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Two Cobalt(II) Complexes Derived from the Hydrolysis Product of Di-Schiff Base Ligand N,N'-Bis-(1-benzimidazo-2-yl-ethylidene)-ethane-1,2-diamine:Preparation,Characterization and Crystal structure of the 6-Coordinate Species [CoL_2]X·H_2O (X = ClO_4^-, N

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Chinese Journal of Structural Chemistry 2008年第7期27卷 805-811页

作者：夏昌坤吴小园吴鼎铭蒋晓瑜卢灿忠 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

The reactions of Co（C1O4）2·6H2O and Co（NO3）2.6H2O with the di-Schiff base ligand N,N＇-bis-（1-benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine （LA） in ethanol have been investigated. The reactions of LA with excess amount of cobalt salts yield the six-coordinate complexes [CoL2]（ClO4）E·H2O 1 and [CoL2]（NO3）E·H2O 2 as isolatable products （L= N-（1- benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine）, where L is a tri-dentate mono-Schiff base ligand, resulting from the hydrolysis of the precursor di-Schiff base LA. Both complexes were characterized by X-ray crystallography. Crystal data for complex 1： monoclinic, space group P21/c, a = 11.9214（10）, b = 23.5828（17）, c = 14.0387（12）A, β = 135.219（4）°, C22H30Cl2CoN8O9, Mr = 680.37, V = 2780.1（4） A^3 ,Z = 4, Dc = 1.625 g/cm^3,μ（MoKa） = 0.876 mm^-1, F（000） = 1404, the final R = 0.0725 and wR = 0.1530 for 5726 observed reflections （I 〉 2σ（I））. Crystal data for complex 2： monoclinic, space group P21/c, a = 18.2162（16）, b = 10.0610（6）, c = 18.593（2）A, β = 130.099（3）°, C22H30CoN10O7, Mr = 605.49, V = 2606.5（4） A3 Z = 4, Dc = 1.543 g/cm^3,μ（MoKa） = 0.722 mm^-1, F（000） = 1260, the final R = 0.0619 and wR = 0.1429 for 5194 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that each cobalt atom in the two complexes is chelated by six nitrogen atoms from two tridentate iigands L, exhibiting a slightly distorted octahedral coordination sphere. In both complexes, the strong hydrogen-bonding interactions between the lattice waters and N-H groups of the ligands result in 1D chains which are further connected by ClO4^- （or NO3^-） groups to form a 3D framework. In complex 2, the strong π-π interactions increase the stability of the structure.

关键词： 2-acetylbenzimidazole di-Schiff base ligand crystal structure hydrolysis hydrogen-bonding interactions coordination complex N,N -bis-(1-benzimidazo-2-yl-ethylidene)-ethane- 1,2-diamine N-(1-benzimidazo-2-yl-ethylidene)-ethane- 1,2-diamine

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Solvothermal Synthesis and Characterization of HgTe Nanoplatelets Using Mercury(I) Source

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Chinese Journal of Structural Chemistry 2008年第4期27卷 461-466页

作者：吴科俊王明盛邹建平徐刚丁同勇郭国聪黄锦顺 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

Mercury telluride （HgTe） nanoplatelets were obtained via a facile solvothermal reaction of mercury（I） chloride and tellurium powder in ethylenediamine （en）. Mercury（I） was first applied as the mercury sources to prepare nanocrystal HgTe; moreover, the proposed mechanism for the fabrication of the sample was discussed in detail. The HgTe nanoplatelets were characterized by powder X-ray diffraction （PXRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, high-resolution transmission electron microscopy （HRTEM） and Fourier transform infrared spectroscopy （FT-IR）. The absence of IR absorption may render the title nanocrystal useful as an IR transparent material in the region.

关键词： crystal growth mercury telluride nanomaterials solvothermal synthesis X-ray techniques

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Syntheses and Crystal structures of Two Gd(Ⅲ) Hydrogen Supramolecules Based on p-Sulfonatothiacalix[4]arene

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Chinese Journal of Structural Chemistry 2008年第5期27卷 558-564页

作者：袁大强吴明燕江飞龙洪茂椿 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

Two novel polymeric complexes, [Gd（HsTCAS）（H2O）7]·4H2O 1 and [Gd（HsTCAS）（CH3COCH3）（H2O）6]·6H2O 2 （H4TCAS = p-sulfonatothiacalix[4]arene）, have been synthesized and characterized by single-crystal X-ray diffraction analyses. Complex 1 crystallizes in monoclinic, space group C2/m with a = 20.2308（12）, b = 19.0894（10）, c = 12.2448（7）A, β = 101.847（3）°, V = 4628.1（5）A^3, C24H43GdO27S8, Mr = 1169.25, Z = 4, Dc = 1.690 g/cm^3, F（000） = 2380,μ = 1.879 mm^-1, the final R = 0.0404 and wR = 0.1038 for 5127 observed reflections with I 〉 2σ（I）. Complex 2 is pseudo-isostructural with complex 1.

关键词： crystal structure p-sulfonatothiacalixarene gadolinium complexes hydrogen bond

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Thermal effects in a tetragonal Nd:YLF crystal laser

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Chinese Science Bulletin 1996年第20期41卷 1711-1717页

作者：沈鸿元 Fujian institute of research on the structure of matter Chinese Academy of Sciences Fuzhou 350002 China

The thermal effects in host material are an important subject for solid state laser. Recently, tetragonal Nd:YLF crystal with the space group of 41/α has received great attention. The high efficiency, 40W cw Nd:YLF laser with large TEM00 mode has been reported by Giulio Cerullo and his colleagues. But the theory of thermal effects for tetragonal crystal has not been reported so far. For the first time, the calculated results of thermal effects during the lamp-pumped process for an α-axis Nd:YLF rod have been achieved in this note.

关键词： thermal effects tetragonal Nd:YLF crystal.

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Is Water Physisorption Reversible for TiO_2 Nanocrystals? A Combinational Spectral Study

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Chinese Journal of Structural Chemistry 2011年第4期30卷 550-562页

作者：郑菁关翔锋李莉萍 Key Laboratory of Optoelectronic Materials Chemistry and Physics Fujian Institute of Research on the Structure of MatterChinese Academy of Sciences State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterChinese Academy of Sciences

In this work,the nature of physisorbed water and its impacts on the structure,surface chemistry,and proton conduction properties of TiO2 nanocrystals were investigated by a combinational spectral *** TiO2 nanocrystals were directly prepared by a hydrothermal method,which showed highly hydrated and sulfated *** surface water molecules were indicated to exist in a wide set of energetically nonequivalent surface hydration groups,leading to the removal of physisorbed and chemisorbed water in sequence with increasing *** heating treatment at 100 ℃ in air,physisorbed water layers were recovered with no significant impacts on the TiO2 *** the other hand,when treated at the same temperature in vacuum,the recovery of physisorbed water layers was partially reversible,while a new hydration state appeared due to the filling of the high-energy adsorption sites by water molecules,which led to a significant increase in the amount of water molecules for surface hydration and an accelerated dehydration process toward lower *** a result,an abnormal increase was observed in proton *** observations were explained in terms of thermally induced changes of surface chemistry and the amount of hydrated *** results reported in this work are important,which may help understand the roles that the physisorbed water plays in stabilizing the nanostructures and therefore could have a broad class of implications.

关键词： TiO2 nanocrystal hydrated and sulfated surfaces vacuum proton conductivity

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Saucer-and Rod-like WO_3 3-D Microstructures:Synthesis,Characterization,and Optical Properties

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Chinese Journal of Structural Chemistry 2011年第10期30卷 1428-1436页

作者：陈林颜廷江郑菁李莉萍 Key Laboratory of Optoelectronic Materials Chemistry and Physics Fujian Institute of Research on the Structure of MatterChinese Academy of Sciences State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterChinese Academy of Sciences

Three-dimensional（3-D）saucer-and rod-like WO3 microstructures have been synthesized by a simple hydrothermal route using tartaric acid as the assistant agent.X-ray powder diffraction（XRD）patterns indicate that the as-prepared samples are the pure hexagonal phase *** morphologies are characterized by scanning electron microscope（SEM）and are found to be highly sensitized to the reaction temperature.A probable formation mechanism of the WO3 microstructures from saucer-like at low temperatures to rod-like at high temperatures is *** optical properties of the novel WO3 microstructures are studied by UV-vis diffuse reflectance spectroscopy（DRS）.The mechanism of strong absorption at visible region and red shift of calcined sample is also discussed.

关键词： hydrothermal three-dimensional adsorbed water electronic structure

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Robust 3D network architectures of MnO nanoparticles bridged by ultrathin graphitic carbon for high-performance lithium-ion battery anodes

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Nano research 2018年第2期11卷 1135-1145页

作者： Jingchun Jia Xiang Hu Zhenhai Wen Key Laboratory of Design and Assembly of Functional Nanostructures Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou China Fujian Provincial Key Laboratory of Nanomaterials Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou China

A strategy was developed to fabricate a set of MnO@C nanohybrids with MnO nanopartides （NPs） embedded in an ultrathin three-dimensional （3D） carbon framework for use as anode materials for lithium-ion batteries （LIBs）. The 3D carbon frameworks provide MnO NPs with electrical pathways and mechanical robustness, which efficiently improved the reaction kinetics, prevented the MnO from fracturing and agglomerating, and limited the formation of a solid electrolyte interface （SEI） at the MnO-electrolyte interface. Benefitting from the unique 3D framework structure, the MnO/C nanohybrids carbonized at 500 ℃ exhibited a highly reversible specific capacity of 1,420 mAh.g-1 at 0.2 A.g-1, excellent cycling stability with 98% capacity retention, and enhanced rate performance of 680 mAh-g-1 at 2 A.g-L The feasibility of the large-scale production of such MnO/C nanohybrids, associated with their outstanding Li-ion storage properties, opens a promising avenue for the development of high-performance anodes for next- generation LIBs.

关键词： network architectures ultrathin carbon MnO Li-ion batter anode

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Synthesis and Structural Characterization of Gd(Ⅱ ) Coordination Polymer [Gd_2(μ-phth)_3(b-pd)(H_2O)_5]_n

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Chinese Journal of Structural Chemistry 2006年第4期25卷 453-458页

作者：黄美华刘平王艰陈云刘政 Fujian institute of research on the structure of matter The Chinese Academy of SciencesFuzhou Fujian 350002 China Graduate School of the Chinese Academy of Sciences Beijing 100039 China Fujian institute of research on the structure of matter The Chinese Academy of SciencesFuzhou Fujian 350002 China

A new Gd（Ⅱ） complex [Gd2（μ-phth）3（b-pd）（H2O）5], （phth = o-phthalato, b-pd = N,Nbipyridine） has been ＇synthesized by the reaction of GdO2 with o-phthalate, H2O and 2,2＇-bipyridine. The crystal structure has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1^- with a = 11.82920（10）, b = 13.53550（10）, c = 13.7381（2）A^°, α= 88.99,β= 66.9120（10）, γ = 66.2370（10）°, V = 1826.02（3） ,A^°3, Dc= 1.915 g/cm^3, C34H30N2O17Gd2, Mr= 1053.10, F（000） = 1024,μ = 3.680 mm^-1, Z = 2, R = 0.0612 and wR = 0.1320 for 6259 observed reflections （I〉 2σ（I））. In the title complex, the Gd（Ⅱ） ions are bridged by o-phthalate ligands in a bidentate mode, producing a 1D infinite chain structure. Each eight-coordinated Gd（Ⅱ） center is coordinated by eight oxygen atoms from phth to give a distorted dodecahedral geometry, and each nine-coordinated Gd（Ⅱ） center is coordinated by two N atoms from b-pd and seven oxygen atoms from phth to give a distorted geometry of capped square antiprism. The chains are linked by π-π interactions and hydrogen bonds between oxygen atoms of carboxylate groups and H2O molecules and hydrogen atoms of H2O, b-pd and o-phth molecules, forming an unusual three-dimensional coordination polymer.

关键词： Gd(Ⅱ) complex o-phthalate complex 2,2'-bipyridine complex,π-π interactions hydrogen bonds

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Synthesis and Crystal structure of a 1D Alternate Chain Polymer [Zn_2(NBA)_2(4,4'-bipy)]_n

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Chinese Journal of Structural Chemistry 2008年第9期27卷 1093-1096页

作者：王克伟尹培秀沈艺程李兆基覃业燕姚元根 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterThe Chinese Academy of Sciences

A one-dimensional zinc-containing coordination polymer, [Zn2（NBA）2（4,4′-bipy）]n （NBA = 3-nitrobenzoic acid, 4,4′-bipy = 4,4′-bipyrindine）, has been solvothermally synthesized and characterized by single-crystal X-ray diffraction, IR and elemental analysis. The crystal structure is of monoclinic, space group C2/c with a = 24.6478（2）, b = 14.0964（3）, c = 11.4275（2）A, β=108.7870（10）°, V = 3758.89（11） ,A^3, C38H20N6O16Zn2, Mr = 947.34, Z = 4, De = 1.674 g/cm^3 μ= 1.363 mml, F（000） = 1912, R = 0.0720 and wR = 0.2277 for 2841 observed reflections （I 〉 2σ（I）. In this compound, NBA in syn-syn coordination mode bridges zinc centers into dimericzinctetracarboxylate [Zn2（COO）4] secondary building units （SBUs） which are linked through μ-4,4′-bpy affording 1D alternating chains. These adjacent chains are further stacked through intermolecular π...π interactions to form a 3D framework.

关键词： zinc polymer NBA 4,4′-bipy 3D framework

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Synthesis and Crystal structure of [K(18-Crown-6)]_3P_(11)·2en

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Chinese Journal of Structural Chemistry 2007年第1期26卷 45-48页

作者：戴枫荣徐立 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterThe Chinese Academy of Sciences

The undecaphosphide anion in ethylenediamine/18-crown-6 solution is isolated as [K（18-crown-6）]3P11·2en 1. The crystal structure has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21 with α = 13.4731（7）, b = 16.1123（6）, c = 16.5117（9） A, β = 112.133（2）°, Y = 3320.3（3） A3, Dc = 1.371 g/cm^3, C40H88K3N4O18P11, Mr = 1371.11, F（000） = 1444,μ = 0.532 mm^-1, Z= 2, R = 0.0544 and wR = 0.1326 for 11423 observed reflections （I 〉 20（I））. The ＂naked＂ P11^3- ion is stabilized by two partly sequestered potassiums, The third partly sequestered potassium does not interact with the P atom （P（6）） but with two solvent molecules.

关键词： zintl ions phosphorus crystal structure undeeaphosphide

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