共查询到20条相似文献,搜索用时 15 毫秒
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Yunling LiuWang Liu Yan XingZhan Shi Yunlong FuWenqin Pang 《Journal of solid state chemistry》2002,166(2):265-270
A new two-dimensional zinc phosphate Zn6(PO4)5(HPO4)·C8N5H28·5H2O has been synthesized hydrothermally using tetraethylenepentamine (TEPA) as structure-directing agent and its structure was determined by means of single-crystal X-ray diffraction. The title compound crystallizes in the orthorhombic system, space group Pca21 (No.29) with lattice parameters a=18.6286(12) Å, b=8.0804(5) Å, c=22.5019(15) Å, V= 3387.1(4) Å3, Z=4, R1=0.0389 and wR2=0.0862 [4042 observed reflections with I>2σ(I)]. The structure involves a network of ZnO4, PO4, and PO3(OH) tetrahedra forming macroanionic inorganic layers with eight-membered apertures. The charge compensation is achieved by the quintuply protonated TEPA molecule in interlamellar space, which interact with the inorganic layers via hydrogen bonding. 相似文献
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在140℃下,以3-溴-4-甲基苯甲酸和咪唑为配体,通过水热法在甲醇/水混合溶剂中反应24 h合成了锌(Ⅱ)配合物Zn(C3H4N2)2(C8H6O2Br)2。通过元素分析、红外光谱、热重分析和X射线粉末衍射对配合物进行了结构表征,同时用X射线单晶衍射分析确定了其晶体结构。结果表明,其晶体属单斜晶系,空间群为C2/c,晶胞参数:a=13.257(3),b=9.765(2),c=20.494(4),β=107.79(3)°,V=2526.3(9)3,Dc=1.655g·cm-3,μ=4.170mm-1,F(000)=1248,Z=4,最终残差因子R1=0.0552,wR2=0.1378。配合物为单核结构,中心锌(Ⅱ)离子与来自2个3-溴-4-甲基苯甲酸根的2个O原子及2个咪唑分子的2个N原子配位,形成了畸变的四方锥几何体。晶体内,分子间则通过N—H…O氢键作用在ab面形成了层状结构。研究了配合物的发光性质。 相似文献
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The title compound [C4H12N2] 3 [PMo12O40] was synthesized from the hydrothermal reaction and charac-terized by IR, elemental analysis and X-ray signal crystal structural analysis. The crystal of the title complex belongs to trigonal space group R3c with a=1.788 62 nm, c=2.354 3 nm, and V=6.522 62 nm3, Z=6, R1=0.038 4, wR2=0.102 0. The compound consisted of piperazine and PMo12O403-, and the structure is extended to three dimensional framework owing to the hydrogen bond between the O atoms and N atoms. The bulk-modified carbon paste electrode (APM-CPE) using this compound as modifier shows a good electrocatalytic activity toward the oxidation of ascorbic acid(AA). CCDC: 707968. 相似文献
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Lei Wang 《Journal of solid state chemistry》2004,177(1):80-88
Two organically templated zincophosphites, (C6H14N2)·[Zn3(HPO3)4] and (C4H14N2)·[Zn3(HPO3)4] have been prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction. (C6H14N2)·[Zn3(HPO3)4] crystallizes in the triclinic space group , with cell parameters, a=9.363(4) Å, b=10.051(4) Å, c=10.051(4) Å, α=85.777(13)°, β=82.091(9)°, and γ=79.783(9)°. (C4H14N2)·[Zn3(HPO3)4] crystallizes in the monoclinic space group P21/c, with cell parameters, a=9.9512(3) Å, b=10.1508(3) Å, c=17.8105(5) Å, and β=95.6510(10)°. Although the two structures are different, they have the same anionic framework compositions of [Zn3(HPO3)4]2−. Their frameworks are built up from strictly alternating ZnO4 tetrahedra and HPO3 pseudo pyramids by sharing vertexes. There exist channels with an eight-membered ring window along the a- and c-axis. Powder X-ray diffraction, IR spectroscopy, 31P MAS solid-state NMR, thermogravimetric and differential thermal analyses were also carried out. 相似文献
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Open-framework metal phosphates have been the subject of intense research owing to their interesting structural chemistry and potential applications in catalysis and ion exchange. The gallium phosphate family has exhibits rich structural chemistry. A novel gallium phosphate Ga3P2O8(OH)3(H2O)(GaPO-CJ36) has been prepared in a hydrothermal reaction system of GaO(OH)-H3PO4-Co(chxn)3Cl3-H2O at 180 ℃ for 7 days. Single-crystal X-ray analysis shows that GaPO-CJ36 crystallizes in the P21/c space group with a=1.833 35(12) nm, b=0.503 94(3) nm, c=1.062 90(9) nm, V=0.982 01(12) nm3, and Z=4. The connection of GaO2(OH)3(H2O) octahedra, PO4 and GaO4 tetrahedra through vertex oxygen atoms forms a three-dimensional open framework, which contains 8-ring channels along the [010] direction. Its structure is composed of interesting [344484] cages, which have not been found in known gallium phosphates. CSD: 416779. 相似文献
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以3-甲氨基丙胺为结构导向剂,在水热条件下合成了1个具有三维开放骨架结构的微孔磷酸铝化合物[C4N2H14][H2Al3P3O14](1),并通过X射线单晶衍射确定了其结构,用粉末X射线衍射(PXRD)、热重(TG)、元素分析(ICP及CHN)和扫描电子显微镜(SEM)对其进行表征.结果表明,化合物1属正交晶系,Pbca空间群,晶胞参数a=1.59839(11)nm,b=0.99402(6)nm,c=1.82261(11)nm,V=2.8958(3)nm3.化合物1的无机骨架由铝氧多面体(AlO5/AlO6)和磷氧四面体(PO4)严格交替连接构筑而成,形成了在[010]方向上具有一维十元环孔道的三维阴离子开放骨架.每个P原子通过桥氧原子与相邻的4个Al原子相连,而Al原子除了通过桥氧原子与相邻的4个P原子相连之外,还通过羟基的桥氧原子与1个或2个Al原子相连,分别形成五配位和六配位的Al.化合物1在550℃空气或氧气气氛下灼烧5 h后转变为具有ATV分子筛结构的微孔磷酸铝分子筛AlPO4-25,且一直稳定到800℃. 相似文献
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Employing 3-dimethylamino-1-propylamine as a template, a new three-dimensional (3-D) zincophosphite (C5H16N2)·[Zn3(HPO3)4]·H2O has been prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction (XRD), FTIR, elemental analysis, powder XRD, and thermogravimetric analysis (TGA). The compound crystallizes in the triclinic space group , with cell parameters, a=8.9884(2) Å, b=10.326(2) Å, c=11.917(2) Å, α=66.98(3)°, β=89.01(3)°, and γ=78.98(3)°, V=997.2(3) Å3 and Z=2. The connectivity of the ZnO4 tetrahedra and HPO3 pseudo pyramids results in inifinite edge-sharing, ladderlike chains of 4-membered rings, which are further linked by Zn-O-P bonds to form a 3-D structure that with interesting 12-membered ring channels along the [100] and [001] directions. The diprotonated amine molecules sit in the middle of the channels along the [100] direction and interact with the framework via hydrogen bonds. There also exist channels with 8-membered ring window along the [100] and [010] directions. 相似文献
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Zoe A.D. Lethbridge 《Journal of solid state chemistry》2003,172(1):212-218
Three manganese oxalates have been hydrothermally synthesized, and their structures determined by single-crystal X-ray diffraction. MnC2O4·2H2O (I) is orthorhombic, P212121, , , , , Z=4, final R, Rw=0.0832, 0.1017 for 561 observed data (I>3σ(I)). The one-dimensional structure consists of chains of oxalate-bridged manganese centers. [C4H8(NH2)2][Mn2(C2O4)3] (II) is triclinic, , , , , α=81.489(2)°, β=81.045(2)°, γ=86.076(2)°, , Z=1, final R, Rw=0.0467, 0.0596 for 1773 observed data (I > 3σ (I)). The three-dimensional framework is constructed from seven coordinate manganese and oxalate anions. The material contains extra-framework diprotonated piperazine cations. Mn2(C2O4)(OH)2 (III) is monoclinic, P21/c, , , , β=91.10(3)°, , Z=1, final R1, wR2=0.0710, 0.1378 for 268 observed data (I>2σ (I)). The structure is also three dimensional, with layers of MnO6 octahedra pillared by oxalate anions. The hydroxide group is found bonded to three manganese centers resulting in a four coordinate oxygen. 相似文献
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Suhua Shi 《Journal of solid state chemistry》2004,177(11):4183-4187
A new vanadium(III) phosphite, (C4H8N2H4)0.5(C4H8N2H3)[V4(HPO3)7(H2O)3]1.5H2O, has been synthesized hydrothermally by using V2O5, H3PO3 as reactants, piperazine as the structure-directing agent. The as-synthesized product was characterized by powder X-ray diffraction, IR spectroscopy, inductively coupled plasma analysis, thermogravimetric analysis, and SQUID magnetometer. Single-crystal X-ray diffraction analysis shows that the title compound crystallized in the trigonal space group (No. 165) with the parameters: , , and Z=4. Its structure is built up by alternation of octahedral VO6 or VO5(H2O) and pseudo-pyramidal HPO3 units to form infinite 2D layers, and these layers are interconnected by sharing vertex-oxygen with octahedral VO6 units to generate a 3D open-framework structure with 12-membered ring channels in a and b directions, respectively, where there exist entrapped diprotonated and mono-protonated piperazine cations, and water molecules. Magnetic measurement indicates that paramagnetic behavior is observed down to 4 K. 相似文献
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A novel nickel(Ⅱ) complex with 2,4-dihydroxybenzalidene benzoylhydrazone and pyridine ligands, Ni(C14H10N2O3)(C5H5N), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex has been determined by single crystal X-ray diffraction techniques. The crystal belongs to orthorhombic, space group Pbca. The cell parameters are: a=1.580 20(19) nm, b=1.362 18(16) nm, c=1.616 50(19) nm, and V=3.479 5(7) nm3, Z=8, Dc=1.497 Mg·m-3, μ(MoKα)=1.139 mm-1, F(000)=1 616, R=0.032 9 and wR=0.077 0 for 2 772 observed reflections (I>2σ(I)) out of 3810 unique ones. The nickel(Ⅱ) ion lies in a distorted square-planar environment composed of two oxygen atoms, one nitrogen atom of tridentate acyhydrazone schiff base ligand and one nitrogen atom of the pyridine ligand. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 244668. 相似文献
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A novel porous coordination polymer [La(C8H6NO2)3]n was synthesized by hydrothermal reaction of flexible ligands 3-(3-pyridyl)acrylate and La(NO3)3·6H2O. The structure was characterized by elemental analysis, IR spectroscopy and X-ray single crystal diffraction. X-ray single crystal analysis reveals the structure consists of [La(C8H6NO2)3]n. It crystallizes in monoclinic crystal system with space group P2(1)/c. Crystallographic date: a=0. 7889(3)nm, b=2.5916(9)nm, c=1.1489(4)nm, α=90.00°, β=95.219(6)°, γ=90.00°, V=2.3393(15)nm3, Z=4, Dc=1.656g·cm-3, μ=1.871mm-1, F(000)=1152, R1=0.0328, wR2=0.0522. CCDC: 211700. 相似文献
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The title coordination compound with N-substituted-salicyl Schiff ligand, Cu(C15H12N2O3)(C5H5N), has been synthesized. The coordination compound crystallizes in orthorhombic system, space group Pbca with a=2.037 62(7) nm, b=0.698 45(2)nm, c=2.508 76(9)nm, V=3.570 4(2) nm3, Z=8, F(000)=1 688, Dc=1.529 g·cm-3, Mr=410.91, μ=1.250 mm-1, R=0.031 3 and wR=0.077 0. In the coordination compound, one phenolate oxygen, one carbonyl oxygen and one hydrazine nitrogen atom from the dianionic ligand N-salicylaldehyde-N′-(4-methoxybenzoyl) hydrazone and one pyridine nitrogen atom coordinate to Cu(Ⅱ) ion, forming a distorted square plane. CCDC: 218182. 相似文献
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Yu Wang Jihong Yu Yi Li Yu Du Ruren Xu Ling Ye 《Journal of solid state chemistry》2003,170(2):303-307
Employing trans-1,4-diaminocyclohexane (trans-1,4-DACH) as a template, a new two-dimensional layered zinc phosphite (C6H16N2)Zn3(HPO3)4H2O (1) has been prepared hydrothermally. Single-crystal X-ray diffraction analysis shows that it crystallizes in the monoclinic space group P21/n with a=10.458(2) Å, b=14.720(3) Å, c=13.079(3) Å, β=97.93(3)°, V=1994.1(7) Å3, Z=4, R1=0.0349 (I>2σ(I)) and wR2=0.0605 (all data). The inorganic layer is built up by alternation of ZnO4 tetrahedra and HPO3 pseudo pyramids forming a 4.6.8-net. The sheet is featured by a series of capped six-membered rings. The diprotonated trans-1,4-DACH molecules reside in the interlayer region and interact with the inorganic network through H-bonds. 相似文献
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The novel copper(Ⅱ) complex with salicylaldehyde benzoylhydrazone and pyridine ligands, Cu(C14H10N2O2)(C5H5N), has been synthesized and characterized by elemental analysis, IR and thermal analysis. The crystal structure of the title complex has been determined by single crystal X-ray diffraction techniques. The crystal belongs to monoclinic with space group P21/c. The cell parameters are: a=1.6362(9)nm, b=1.7140(9)nm, c=1.2255(7)nm, β=105.168(9)°, V=3.317(3)nm3, Z=8, Dc=1.525g·cm-3, μ(MoKα)=1.334mm-1, F(000)=1560. The structure was refined to final R1=0.0376, wR2=0.0909. The copper(Ⅱ) ion lies in a dis-torted square-planar environment composed of two oxygen atoms, one nitrogen atom of tridentate acyhydrazone Schiff base ligand and one nitrogen atom of the pyridine ligand. CCDC: 193111. 相似文献
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Ray-Kuang Chiang Niang-Tsu ChuangChing-Shuei Wur Mong-Fu ChongChung-Rong Lin 《Journal of solid state chemistry》2002,166(1):158-163
A new hybrid organic-inorganic three-dimensional compound, [Co4(OH)2(H2O)2](C4H11N2)2[C6H2(CO2)4]2·3H2O 1, has been synthesized via hydrothermal reactions and characterized by single-crystal X-ray diffraction, infrared spectroscopy, thermogravimetric analysis, and magnetic techniques. Compound 1 crystallizes in the monoclinic space group P21/n (no. 14) with a=6.3029(9) Å, b=16.413(2) Å, c=17.139(2) Å, β=98.630(2)°, V=1735.0(4) Å3, Z=2. Compound 1 contains tetranuclear Co4(μ3-OH)2(H2O)2 clusters that are inter-linked by pyromellitate bridging ligands into a three-dimensional structure containing one-dimensional tunnels along the a-axis with water and pendant monoprotonated piperazine molecules in the center. The variable temperature magnetic susceptibility was measured from 2 to 300 K at 5000 Oe showing a predominantly anti-ferromagnetic interaction in 1, and the field dependence of magnetization was measured at 2, 5, 15, and 20 K indicating the competition of magnetic interactions in the tetranuclear centers. 相似文献