Synthesis and structure determination of a new layered zincophosphate: [H2N2C6H16]0.5[Zn2(PO4)(HPO4)(H2O)]·H2O

The synthesis and crystal structure of a new microporous zincophosphate are described. [H₂N₂C₆H₁₆]_0.5[Zn₂(PO₄)(HPO₄)(H₂O)]·H₂O crystallizes in the triclinic space group P1¯ with a = 8.822(4), b = 9.236(4), c = 8.451(3) Å, = 67.19(3), = 91.32(3), = 111.10(3)°, V = 586.7(4) ų and Z = 2. This new material consists of infinite two-dimensional anionic layers alternated with planes containing organic diprotonated templates, N, N, N, N-tetramethylethylenediamine [H₂N₂C₆H₁₆]²⁺ molecules. The framework structure is built up of ZnO₄, ZnO₃OH₂, PO₄, and PO₃OH tetrahedra, linked through oxygen vertices. The presence of terminal OH₂ and OH groups, leads to an open structure containing four- and eight-rings. The organic molecules are interconnected to the framework through hydrogen bonds.     

Synthesis and characterization of a layered chlorozincophosphate templated by protonated 4‐methylpiperidine

A chlorozincophosphate with the composition Zn(HPO₄)Cl·[C₆H₁₄N] has been synthesised under mild conditions in water medium in presence of 4‐methylpiperidine as organic template. The structure was determinated by single crystal X‐ray diffraction. The unit cell is orthorhombic (space group Pcab) with a = 8.743(9), b = 9.592(6), c = 26.573(6) Å, Z = 8 and V = 2228.91(12) ų. The structure involves a network of ZnO₃Cl and PO₃(OH) tetrahedra forming macroanionic inorganic layers with four and eight‐membered rings. Charge balance is achieved by the protonated amine which is trapped in the interlayers space and interacts with the organic framework through hydrogen bonding. Solid state ³¹P and ¹³C MAS‐NMR spectroscopies are in full agreement with the X‐ray structure. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure and spectroscopic studies of a new organic monohydrogenmonophosphate dihydrate

The crystal synthesis and structure of a new organic monohydrogenmophosphate (3,4‐Cl₂‐CH₂C₆H₃NH₃)₂HPO₄·2H₂O are reported. This compound crystallizes in the monoclinic P2₁/n with a = 9.081(7) Å, b = 6.501(5) Å, c = 35.423(12) Å, β = 91.09(5)°, V = 2090.9(2) ų, and Z = 4. Crystal structure was solved and refined to R = 0.042, using 2543 independent reflections. It can be described by inorganic layers, including the HPO₄^‐ anions and the H₂O molecules, parallel to (a, b) planes and situated at z = 0 and z = 1/2. The interlayer spacing is occupied by the organic molecules which perform different interactions around the 3D network cohesion. A characterization of this compound by solid‐state (¹³C, ³¹P) MAS NMR and IR spectroscopies is also reported. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and X-ray structure analysis of 2-acetylamino-benzoic acid

The title compound crystallizes in the orthorhombic space group Fdd2 with unit cell parameters a = 10.848(1) Å, b = 30.264(1) Å and c = 10.577(1) Å, V = 3472.47(2) ų, and Z = 4. The final reliability index is 0.030 for 700 observed reflections. Nitrogen of the amide group and carbon atom of the acid group deviate significantly below and above the plane of the phenyl ring. The crystal cohesion is accentuated by N—HO and O—HO hydrogen bonds.     

Synthesis and crystal structure determination of two dispiro compounds from laboratory x‐ray powder diffraction data

The crystal structures of the dispiro compounds 1,3,4,8,10,11‐Hexaphenyl‐13‐methyl‐1,2,8,9,13‐pentaazadispiro[4.1.4.3]tetradeca‐2,9‐dien‐6‐one ( 3a ) and 4,11‐Bis(4‐methoxyphenyl)‐13‐methyl‐1,3,8,10‐tetraphenyl‐1,2,8,9,13‐pentaazadispiro‐[4.1.4.3]tetradeca‐2,9‐dien‐6‐one ( 3b ) have been determined at room temperature from X‐ray powder diffraction data using the method of simulated annealing as implemented in the programs DASH and TOPAS. Subsequent Rietveld refinements using the data collected to 1.5 Å resolution yielded R‐Bragg values of 2.2% for ( 3a ) and 3.7% for ( 3b ). It was found, that both compounds crystallize in the monoclinc space group P 2₁/n with lattice parameters of a = 17.1656(5) Å, b =13.8128(3) Å, c = 16.1016(5) Å, and β = 103.7330(2)° for ( 3a ) and a = 17.2529(8) Å, b = 13.8729(5) Å, c =16.1287(10) Å, and β = 103.6910(3)° for ( 3b ). Both compounds exhibit a distorted hexagonal close type of packing (hcp) of the molecular centers of gravity. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and crystal structure of indium arsenate and phosphate dihydrates with variscite and metavariscite structure types

The hydrothermal synthesis, crystal structure analysis, and spectroscopic studies of InPO₄·2H₂O (1) and InAsO₄·2H₂O (2) are reported. Compound 1 is isomorphic with metavariscite: monoclinic P2₁/n (No. 14), a = 5.4551(3) Å, b = 10.2293(4) Å, c = 8.8861(3) Å, = 91.489(4)°, Z = 4, and compound 2 is isomorphic with variscite: orthorhombic Pbca (No. 61), a = 10.478(1) Å, b = 9.0998(8) Å, c = 10.345(1) Å, Z = 8. Their three-dimensional frameworks are built of corner sharing InO₄(H₂O)₂ octahedra and MO₄ (M = P⁵⁺ or As⁵⁺) tetrahedra. The water molecules in both compounds have different environments and are involved in different types of hydrogen bonding. Infrared spectroscopy indicates that water molecules are true H₂O species.     

Synthesis and Crystal Structure of Open Framework Zinc‐Cobalt Phosphate with Zeolite DFT Topology

The synthesis and crystal structure of Zn_(2‐x)Co_x(PO₄)₂(NH₃CH₂CH₂NH₃) (x = 0.61) (ZCP‐DFT) is described. ZCP‐DFT is characterized by means of single‐crystal and powder X‐ray diffraction. Crystal data for ZCP‐DFT: tetragonal, space group P4₂ bc (No. 106), a = 14.7236(6) Å, b = 14.7236(6) Å, c = 8.9544(5) Å, V = 1941.17(16) ų, Z = 8. The structure has 3‐D 8‐ring channel system with protonated ethylenediamine cations in the channel junctions. The framework structure type is the same as the zeolite DFT topology. The synthesis of ZCP‐DFT indicates that cobalt can partially substitute the metal sties of zinc phosphate, which can lead to the modification of physical and chemical properties of the parent compounds.     

Synthesis and structure of a 2D Zn complex with mixed ligands stacked in offset ABAB manner

The title complex, {[Zn(ODIB)_1/2(bpdc)]·2DMF}_n was prepared under hydrothermal conditions (dimethylformamide and water) based on two ligands, namely, 1,1′-oxy-bis[3,5-diimidazolyl-benzene] (ODIB) and biphenyldicarboxylic acid (H₂bpdc). ODIB ligands link Zn cations to give layers in crystal. bpdc^2– anions coordinate to Zn atoms, however, their introduction does not increase the dimension of the structure. Each layer is partially passes through the adjacent layers in the offset ABAB manner.     

Synthesis,structure and optical properties of zinc oxide hexagonal microprisms

Zinc oxide (ZnO) pencil‐head‐like (PHL) microprisms were synthesized by a hydrothermal route using a zinc (Zn) plate as a source and substrate. The structural analysis confirmed the formation of ZnO with hexagonal wurtzite phase on the hexagonal Zn substrate and the growth of the ZnO microparticles along the [101] direction. The room temperature photoluminescence (PL) of the ZnO microprisms showed a sharp UV emission band located at around 380 nm, which is expected to originate from the radiative recombination of free excitons. The sharp UV emission band, with a full width at half‐maximum of about 15 nm and an extremely weak visible emission, confirms the high crystal quality of the synthesized ZnO microprisms. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and crystal structure of a novel 2D Ni(II) complex with malate

An exploration of the nickel‐ malate‐bpa system under hydrothermal conditions, has led to the isolation of a novel framework {[Ni(Hmal)(bpa)]·2.5H₂O}_n ( 1 ) (Hmal = malate dianion, bpa = 1,2‐bi(4‐pyridyl)ethane). Single‐crystal X‐ray analyses reveal that it crystallizes in the orthorhombic space group Fdd2. a = 21.9944(13) Å, b =33.3369(19) Å, c = 10.3969(5) Å, β = 90°. The Ni^II ions are linked into an extended helical chain via Hmal molecules. Further these chains are united together through the bridging bpa to form a 2D grid layer, which exhibits a typical (6,3) topological network. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

有机熔盐(OMS)法制备AgInS2纳米针

本文以AgNO3、INCl3·4H2O和硫代尿素为原料,尿素和氯化胆碱为有机熔剂,用有机熔盐法(OMS)在200℃制备出纯度较高的黄铜矿结构AgInS2纳米针.使用X射线衍射(XRD)、扫描电镜(SEM)、X射线能谱(EDS)等对纳米针的物相、形貌和化学配比进行了定性和定量表征.XRD测试结果表明,实验获得产物确为黄铜矿结构AgInS2.使用Scherrer公式估算了AgInS2产物的晶粒平均粒度大小约为50 ～ 80 nm,表明所得确为AgInS2纳米晶.SEM观测到的纳米晶形貌外形均匀呈针状,纳米针的几何尺寸基于60 ～80 nm×1000～1500 nm.EDS测试结果显示AgInS2纳米针中Ag、In和S三元素的原子相对百分含量为26.66;、24.82;和50.52;,其化学计量比几近于1:1∶2物质的量比.通过紫外可见透过光谱得到截止波长为661 nm,禁带宽度为1.88 eV.以上结果充分表明OMS法是一种制备AgInS2纳米针的有效方式.     

Synthesis,characterization and crystal structure of a novel 2D Cu(I) complex with flexible ligand

An exploration of the Cu(I)‐L system under hydrothermal conditions, has led to the isolation of a novel framework [Cu(I)(L)]_n ( 1 ) (L = bis(3,3‐dimethyl‐4,4‐dihydro‐1H‐pyrazol‐4‐yl)methane). Single‐crystal X‐ray analysis reveals that it crystallizes in the monoclinic, space group C2/c, a = 19.781(4) Å, b =11.026(3) Å, c = 16.339(4) Å, β = 127.186(3)°. The Cu ions are linked into an extended rainbow‐like chain via L molecules. Further, these adjacent chains are united together through hydrogen‐bonded interaction to a 2D layer. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and X-ray crystal structure determination of N-p-methylphenyl-4-benzoyl-3,4-diphenyl-2-azetidinone

The title compound, C₂₉H₂₃NO₂, has been characterized by single-crystal X-ray diffraction at two different temperatures (303 K and 120 K) and wavelengths (MoK _α and CuK _α). The non-centrosymmetric hexagonal crystal structure contains four-membered planar β-lactam ring with an unusually long C-C bond. The β-lactam ring is almost planar.     

Synthesis by organic molten salt method and characterization of chalcopyrite AgInS2 nanorods

In this paper, chalcopyrite AgInS₂ nanorods were synthesized for the first time by a one‐step, ambient pressure, environment friendly organic molten salt (OMS) method at 200 °C. The as‐synthesized products were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS), respectively. The XRD results reveal that the as‐synthesized products at 120–160 °C under ambient pressure contain AgIn₅S₈ which will decrease with the increase of growth temperature. A sample containing only the chalcopyrite AgInS₂ phase is successfully obtained at 200 °C. Furthermore, the elemental compositions are found to become increasingly stoichiometric with increasing temperature. UV‐Vis and photoluminescence (PL) spectra are utilized to investigate the optical properties of AgInS₂ nanorods. By testing on UV‐Vis spectra, it is concluded that the limiting wavelength of the AgInS₂ nanorods is 661 nm and the band gap is 1.88 eV. A broad red emission band peak centered at about 1.874 eV (662 nm) is clearly observed at room temperature, and the intensity of the emission increases with excitation wavelength. In addition, the photoluminescence quantum yield (PLQY) of the nanocrystals at the excitation wavelength of 250 nm was determined to be 13.2%. A possible growth mechanism of AgInS₂ nanorods was discussed. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

利用界面调控制备二维有机半导体晶体及其机制研究

二维有机半导体晶体是利用分子间的范德瓦耳斯力进行自组装生长的单晶材料。本质上的单晶属性使其具备优异的电学特性。更重要的是,二维极限下增强的界面特性能够大幅调控器件行为,为构建多功能界面器件提供可能。此外,充分暴露的电荷输运沟道和极少的晶面内缺陷能够为研究本征的有机电子输运特性创造可能。目前,对于二维有机半导体晶体的生长工艺研究已经取得了较大的进展,但是从理论层面上研究二维晶体生长的自组装过程仍然十分匮乏。本工作利用添加剂辅助结晶技术成功制备出二维有机半导体晶体,并通过偏光显微镜和原子力显微镜对二维晶体进行了全面的表面形貌和结构表征。通过SEM结合EDS技术对关键的形核界面进行了结构和组成的表征以研究晶体生长的机制。研究结果表明:在添加剂界面上,生长材料能够稳定形核,并计算出添加剂构建的有利界面能够将形核势垒降低为SiO₂界面上的1/5。这项工作充分展现了生长界面对于晶体生长的关键作用,并从理论上揭示了界面的调控行为,为二维有机半导体晶体的生长工艺设计提供了可靠的思路。     

Synthesis, characterization and crystal structure of a mononuclear zinc(II) complex derived from 2-methoxy- 6-[(3-cyclohexylaminopropylimino)methyl]phenol

Colourless block-shaped crystals of Dichloro{2-methoxy-6-[(3-cyclohexylaminopropy-limino)methyl]phenolato}zinc(II) methanol, [Zn(C₁₇H₂₆N₂O₂)Cl₂].CH₃OH, have been obtained and characterized by elemental analysis, IR and X-ray single crystal determination. The complex crystallizes in the monoclinic space group P2₁/n with unit cell dimensions a=12.980(3) ?, b=13.139(3) ?, c=13.277(3) ?, β=107.00(3)°, V=2165.4(8) ?³, Z=4, R ₁=0.0631 and wR2=0.1110. X-ray structure determination revealed that the complex consists of a [Zn(C₁₇H₂₆N₂O)Cl₂] moiety and a lattice MeOH molecule. In the crystal structure, molecules are linked through intermolecular N–HO, C–HCl and O–HCl hydrogen bonds, forming chains. It is the first complex derived from the Schiff base ligand 2-methoxy-6-[(3-cyclohexylaminopropylimino)methyl]phenol.Supplementary materialCCDC-606067 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam.ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Synthesis and structure of a bicyclo[2.4.0]-2-nonene

The hydroxy carboxylic acid 1,6-dimethyl-1-hydroxymethyl-6-carboxybicyclo[2.4.0]-2-nonene crystallizes in the space group Pca2₁ (No. 29) with a = 18.563(1), b = 6.393(1), c = 20.750(1) Å, and Z = 8. The two independent molecules in the asymmetric unit each exhibit intra- and intermolecular hydrogen bonding and have closely similar geometries and conformations.     

Synthesis,structure and photoluminescence of a 3D pillared heterometallic coordination polymer containing 2D inorganic cadmium‐potassium‐oxide layer subunits

Self‐assembly of Cd(NO₃)₂ with o ‐phthalic acid monopotassium salt (KHphth) in the presence of ethylenediamine (en) produced a new heterometallic coordination polymer [CdK₂(phth)₂(en)_0.5(H₂O)]_n ( 1 ). Single‐crystal X‐ray analyses reveal that it crystallizes in a monoclinic space group P 2₁/c. a = 11.6707(6) Å, b = 8.1019(4) Å, c = 20.9503(11) Å, β = 94.6640(10)^o. The complex displays an en‐pillared 3D framework, which is constructed from 2D [CdK₂(phth)₂(H₂O)]_n layers featuring uncommon inorganic cadmium‐potassium‐oxide layers containing potassium‐oxide layers. In the solid state, complex 1 shows photoluminescence with the maximum emission intensities at 355 nm upon excitation at 312 nm. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and crystal structure of a 2D Cd(II) complex with a 4,4'‐diazenediyldiphthalic acid ligand

An exploration of the cadmium‐L system under hydrothermal condition, has led to the isolation of a novel framework {[Cd(L)_0.5(H₂O)₃]}_n ( 1 ) (H₄L = 4,4'‐diazenediyldiphthalic acid). Single‐crystal X‐ray analysis reveals that it crystallizes in the triclinic space group P‐1. a = 5.746(3) Å, b =6.526(4) Å, c = 14.701(8) Å, α=92.348(8), β = 99.622(6), γ=106.877(7)°. The Cd^II ions are linked into an extended 2‐D rectangle‐like structure via L ligands, which exhibits an attractive three‐connected honeycomb topological network. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

功能模板导向合成介孔三氧化钨及其光电化学性能

以钨酸(H₂WO₄)为钨前驱体,十二烷胺(DDA)为模板剂,利用模板剂的结构导向功能,合成了比表面积为57.3 m²·g^-1的介孔三氧化钨(DDA-WO₃),是未用DDA制备的非介孔WO₃(H₂WO₄-WO₃)的2.35倍。X射线衍射(XRD)结果表明,400℃下煅烧的DDA-WO₃是具有单斜晶型结晶孔壁的无序介孔结构。此外,400～550℃下煅烧的DDA-WO₃的结晶度均高于同条件的H₂WO₄-WO₃。400℃下的DDA-WO₃/FTO(掺氟氧化锡)在1.0 V的Ag/AgCl偏压作用下,可以产生0.18 mA·cm^-2的饱和光电流,是H₂WO₄-WO₃/FTO(0.06 ...