hg2Cl5–连接[Er(C6NO2H4)3(H2O)2]链形成。该二维层和氯化汞及结晶水之间通过氢键形成三维结构,甲醇分子和水合锌离子位于该三维结构的空隙中。对化合物1的磁性测试显示该化合物具有反铁磁作用。     

镍配合物[Ni（phen）：（tovsb）]·4H2O的合成与晶体结构

以牛磺酸、邻香草醛为原料,合成了配体牛磺酸缩邻香草醛席夫碱,再用所得配体与醋酸镍、邻菲啰啉作用,合成了配合物[Ni（phen）2（tovsb）]·4H2O（phen=邻菲啰啉,tovsb=牛磺酸缩邻香草醛席夫碱）,其结构通过IR,元素分析和x-射线单晶衍射法测定。标题配合物属三斜晶系,PI空间群;α=1．04661（16）,b=1．2303（2）,c=1．4063（2）nm,α=83．714（4）,β=88．539（3）,γ=69．398（3）°,V=1．6947（5）nm^3,Z=2。结构分析表明,两个邻菲哕啉共提供四个配位原子,牛磺酸缩邻香草醛席夫碱提供两个配位原子,中心Ni（Ⅱ）离子是一个六配位的畸变八面体结构。该聚合物中含有四个结晶水分子,水分子通过氢键作用,形成了一个六聚水簇。配合物分子通过氢键和π-π堆积作用形成三维超分子结构。     

镍配合物[Ni(C_(10)H_8N_2)(C_7H_4O_5N_3)(H_2O)]·ClO_4的合成及晶体结构

含C=N结构的过渡金属配合物具有抗肿瘤、抗细菌、抗癌等多种生物活性[1].亚胺金属配合物大多具有优异的光电性能和功能性,而且可以通过扩充配合物中心离子的种类、调整自由配体的结构及取代基效应、立体效应和溶剂效应等使其具有结构多样性和性质可调变性,是合成大环配合物、自组装分子及分子器件的重要原料,日益受到物理、化学和材料科学家的关注[2-11].     

钴配合物[Co_2(H_2O)_8(C_(10)H_8N_2)_2]·(HO_3PCH_2CH_2SO_3)(SO_4)(H_2O)_4的合成与晶体结构研究

用硫酸钴、4,4'-联吡啶和2-磺酸基乙基膦酸合成了一个新颖的钴化合物:[Co_2(H_2O)_8(C_(10)H_8N_2)_2]·(HO_3PCH_2CH_2SO_3)(SO_4)(H_2O)_4,并对其进行了红外.元素分析、热重测试,通过单晶衍射仪测定了其晶体结构.结果表明,配合物属单斜晶系C2/c空间群,分子式为C_(22)H_(45)Co_2N_4O_(22)PS_2,分子量为930.57,晶胞参数为a=19.8456(18),b=11.2957(10),c=34.719(3)(A),β=106.095(3)°,晶胞体积为7477.9(12)(A)~3,Z=8,Dc=1.653 g/cm~3,F(000)=3856,μ=1.131 mm~(-1),最终残差因子R_1=0.0726,wR_2= 0.1719(相对于5612个I>2σ(I)的可观测衍射点).在这个化合物中,二齿配体4,4'-联吡啶把Co(II)桥连成[Co(4,4'-bipy)]~(2+)链.化合物中的[Co(4,4'-bipy)]~(2+)链有三个不同的朝向.2-磺酸基乙基膦酸没有参与配位而是做为一个有机模板剂填充在[Co(4,4'-bipy)]~(2+)链形成的空隙中.     

CoNi_2S_4 Microspheres Prepared by One-pot Hydrothermal Reaction as Supercapacitor

A microsphere discrete structure of CoNi_2S_4 was prepared through one-pot hydrothermal reaction and characterized by FTIR, XRD and SEM. The as-prepared CoNi_2S_4 served as a supercapacitor, showing a specific capacitance of 1129.5 F/g with over 99% coulombic efficiency at a current density of 4 A/g in 3 M KOH. And after 3000 cycles of charge and discharge tests, 92.3% of its initial capacitance can be still maintained. The results demonstrate that the material is promising as an electrode material for supercapacitors in energy storage.     

琥珀酸构建具有超级电容器性能的混合金属有机骨架

采用简单的溶剂热法合成了混合金属有机骨架材料（MOF （Ni,Co））,然后通过X射线衍射、FT-IR、扫描电子显微镜、X射线光电子能谱和N₂吸附-脱附对制备的材料进行了表征,并进一步研究了其作为超级电容器电极材料的性能。结果表明,具有独特的纳米花状结构的MOF （Ni_1.2Co_0.8）可以提供更多的电活性位点,从而具有优异的电化学性能,在1 A·g^-1时的比电容为850 F·g^-1。同时本研究工作说明MOF （Ni）电极材料在掺杂适量钴元素后,可增强电极内部电子/离子转移,降低活性物质和电解液之间的接触电阻,提高导电性,增强电化学性能。     

Syntheses and Crystal Structures of Two New Metal Phosphonates:[Mn(H_2O)_2(C_(12)H_8N_2)(HO_3PCH_2CH_2CO_2)] and [Co(H_2O)_4(C_(10)H_8N_2)]·(HO_3PCH_2CH_2CO_2)

By the reactions of manganese(II) acetate, 2-sulfoethylphosphonic acid, 1,10-phen (1,10-phen = 1, 10-phenanthroline) or cobalt(II) acetate, 4,4'-bipy and 2-carboxyethylphosphonic acid, two novel compounds of [Mn(H2O)2(C12H8N2)(HO3PCH2CH2CO2)] (1) and[Co(H2O)4 (C10H8N2)]· (HO3PCH2CH2CO2) (2) have been synthesized and characterized by IR spectroscopy, elemental analyses and single-crystal X-ray diffraction. Compound 1 has a 0D structure. Two Mn(II) ions are linked by two 2-carboxyethylphosphonic acid ligands, forming a centrosymmetric dimer. These dimers are further interlinked into a 2D layer structure by π-π stacking interactions and hydrogen bonds. Compound 2 has a 1D chain structure. The 2-carbo- xyethylphosphonic acid remains uncoor- dinated and acts as the organic template. By the bridge of 4,4'-bipy, the [Co(4,4'-bipy)]2+ chains are formed.     

镍配合物[Ni(phen)_2(tovsb)]·4H_2O的合成与晶体结构(英文)

以牛磺酸、邻香草醛为原料,合成了配体牛磺酸缩邻香草醛席夫碱,再用所得配体与醋酸镍、邻菲啰啉作用,合成了配合物 [Ni(phen)2(tovsb)]·4H2O(phen=邻菲啰啉,tovsb=牛磺酸缩邻香草醛席夫碱),其结构通过IR,元素分析和X-射线单晶衍射法测定.标题配合物属三斜晶系,Pī空间群;a=1.04661(16),b=1.2303(2),c=1.4063(2) nm,α=83.714(4),β=88.539(3),γ=69.398(3)°,V=1.6947(5)nm3,Z=2.结构分析表明,两个邻菲啰啉共提供四个配位原子,牛磺酸缩邻香草醛席夫碱提供两个配位原子,中心Ni(II)离子是一个六配位的畸变八面体结构.该聚合物中含有四个结晶水分子,水分子通过氢键作用,形成了一个六聚水簇,配合物分子通过氢键和π-π堆积作用形成三维超分子结构.     

牛磺酸缩5-溴水杨醛席夫碱合镍(II)配合物的合成及晶体结构

The reaction of Ni(Ac)₂, Taurine, 5-bromo-salicylaldehyde afford a complex, [Ni(C₉H₈BrNO₄S)(H₂O)₃]·H₂O. Its structure has been determined by single crystal X-ray diffraction. It crystallizes in monoclinic, P2₁/c, a=1.479 98(6) nm, b=1.397 97(6) nm, c=0.746 60(3) nm, β=99.364(2)°, V=1.524 11(11) nm³. Nickel(II) coordinated with six atoms, forming a octahedron. These octahedrons are further interlinked by the hydrogen bonds. CCDC: 639681.     

Synthesis and Crystal Structure of a Novel Layered Lead（Ⅱ） Carboxylate-sulfonate Compound Templated by 4,4＇-Bipyridine

A new lead(Ⅱ) carboxylate-sulfonate has been hydrothermally synthesized and characterized by X-ray single-crystal and elemental analyses. It crystallizes in triclinic, space group P, with a = 8.1573(6), b = 9.4663(7), c = 12.7488(9) , α = 89.2320(10), β = 80.7380(10), γ = 77.9760(10)°, Z = 2, V = 950.10(12) 3, Mr = 599.57, Dc = 2.096 g/cm3, μ = 9.032 mm-1, F(000) = 572, the final R = 0.0412 and wR = 0.1035. It has a 1D chain structure, and the Pb(Ⅱ) is six-coordinated. Two PbO6 polyhedra are interconnected via edge-sharing into a two-core unit. Such units are further interconnected by 3-sulfonato-benzoic acids into 1D chains which are linked by hydrogen bonds into a layer structure. The 4,4'-bipyridines are located at the interlayer space and link the layers into a supramolecular structure by π-π stacking interactions.