Synthesis, crystal structure and properties of [Nd(C6NO2H5)3(H2O)2]2n · (nH5O2)(nHgCl5)(2nHgCl4) · (nH2O) with unprecedented polycationic chains

A novel inorganic-organic hybrid complex, [Nd [Nd (C₆NO₂H₅)₃(H₂O)₂]_2n · (nH₅O₂)(nHgCl₅)(2nHgCl₄) · (nH₂O)(1), was obtained by hydrothermal reactions and structurally characterized by X-ray diffraction. The unit cell parameters are as follows: a = 9.579(1), b = 21.462(2), c = 15.801(1) ?, β = 102.339(6)^ℴ, V = 3173.5(5) ?³, Z = 4, space group P2₁/c. The crystal structure analysis reveals that the title complex is characteristic of a novel polycationic [Nd(C₆NO₂H₅)₃(H₂O)₂]_2n ⁶ⁿ⁺ one-dimensional chain-like structure. Photoluminescent investigation shows that the title complex displays strong emission in blue region, which is attributed to the intraligand π-π*-transition of nicotinic ligands. Optical absorption spectra of 1 reveal the presence of an optical gap of 3.45 eV. The article is published in the original.     

Synthesis and structures of Cs4[(UO2)2(C2O4)(SO4)2(NCS)2] · 4H2O and (NH4)4[(UO2)2(C2O4)(SO4)2(NCS)2] · 6H2O

Single crystals of Cs₄[(UO₂)₂(C₂O₄)(SO₄)₂(NCS)₂] · 4H₂O (I) and (NH₄)₄[(UO₂)₂(C₂O₄)(SO₄)₂(NCS)₂] · 6H₂O (II) have been synthesized and studied by X-ray diffraction. The crystals of both compounds are orthorhombic with the space group Pbam, Z = 2, and unit cell parameters a = 12.0177(3) ?, b = 18.6182(5) ?, c = 6.7573(10) ?, R = 0.0376 (I); a = 11.6539(9) ?, b = 18.3791(13) ?, c = 6.7216(5) ?, R = 0.0179 (II). The main structural units of crystals I and II are [(UO₂)₂(C₂O₄)(SO₄)₂(NCS)₂]⁴⁻ chains belonging to the crystal-chemical group A₂K⁰²B₂²M₂¹ (A = UO₂²⁺, K⁰² = C₂O₄²⁻, B² = SO₄²⁻, M¹ = NCS⁻) of the uranyl complexes. The uranium-containing chains are joined into a three-dimensional framework due to a system of electrostatic interactions with the cesium or ammonium ions in the structure of I. In the structure of II, this framework is additionally stabilized by hydrogen bonds involving the outer-sphere water molecules and ammonium ions. Original Russian Text ? I.V. Medrish, A.V. Virovets, E.V. Peresypkina, L.B. Serezhkina, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 7, pp. 1115–1120.     

RuO2·xH2O / MWNTs纳米复合物的超级电容特性研究

本文采用超声波技术合成了水合氧化钌/多壁碳纳米管纳米复合材料(Ru-MWNTs)前驱物，在150 ℃下热处理15 h后得到Ru-MWNTs。采用XRD及TEM对纳米复合材料进行表征，结果表明，水合氧化钌以无定型态比较均匀地沉积在MWNTs上。在1.0 mol·L^-1 H₂SO₄电解液中对Ru-MWNTs复合电极进行了电化学测试，循环伏安结果表明纳米复合物具有良好的电容性能，其比容量为100 F·g^-1，是MWNTs的6倍(MWNTs的比容量为15.5 F·g^-1)；本文还采用交流阻抗方法来分析频率与电容的关系，比较分析了MWNTs和复合材料的孔结构，表明在MWNTs中复合少量的水合氧化钌可以提高电极材料的充、放电速度。     

一维链状铜配位聚合物[Cu(bpb)(PPh3)2]n·nClO4·nCH2Cl2·nH2O的合成、晶体结构与荧光性质研究

A coordination polymer of [Cu(bpb)(PPh₃)₂]_n·nClO₄·nCH₂Cl₂·nH₂O(bpb=1,4-bis(pyridine-3-aminome-thyl)benzene) has been synthesized and characterized by elemental analysis, IR, TG, PL and X-ray single crystal diffraction. The title complex crystallized in triclinic with space group P1, a=1.065 8(4) nm, b=1.542 4(6) nm, c=1.690 8(6) nm, α=80.11(10)°, β=76.00(10)°, γ=82.72(10)°, and V=2.646 5(17) nm³, Z=2, R=0.068 4. In the title complex, each Cu(Ⅰ) ion displays a distorted tetrahedron coordination configuration, defined by two N atoms from two different bpb groups, and two P atoms from PPh₃. Two adjacent Cu(Ⅰ) tetrahedron units are linked into a one-dimensional chain by the bpb ligands, which are further connected by hydrogen bonds to form a two-dimensional layer structure. Furthermore, the solid-state fluorescent property of the title complex was studied at room temperature. CCDC: 743417.     

L-丙氨酸桥联配位聚合物[Cu2(L-ala)2(phen)2]n·2nClO4·2nH2O的合成及其结构

The complex, [Cu₂(L-ala)₂(phen)₂]_n·2nClO₄·2nH₂O(L-ala=L-alaninate, phen=1,10-phenanthroline) has been synthesized and investigated by elemental analysis, IR spectroscopy, and X-ray diffraction methods. The complex crystallizes in the monoclinic space group P2₁ with a=1.161 1(4) nm, b=0.717 2(2) nm, c=2.074 1(7) nm, β=101.028(6)°, V=1.695 4(9) nm³, D_c=1.760 g·cm^-3, Z=4, μ=1.493 mm^-1, F(000)=916, R=0.052 2, wR=0.127 9 for 7 131 unique reflections. The cations of [Cu₂(L-ala)₂(phen)₂]_n²ⁿ⁺ have an one-dimensional polymeric structure, due to the bridging of two Cu(phen)²⁺ units by a carboxylate group of L-alaninate, and each Cu(Ⅱ) ion is in a slightly distorted square-pyramidal coordination geometry, with the phen (N,N′) and the L-ala(N,O) acting as bidentate ligands in the equatorial plane and another carboxylate oxygen atom from a symmetry-related neighboring L-alaninate ion in the apical position. CCDC: 277541.     

Noncentrosymmetric K2Mn3(SO4)3F2·4H2O and Rb2Mn3(SO4)3F2·2H2O with pseudo-KTP structures

Two fluoride sulfates,K₂Mn₃(SO₄)₃F₂·4H₂O(Ⅰ) and Rb₂Mn₃(SO₄)₃F₂·2H₂O (Ⅱ) are obtained by water solution method.Single-crystal X-ray diffraction analysis indicated that they crystallize in space groups of Cmc2_1.Their structures feature a pseudo-KTP structure consisting of interconnecting[Mn₃(SO₄)3F₂(H₂O)2]_∞ layers,which are further packing along the a axis with alkali metal cations balancing the charges.The structure relationships between the two compounds are discussed.Secondharmonic generation measurements manifest that Ⅰ and Ⅱ have similar second-harmonic generation responses of about 0.2 and 0.25 times that of KH₂PO₄.     

二维铅配合物[Pb2(C8H4O4)2(C19H12N4O)2]n·3.5nH2O的水热合成、晶体结构与荧光性质研究

In the title compound, [Pb₂(C₈H₄O₄)₂(C₁₉H₁₂N₄O)₂]_n·3.5nH₂O(1), has been synthesized by the hydrothermal assembly of 1,4-benzenedicarboxylate and 4-(1H-1,3,7,8-tetraazacyclopenta[l]-phenanthren-2-yl)phenol(TCPP) with lead acetate. Elemental analysis, X-ray crystal structure analysis, IR spectrum, thermogravimetric analysis and luminescence property were carried out for the structural determination and characterization of the title compound. Compound 1 crystallizes in triclinic, space group P1 with a=1.013 54(10) nm, b=1.104 84(11) nm, c=1.210 05(12) nm, α=76.812 0(10)°, β=74.814 0(10)°, γ=86.030 0(10)°, V=1.273 1(2) nm³, Pb₂C₅₄H₃₉N₈O_13.5, M_r=1 430.31, Z=1, D_c=1.866 g·cm^-3, μ=6.680 mm^-1, F(000)=691, R=0.027 3 and wR=0.068 7 for 4 042 observed reflections (I>2σ(I)). The compound 1 exhibits two-dimensional network structures, which are further stacked through π-π interactions and hydrogen bonds to form three-dimensional supramolecular polymer. Solid-state luminescent spectrum of the compound 1 indicates intense fluorescent emission. CCDC: 748883.     

配位聚合物[Mn(2，4，6-TMBA)2(H2O)3]n·2nH2O的水热合成和晶体结构

The title compound, [Mn(2,4,6-TMBA)₂(H₂O)₃]_n·2nH₂O(1), where 2,4,6-TMBA=2,4,6-trimethylbenzoic acid, was synthesized and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic, space group C2/c with a=2.929 9(6) nm, b=1.036 4(2) nm, c=8.222 04(17) nm, V=2.494 7(9) nm³, Z=4, M=471.40, D_c=1.255 g·cm^-3, μ=0.571 mm^-1, F(000)=996, R_int=0.029 4, R=0.037 6 and wR=0.094 9. The Mn atoms are octahedrally coordinated by two O atoms of two ligands and four O atoms of water. The carboxyl group coordinates to Mn(Ⅱ) in the mode of monodentate, while the O atoms of water molecules coordinates in bridging mode. The complex shows a one-dimensional chain structure bridged by water molecules. CCDC: 297750.     

FePO4·4H2O的脱水动力学研究

用热分析(TG-DTG-DTA)、X射线衍射(XRD)技术研究了固态物质FePO4·4H2O在空气中脱水过程.热分析结果表明,FePO4·4H2O在空气中脱水的质量变化率与理论计算相吻合.XRD结果表明,FePO4·4H2O脱水产物为FePO4.由等转换率法得到脱水过程的活化能,依此为初始值,用多元非线性回归得到了失水反应拟合的最可几模型为两步连串反应:D4→Fn,活化能分别为79.62和103.04 kJ·mol-1,IgA值分别为8.40和11.02.     

Solid state synthesis of CuFe2O4 from Cu(OH)2?·?CuCO3–4FeC2O4?·?2H2O mixtures: mechanism of reaction and thermal characterization of CuFe2O4

Copper Ferrite has been prepared by solid state synthesis of milled mixtures of copper basic carbonate [Cu(OH)₂ · CuCO₃] and iron (II) oxalate dihydrate [FeC₂O₄ · 2H₂O]. The reaction mechanism has been studied by simultaneous TG/DSC analysis: the different steps of the mass loss process have been individuated along with the relevant enthalpy terms starting from both physical and mechanically activated mixtures. CuFe₂O₄ has been synthesized by annealing the mechanically activated mixture at 750–800 °C while no pure CuFe₂O₄ is obtained by annealing the physical mixture at temperatures as high as 1100 °C. CuFe₂O₄ has been characterized as concerns the molar het capacity, the tetragonal–cubic transition enthalpy and the Curie point.     

Synthesis and characterization of a new octamolybdate (NH4)4[Mo8O24(C3H2O2)2] · 4H2O

A new complex with the formula (NH₄)₄[Mo₈O₂₄(C₃H₂O₂)₂] · 4H₂O (1) has been synthesized and characterized by single crystal X-ray diffraction and infrared spectrum. The complex is small yellow crystal and space group P ₁ with a = 9.9869(18) ?, b = 10.030(19) ?, c = 10.366(19) ?, α = 91.68(3)°, β = 98.94(3)°, γ = 119.37(2)°, V = 887(3) ?³, and Z = 1. The complex contains two malonic acid ligands bonded to the γ-Mo_{8 26}⁴⁻ ions which consist of eight MoO₆ edge-sharing octahedral. In this crystal structure, the octamolybdate anion is mutually hydrogen bonded by ammonium ions and water molecules.     

Crystal structure of K2[Mo3(PdPPh3)S4(C2O4)3(H2O)3]·0.5H2O

By the reaction of [Mo₃S₄(C₂O₄)₃(H₂O)₃]²⁻ with PdCl₂ and NH₄H₂PO₂ as a reducing agent, followed by the addition of PPh₃, a new oxalate cuboidal cluster complex [Mo₃(PdPPh₃)S₄(C₂O₄)₃(H₂O)₃]²⁻ is obtained. It was isolated and structurally characterized as K₂[Mo₃(PdPPh₃)S₄(C₂O₄)₃(H₂O)₃]·0.5H₂O. Original Russian Text Copyright ? 2008 by A. L. Gushchin, M. N. Sokolov, D. Yu. Naumov, and V. P. Fedin __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 49, No. 4, pp. 775–778, May–June, 2008.     

Synthesis, crystal structure and luminescence of a novel metal-organic polymer {Cd2(C4H2O4)2(C4H6N2)2(H2O)2 · 2H2O}n

The novel 3D coordination polymer {Cd₂(C₄H₂O₄)₂(C₄H₆N₂)₂(H₂O)₂ · 2H₂O} _n (I) has been synthesized and characterized by standard solid state methods including single-crystal X-ray crystallography. The compound crystallizes in triclinic space group P [`1]\bar 1 with a = 8.589(4), b = 10.585(3), c = 13.094(1) ?, α = 84.91(4)°, β = 79.21(0)°, γ = 83.76(4)°, V = 1159.5(1) ?³, Z = 2. The fumaric acid acts as a multimodal bridging ligand in the polymer unit. One of the fumaric acid ligands tridentately chelates to two Cd²⁺ cations in the same dinuclear unit, while the other bidentately chelates to two Cd²⁺ cations in another dinuclear unit. The two metal centers possess slightly distorted pentagonal bipyramid geometry with four Cd {(μ₄-fumarato)-(μ₂-fumarato)-bis(2-methylimidazolyl)-diaqua} units joining together to form a 28-membered ring. The whole molecule exhibits a through channel along y-axis and 2D layers in xz plane. With hydrogen bond and π-π interaction, the 2D layers construct a 3D microporous network.     

Synthesis and crystal structure of (C3N5H6S)2[UO2(C2O4)2(H2O)] · C2N4H4

The formation of the thioammelinium cation in an aqueous solution in the presence of uranyl ions is demonstrated. Single crystal X-ray diffraction study of (C₃N₅H₆S)₂[UO₂(C₂O₄)₂(H₂O)] · C₂N₄H₄ was carried out and the geometric characteristics of thioammelinium were determined for the first time. The crystals are triclinc, space group , Z = 2, a = 8.5201(11) ?, b = 11.4027(14) ?, c = 14.329(2) ?, α = 103.182(5)°, β = 99.607(6)°, γ = 109.698(4)°, R = 0.0526. The main structural units in the crystal are mononuclear complex groups [UO₂(C₂O₄)₂(H₂O)]²⁻ corresponding to the crystal chemical group AB ₂ ⁰¹ M¹ (A = UO ₂ ²⁺ , B⁰¹ = C₂O ₄ ²⁻ , M¹ = H₂O) of uranyl complexes. Uranium-containing mononuclear complexes are connected into a three-dimensional framework through electrostatic interactions and hydrogen bonds involving thioammelinium ions, water molecules, and cyanoguanidine. Original Russian Text ? L.B. Serezhkina, A.V. Virovets, E.V. Peresypkina, I.V. Medrish, 2007, published in Koordinatsionnaya Khimiya, 2007, Vol. 33, No. 5, pp. 380–385.     

[Gd(C10H9N2O4)(C10H8N2O4)(H2O)3]2·phen·4H2O的晶体结构和生物活性

在水乙醇混合溶剂中，首次得到了2-羰基丙酸水杨酰腙、1，10-菲啰啉与硝酸钆形成的配合物[Gd(C₁₀H₉N₂O₄)(C₁₀H₈N₂O₄)(H₂O)₃]₂·phen·4H₂O，并测试了其单晶结构。该配合物属三斜晶系，空间群为P-1。每个配合物分子中有两个九配位的钆的结构单元，每个钆离子与两个三齿配体2-羰基丙酸水杨酰腙（分别以负一价和负二价形式）和三个水分子配位。每个钆单元在空间呈扭曲的单帽四方反棱柱。同时还有一个游离的1，10-菲啰啉存在于晶格中，通过氢键与配位水作用。生物活性试验表明该配合物对三种病原菌有一定的抑菌活性。     

[Pt2(P2O4H2)4]4-和[Pt2(P2O4CH4)4]4-基态和激发态性质的理论研究

采用从头计算MP2和CIS方法分别优化等电子双核d⁸配合物[Pt₂(P₂O₄H₂)₄]^4-和[Pt₂(P₂O₄CH₄)₄]^4-的基态和激发态结构。结果表明基态Pt-Pt距离分别为0.290 5和0.298 7 nm，与实验的0.292 5和0.298 0 nm符合。NBO计算的Pt-Pt键级以及Pt原子间伸缩振动说明Pt-Pt相互作用具有吸引本质。CIS计算揭示电子激发到Pt-Pt的σ(p_z)成键轨道使得相互作用增强。保持激发态几何，含时密度泛函理论(TD-DFT)计算的溶液发射分别为449和475 nm，与实验值512和510 nm接近。     

配合物[Co(2，3-tri)2Cl]·ZnCl4·Cl·H2O和[Co(amp)3]·amph·Cl·2ZnCl4·H2O合成及晶体结构

采用三元胺及二元胺混配方法进行[Co(N)₅Cl]²⁺配合物的合成，分离出分别由三元胺配体和二胺配体构成的2个钴胺配合物。晶体结构测定表明由三元胺配体构成的钴胺配合物中，三元胺为N-(2-Aminoethyl)-1，3-propanediamine(记为2，3-tri)，但并未以六胺形式配位[Co(N)₆]³⁺，而以六胺五配位形式形成[Co(N)₆Cl]²⁺，这     

复盐K2Zn(IO3)4·2H2O的热化学研究

The standard enthalpy of formation (Δ_fH^?_m［K₂Zn(IO₃)₄·2H₂O,s,298.2K］=-2210.68 kJ·mol^-1) of a double salt K₂Zn(IO₃)₄·2H相似文献   

水系混合离子全电池LiMn2O4//NaTi2(PO4)3

分别以LiMn_2O_4,NaTi_2(PO_4)_3为正负极,1 mol·L~(-1) Li_2SO_4和0.5 mol·L~(-1) Na_2SO_4的混合水溶液为电解液组装成一种水系混合离子全电池。分别将正负极材料在3种不同水相电解液(1 mol·L~(-1) Li_2SO_4、0.5 mol·L~(-1)Na_2SO_4以及1 mol·L~(-1) Li_2SO_4+0.5 mol·L~(-1)Na_2SO_4混合电解液)中进行循环伏安和恒流充放电测试,结果发现,LiMn_2O_4在上述电解液中仅有Li~+的脱出/嵌入而Na~+由于半径较大而不参与该过程,NaTi_2(PO_4)_3在3种电解液中Li+、Na+均参与嵌入/脱嵌过程,且Li~+和Na~+的嵌入/脱出峰电位相差不大,分别为-0.82和-0.64 V,-0.95和-0.75 V;全电池在265 mA·g~(-1)电流密度下平均放电电压为1.55 V,充放电比容量分别为100.1和74.9 m Ah·g~(-1)。     

氯桥连1-甲基-3-羧甲基咪唑镉一维配位聚合物：[Cd2(C6H8N2O2)2Cl4]n·3nH2O的合成及晶体结构

A metal-organic coordination polymer [Cd₂(C₆H₈N₂O₂)₂Cl₄]_n·3nH₂O[where C₆H₈N₂O₂ is ionic liquid, 1-carboxymethyl-3-methylimidazolium] 1 has been hydrothermally synthesized and characterized by X-ray diffraction single-crystal structure analysis. The complex crystallizes in orthorhombic, space group Aba2 with a=1.747 6(3) nm, b=1.933 6(4) nm, c=0.692 75(13) nm, V=2.340 9(8) nm³, M_r=700.96, D_c=1.989 g·cm^-3, μ(Mo Kα)=2.312 mm^-1, F(000)=1 368, Z=4, the final R=0.021 4 and wR=0.051 2 for 3 331 observed reflections (I>2σ(I)). Each Cd(Ⅱ) atom is in a distorted octahedral environment, surrounded by an uncommon symmetrical bidentate chelating carboxylato group and two pairs of bridging chloro ligands. Successive octahedra related by the c-glide of eration share edges to generate a one-dimensional polymeric structure. CCDC: 692298.