Hydrothermal synthesis and characterization of two new bicapped Keggin heteropoly tungstovanadated derivatives

Two new heteropoly tungstovanadate derivatives, [Fe(phen)₃]₂[W_10.5V_4.5O₄₂]·3H₂O (1) and [Fe(phen)₃]₂[W₁₀V₅O₄₂].6H₂O (2) (phen=1,10′-phenanthroline), have been synthesized under hydrothermal conditions by using different starting materials, and characterized by elemental analysis, IR, ESR, XPS, TGA and single-crystal X-ray diffraction analysis. Crystal data for compound 1: C₇₂H₅₄Fe₂N₁₂O₄₅V_4.5W_10.5, monoclinic, space group C2/c, , , , β=99.882(8)°, V=10002(5) ų, Z=4; for compound 2, C₇₂H₆₀Fe₂N₁₂O₄₈V₅W₁₀, monoclinic, space group C2/c, a=30.246(6) Å, , c=25.329(5) Å, β=100.34(3)°, V=10483(4) ų, Z=4. The crystal structure analysis reveals that both polyoxoanions are decorated with the [Fe(phen)₃]²⁺ cations_, and that they have analogous structure to each other with slightly different packing modes of the polyoxoanions, [Fe(phen)₃]²⁺ cations and water molecules. They are further linked to form two-dimensional (2D) supramolecular networks through extensive hydrogen bonding.     

两种含氮芳香羧酸配合物的水热合成及结构表征

用水热法合成了两种结构新颖的配合物[Cu(PDA)(H2O)2](Ⅰ)和[Ni(PZCA)2(H2O)2](Ⅱ)(H2PDA=2,6-吡啶-二甲酸,HPZCA=2-吡嗪羧酸);利用元素分析、红外光谱和X射线单晶衍射等分析了产物的组成和结构.结果表明,两种配合物均属单斜晶系,空间群均为P21/c,中心离子Cu(Ⅱ)和Ni(Ⅱ)均采取畸变的六配位八面体配位方式;配合物I通过π-π堆积作用和氢键构筑成三维结构,配合物Ⅱ以氢键联接形成二维层状结构.此外,配合物Ⅱ中的PZCA-来自于Ni(Ⅱ)对2,3-吡嗪-二羧酸(H2PZDA)配体的催化脱羧过程.     

Hydrothermal synthesis and characterization of two organically templated cadmium borophosphates with novel structures

Two organically templated cadmium borophosphates, (C(4)H(16)N(3))[CdClB(2)P(3)O(12)(OH)] (1) and (C(2)H(10)N(2))[CdB(2)P(3)O(12)(OH)] (2), were synthesized hydrothermally in the presence of structure-directing amines. Compound 1 has a complex layered structure (orthorhombic, Pbca (No. 61); a = 9.470(2), b = 12.307(3), c = 27.311(6) A; V = 3183 (1) A(3); Z = 8) with a 9MR channel system, while compound 2 (orthorhombic, Pbca (No. 61); a = 9.286(3), b = 12.459(3), c = 21.626(6) A; V = 2502(1) A(3); Z = 8) presents a 3-dimensional open framework structure of different types of intersecting channels. It is worth noting that both the Cl(-) anions and the organic templates play important and interesting roles in the formation of the structures.     

Hydrothermal synthesis and structural characterization of a novel cadmium-organic framework

A three-dimensional diamondoid cadmium-organic framework, formulated as [Cd(NDC)(H₂O)] (I) (where NDC²⁻=2,6-naphtalenedicarboxylate), has been hydrothermally synthesized and structurally characterized using single-crystal X-ray diffraction. The hydrothermal synthesis of I has been optimized by modifying the composition of the reactive mixture and the temperature programme, so that a highly crystalline and pure homogeneous phase could be obtained. A novel layered structure, formulated as [Cd₂(NDC)(OH)₂], was isolated when the molar ratio of triethylamine exceeds ca. 0.7. Both products have been characterized using powder X-ray diffraction, IR and Raman spectroscopies, and elemental and thermal analyses.     

Hydrothermal synthesis and characterization of a novel polyoxometallate-templated three-dimensional supramolecular network

The well-known polyoxomolybdate anion [Mo₈O₂₆]^4? has been used as a noncoordinating anionic template for the construction of a novel three-dimensional (3D) supramolecular network, [Co(phen)₃]₂[Mo₈O₂₆]·?2.5H₂O (1) (phen?=?o-phenanthroline). Compound 1 has been characterized by elemental analyses, IR spectrum, X-ray photoelectron spectroscopy (XPS), TG analysis and single-crystal X-ray diffraction. Single-crystal X-ray diffraction analysis reveals that [Co(phen)₃]²⁺ coordination complexes are packed together via aromatic?π–π?stacking and hydrogen-bonding interactions, and exhibit an interesting 3D supramolecular network with one-dimensional (1D) box-like channels in which the octamolybdate anions reside.     

Microwave-assisted synthesis,characterization and biological activity of novel pyrazole derivatives

A series of 1-(4-substitutedphenyl)-3-phenyl-1H-pyrazole-4-carbaldehydes 4a–l have been synthesized and tested for their biological activities. Formation of the pyrazole derivatives was achieved by treating with Vilsmeier-Haack reagent. The newly synthesized compounds were evaluated for their anti-inflammatory and analgesic activities compared to Diclofenac sodium as standard drug. Compounds 4g, 4i and 4k exhibited the maximum anti-inflammatory and analgesic activities. The detailed synthesis, spectroscopic and toxicity data are reported.     

Hydrothermal synthesis and structural characterization of two 1-D and 2-D Dawson-based phosphotungstates

Two new Dawson-based phosphotungstates (H₂en)_0.5H[Cu(en)₂(H₂O)]₂{[Cu(en)₂](α₁-P₂W₁₇CuO₆₁)}·8H₂O (1) (en=ethylenediamine) and [4,4′-H₂bpy]₂{[Cu(4,4′-bpy)₃][Cu(4,4′-bpy)₄(H₂O)₂]₂[Cu(4,4′-bpy)][α-P₂W₁₈O₆₂]₂}·6H₂O (2) (4,4′-bpy=4,4′-bipyridine) have been hydrothermally synthesized and structurally characterized. 1 crystallizes in the triclinic space group P−1 with a=11.7626(17), b=13.246(2), c=29.350(5) Å, α=87.355(5), β=79.583(5), γ=66.993(3)°, V=4138.3(11) Å³, Z=2, GOF=1.089, R₁=0.0563 and wR₂=0.1505, whereas 2 belongs to the orthorhombic space group Iba2 with a=22.277(8), b=47.04(2), c=22.153(8) Å, V=23215(17) Å³, Z=4, GOF=1.051, R₁=0.0627 and wR₂=0.1477. 1 consists of a 1-D linear chain structure constructed from monocopper^II-substituted Dawson polyoxoanions, while 2 represents the first 2-D sheet-like structure with a (4,4)-connected topological net built up from plenary Dawson-type polyoxoanions and Cu^II-4,4′-bpy complex cations in polyoxometalate chemistry.     

水热合成具有氢键网络的铜咪唑化合物(英文)

本文采用水热合成方法合成了铜(咪唑)化合物,单晶结构表明:该化合物属于三斜晶系,P-1空间群,晶胞参数为:a=0.88097(18)nm,b=0.90812(18)nm,c=1.0586(2)nm,α=75.08(3)°,β=83.14(3)°,γ=61.84(3)°.在化合物中,[Cu(im)6]2+阳离子和Cl-阴离子通过N-H...Cl氢键形成ABAB交叉模式,没有参加配位的水,Cl-离子在水平面形成复杂的氢键网格.本文报道了该化合物的合成、晶体结构、热稳定性、红外及荧光性质.     

Hydrothermal synthesis and structures of two novel chain-like heteropolymolybdate formed by Keggin cluster units

Two novel heteropolymolybdate, [H₂bpy]₂ [Hbpy] [PCuMo₁₁O₃₉]·H₂O 1 and [H₂bpy]₂ [Hbpy] [PZnMo₁₁O₃₉]·2.75H₂O 2, have been prepared under mild hydrothermal conditions and structurally characterized by single-crystal X-ray diffraction. The two compounds are isostructural and crystallize in the monoclinic space group P2(1)/n (No. 14) with a=13.440(3) Å, b=26.660(5) Å, c=15.240(3) Å, β=99.55(3)°, and Z=4 for the compound 1, and a=13.610(3) Å, b=26.781(5) Å, c=15.205(3) Å, β=100.40(3)°, and Z=4 for the compound 2. Compound 1 and 2 exhibit a zigzag chain structure in which Keggin anions are connected through a common oxygen atom. They are the first characterized compounds containing 1D chains of transition-metal substituted Keggin heteropolymolybdate. Other characterizations by elemental analysis, IR, EPR, TG, and XRPD are also described.     

Synthesis,characterization, and physical properties of two novel nonaheteroacene derivatives

Two novel nonaheteroacene derivatives: 24,27,30,33-tetra-tert-butyl-6,8,10,17,19,21-hexaaza-1.22,4.5,11.12,15.16-tetrabenzono-nonaacene (1) and 24,27,30,33-tetra-tert-butyl-6,10,17,21-tetraaza-8,19-benzodioxin-1.22,4.5,11.12,15.16-tetrabenzono-nonaacene (2), have been successfully synthesized through cyclocondensation reactions. The studies on UV–vis and cyclic voltammogram suggest that compound 1 has a smaller bandgap comparing to that of compound 2, indicating that oxygen atoms can destroy the conjugation in compound 2. The results are further confirmed by theoretical simulation.     

氧化铜纳米片的水热合成与表征

利用水热法一步制备了形貌均一的氧化铜纳米片,借助场发射扫描电子显微镜、X射线粉末衍射仪和透射电子显微镜分析了产物的形貌和晶体结构;并研究了反应物浓度及表面活性剂等因素对氧化铜纳米结构的影响.结果表明,以氢氧化钠作为碱源时,在不添加任何表面活性剂的情况下,随着氢氧化钠浓度的升高,纳米片的尺寸减小、厚度增大;此外,通过添加不同的表面活性剂可以得到不同形貌的氧化铜纳米结构.     

三维钒氧化合物的水热合成与表征

利用水热合成的方法,制备了三维钒氧化合物H3V3O9,X射线衍射实验确定了其结构,结果显示,晶体为单斜晶系,P1空间群,晶胞参数为a=4.9980(10)nm,b=8.4188(17)nm,c=7.8614(16)nm,α=90.00°,β=96.40(3)°,γ=90.00°,Z=328.72(11),D=2.999,F(000)=282,R1=0.023 0,wR2=0.0678.通过IR光谱和热重分析对化合物进行了表征.     

具有生物活性的1,4-二氢吡啶衍生物的水热法合成及结构表征

1,4-二氢吡啶衍生物具有很好的生理活性。在医学上用作心血管疾病的防治保健药物,不仅能治疗肠胃疾病、雷诺氏病、脂肪肝、中毒性肝炎,也有抗衰老、防早熟等作用,还可以用作治疗肺动脉高压和癫痫病的辅助药物[1-2]。近年又发现1,4-二氢吡啶衍生物不但是一类高效的钙拮抗剂,亦是一种绿色饲料添加剂。它的合成通常采用文献报道的Hantzsch法合成[3],即将干燥氨气通入乙酰乙酸乙酯与醛的混合溶液中。该反应时间长、操作复杂,且氨气易对环境造成污染。正因为此,越来越多的化学家和药物学家将有机合成的研究重点放在对环境无污染的绿色合成上。如…     

CdS纳米球的水热制备及性质表征

采用水热方法制备了CdS纳米球.通过扫描电镜和透射电镜可以看出:该方法可直接获得具有较好结构的纳米球,比较不同溶剂中得到产品的SEM,发现甘油对CdS纳米球的形成起到了重要的作用.X射线粉末衍射图谱中无杂质衍射峰出现,表明样品为纯的六方相CdS.CdS纳米球的室温光致发光光谱中有2个不同的峰.     

Hydrothermal synthesis,structures and characterization of two new copper(II) triphosphonate compounds

Two copper(II) triphosphonate compounds, Cu[(APTPH₄)(phen)(H₂O)]?·?2.16H₂O (1) and [Cu(APTPH₄)(2,2′-bipy)(H₂O)]?·?2.63H₂O (2), have been prepared by a low temperature hydrothermal reaction from 1-aminopropane-1,1,3-triphosphonic acid (APTPH₆), CuO and a second ligand, phen?=?1,10-phenanthroline, or 2,2′-bipy?=?2,2′-bipyridyl. These two compounds were characterized by single crystal X-ray diffraction, elemental analysis, IR and TG. Crystal data for 1: Monoclinic, space group P2₁ /c, a?=?14.4830(7)?Å, b?=?9.1721(5)?Å, c?=?16.7403(8)?Å, β?=?90.101(2)°. For compound 2: Triclinic, space group P 1, a?=?7.1215(7)?Å, b?=?10.460(2)?Å, c?=?14.671(2)?Å, α?=?82.983(2)°, β?=?83.882(2)°, γ?=?80.617(2)°. In both compounds, each Cu²⁺ ion is five-coordinate with two oxygen atoms from the triphosphonate, two nitrogen atoms from the second ligand and one water molecule, to form a distorted square-pyramidal geometry. Both complexes have 3D supramolecular structures constructed by hydrogen bonds and π–π stacking interactions.     

Practical synthesis of two novel series of 1,3-disubstituted β-carboline derivatives

The synthesis of two novel series of 1,3-disubstituted β-carbolines from 1-aryl-β-carboline-3-carbaldehyde building blocks is reported. In the first case, an efficient synthesis of 1-aryl-β-carboline C-3 tethered tetrahydro-imidazopyridines and their aromatic counterparts was developed. In the second case, the Willgerodt-Kindler three-component reaction was used for the transformation of aldehydes into the corresponding thioamides.     

Hydrothermal synthesis and structural characterization of three reduced phosphomolybdates

Three reduced molybdenum(V) phosphates, Na₂[H₂DaHex]_4.5[H₃O]{Mn[Mo₆O₁₂(OH)₃(HPO₄)₂(PO₄)₂]₂}·2H₂O (1), [H₂DaHex]₄[Zn(H₂O)]₂{Zn[Mo₆O₁₂(OH)₃(HPO₄)₂(PO₄)₂]₂}·6H₂O (2), and [H₂DaHex]_3.5[Cd(H₂O)₂]_1.5[Cd(H₂O)]{Cd[Mo₆O₁₂(OH)₃(HPO₄)₂(PO₄)₂]₂}·3.5H₂O (3) (DaHex?=?1,6-diaminylhexane), were hydrothermally synthesized by using the same organic template (DaHex) and characterized by elemental analysis, IR, TGA, powder XRD, and single-crystal X-ray diffraction. Crystallographic analysis reveals that the compounds contain M[P₄Mo₆]₂ (M?=?Mn for 1, Zn for 2, Cd for 3) polyanions, which are further connected by various metal ions to form different topological structures. In 1, the cluster anion Mn[P₄Mo₆]₂ is discrete. For 2 and 3, M[P₄Mo₆]₂ (Zn for 2, Cd for 3) clusters are linked by transition metal ions to form different infinite chains. Then, all the 1-D chains are further packed into 3-D supramolecular structures via hydrogen-bonding interactions. The formations of 1, 2, and 3 demonstrate that not only organic templates, but transition metal ions also play very important roles in the M-P₄Mo₆ system.     

Hydrothermal synthesis and characterization of a new Anderson-type polyoxometalate

A new compound based on Anderson-type polyoxometalate, [Cu(phen)H₂O]₂[CrH₅Mo₆O₂₄]?·5H₂O (1) (phen?=?1,10-phenanthroline), has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum, and thermal gravimetric analysis. Luminescent, electrochemical, and electroactivity properties of 1 have been studied.     

Hydrothermal syntheses and structural characterization of two sandwich-type arsenotungstates

Two new organic–inorganic composite sandwich-type arsenotungstates [H₂dap]₆H₈[Ni₄(H₂O)₂(B-α-AsW₉O₃₄)₂]₂ · 33H₂O (1) and {[Ni(dap)₂(H₂O)]₂[Ni(dap)₂]₂[Ni₄(Hdap)₂(B-α-AsW₉O₃₄)₂]} · 4H₂O (2) (dap = 1,2-diaminopropane) have been hydrothermally synthesized by reaction of Na₈[A-α-HAsW₉O₃₄] · 11H₂O with NiCl₂ · 6H₂O in the presence of 1,2-diaminopropane and characterized by elemental analysis, IR spectra, X-ray single-crystal diffraction, and thermogravimetric analysis. 1 crystallizes in the triclinic P 1 space group with a = 16.351(6) Å, b = 16.423(6) Å, c = 19.894(7) Å, α = 110.630(6)°, β = 92.684(7)°, γ =104.946(7)°, V = 4774(3) ų, Z = 1, GOOF = 1.033, R ₁ = 0.0517, wR ₂ = 0.1086. 2 also crystallizes in the triclinic P 1 space group with a = 13.305(4) Å, b = 13.882(4) Å, c = 17.031(5) Å, α = 68.109(5)°, β = 71.511(4)°, γ = 88.407(5)°, V = 2753.5(14) ų, Z = 1, GOOF = 1.051, R ₁ = 0.0491, wR ₂ = 0.1150. Notably, 1 is a discrete structure, composed of two tetra-Ni^II substituted sandwich-type polyoxoanions [Ni₄(H₂O)₂(B-α-AsW₉O₃₄)₂]^10? with different spatial orientation, whereas 2 displays a organic–inorganic composite 2-D sheet architecture constructed by tetra-Ni^II sandwiched [Ni₄(H₂O)₂(B-α-AsW₉O₃₄)₂]^10? units by means of [Ni(dap)₂]²⁺ bridges. Some previously reported transition-metal-substituted sandwich-type polyoxotungstates have been summarized.     

Hydrothermal synthesis and characterization of two cobalt phosphates based on double-four-ring units with fluorine-occlusion and phosphite-substitution modifications

Two new fluorinated microporous cobalt phosphates, (H2en)0.5[F(0.25)Co(H(0.5)PO4)0.5(PO4)0.5].0.25H2O (1) and (H2en)0.5[Fx(H2O)0.25(-x)Co(HPO3)x(PO4)1-x].0.25H2O (x = 0.17; 2), have been synthesized from different P sources, H3PO4 and H3PO3, in the presence of ethylenediamine and F ions. Both structures of 1 and 2 are based on the similar secondary building unit of a double four ring (D4R). 1 crystallizes in the orthorhombic space group Cmcm with a = 14.895(1) A, b = 9.7133(9) A, c = 13.688(1) A, V = 1980.4(3) A(3), and Z = 16 and is built up from fully F-occluded double-four-ring units via corner-sharing Co and P polyhedra and edge-sharing Co polyhedra. 2 crystallizes in the tetragonal space group /42m with a = 10.2033(4) A, c = 9.5545(9) A, V = 994.7(1) A(3), and Z = 8 and adopts an ACO-type framework with strict alternation of corner-sharing Co and P polyhedra. On the basis of the evidence from ion chromatography studies and elemental analyses, 2 contains both phosphate and phosphite ions, and the amount of F ions in 2 is the same as the amount of phosphite ions. This implies that some PO4(3-) groups in 2 are substituted by HPO3(2-) groups with the same amount of F(-) occlusion in the center of D4R as charge compensation. Magnetic susceptibility measurements of both 1 and 2 appear that they contain mainly antiferromagnetic interaction (theta = -27.8 K for 1 and -35.0 K for 2). However, the magnetic coupling is much more complicated in compound 1 because of the Co-O-Co linkages in it. Low-field temperature-dependent magnetization curves of 1 showed spontaneous magnetization in the form of two continuous bumps, one sharp and one broad. This may be related to the temperature dependence of two related but different types of spin canting. At 2 K, 1 also showed a large coercive field of about 5000 Oe.