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1.
Abstract

Magnetic nanoparticles containing mesoporous carbon materials have been synthesized via an one-pot strategy associated with a direct carbonization process from resol, metal ion sources (Co(NO3)2·6H2O, Ni(NO3)2·6H2O) and triblock copolymer F127. The samples exhibited well-ordered 2-dimensional (2-D) hexagonal mesostructures with p6mm symmetry. The Brunauer-Emmet-Teller (BET) surface area and pore size 1.0wt%Co- and 1.0wt%Ni-FDU-15(700) with 1.0?wt% Co and 1.0?wt% Ni content were 700, 528 m2/g and 17.2, 36.4 Å, respectively, after carbonization at 700?°C. The saturation magnetization values of 1.0wt%Co- and 1.0wt%Ni-FDU-15(700) after carbonization at 700?°C were 1.3 and 1.0?emu/g, respectively.  相似文献   

2.
The modification of particle surface properties by the addition of small surfactant molecules in the initial sol is one strategy to minimize the strong tendency to aggregation and coarsening of nanoparticles prepared from the sol–gel process. In this work, the effect of the nature of the surfactant, Tiron® ((OH)2C6H2(SO3Na)2 · H2O, anionic) or Catechol® (C6H4-1,2-(OH)2, non-ionic) or Maptac® ([N(CH3)3(CH2)3NHCOC(CH2CH3)]+Cl?, cationic), grafted on the SnO2 nanoparticles on the mesoporosity of powders fired at 600 °C is presented. SnO2 powders were prepared from an one-pot sol–gel route in which the hydrolysis of SnCl4 · 5H2O in aqueous solution was carried out in presence of the surfactant. The Fourier transform infrared (FTIR) spectroscopy and gravimetric and differential thermo-analysis (TG/DTA) results show that the thermo-stability of surface grafted SnO2 nanoparticles obeys the following series: Tiron® > Catechol® > Maptac®. The N2 adsorption isotherms results evidence that the mesopores texture (specific surface area, pore volume and average pore size) can be tuned in a controlled way by increasing the amounts of Tiron® or Catechol® molecules grafted on the surface of SnO2 nanoparticles.  相似文献   

3.

The spectroscopic characterization (1H, 13C{1H} NMR, UV–Vis) and single-crystal X-ray diffraction (scXRD) analysis accomplished by inspection of the Hirshfeld surface of bis(3-thienoyl) disulfide (1) is described. The title compound 1 crystallizes in the monoclinic space group P21/n. The unit cell parameters are a?=?7.9959(3) Å, b?=?6.4348(3) Å, c?=?22.4924(9) Å, β?=?100.108(4)°, V?=?1139.32(8) Å3, Z?=?4, Rgt(F)?=?0.0278, wRref(F2)?=?0.0667. The packing of 1 is dominated by S?O and S?S interactions, giving a 2D layer structure parallel to (101). The X‐ray crystal structure analysis revealed the packing of 1 is dominated by S?O and S?S interactions, giving a 2D layer structure parallel to (101). The intermolecular interactions in 1 were analyzed using the Hirshfeld surface method including 2D fingerprint plots and enrichment ratios (E), which shows that the most favored intermolecular contacts are the O?H and C?S indicated by E values above 1.30. The interaction energies between molecular pairs revealed the importance of the weak O?H and C?S interactions in stabilizing the molecular structure of 1.

Graphic Abstract

Single crystal X-ray structure analysis, DFT calculations and Hirshfeld surface analysis to identify intermolecular interactions within the solid state structure of bis(3-thienoyl) disulfide (1).

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4.
In this paper the synthesis of SnO2 nanoparticles with average particle size up to about 70 nm using SnCl22H2O and NH4OH in 1‐botanol solution by the precipitation method is reported and the inhibition of sodium dodecyl sulphate (SDS) on the SnO2 particle growth is investigated by soaking SnO2precursor in the SDS solution for 24 h. The as‐prepared SnO2and SDS modified‐SnO2 powders, then, were calcined at different temperatures and the X‐ray powder diffraction (XRD) and Fourier transform infrared spectroscopy (FT‐IR) were used to characterize the output samples. The XRD results reveal that the structure of tin‐dioxide is tetragonal rutile and the as‐prepared SnO2 nanoparticles grow with increasing the annealing temperature, while the SDS treatment prevents the particle growth under the same condition. Furthermore, the FT‐IR results indicate the formation of tin‐hydroxyl group which are then converted into tin‐dioxide with heat treatment. Further characterization of the samples by the transmission electron microscopy (TEM) and the photoluminescence (PL) spectroscopy was carried out. The room temperature PL spectra of SnO2exhibits broad and strong peak attributed to the surface defects such as oxygen vacancies and intensity of which decreases with the increase in particle size. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)  相似文献   

5.
Sensing response of ‘self-binding’ nanoparticles of tin dioxide powder deposited on alumina substrate has been investigated. The nanocrystalline SnO2 powder has been derived from stannic chloride. It has been prepared through fine crystallization in liquid phase. SnO2 powder has been characterized using SEM, TEM and XRD techniques, which reveal that the average crystallite size is of 12 nm. The slurry blobs deposited on alumina substrate of the powder-thus-prepared have been studied for sensing response to ethanol at various temperatures and concentrations. The observations reveal that the material prepared is ‘self-binding’ and is very sensitive even without catalyst.  相似文献   

6.
Uranyl triacetate complexes (Cs0.5Ba0.25)[UO2(CH3COO)3] (I) and Ba0.5[UO2(CH3COO)3] (II) are synthesized for the first time and their structures are determined by X-ray diffraction. Both compounds crystallize in the cubic crystal system. The crystal data are as follows: a = 17.3289(7) ?, V = 5203.7(4) ?3, space group I213 and Z = 16 (I); a = 17.0515(8)?, V = 4957.8(4) ?3, space group I $ \bar 4 $ \bar 4 3d, and Z = 16 (II). In I and II, as in all uranyl triacetates studied earlier, the coordination polyhedron of the uranium atom is a hexagonal bipyramid whose vertices are occupied by the oxygen atoms of the uranyl and three acetate groups. The uranium-containing group belongs to the AB 301 (A = UO22+, B 01 = CH3COO) crystal chemical group of uranyl complexes. It was found that compound II is isostructural to the (Rb0.50Ba0.25)[UO2(CH3COO)3] studied earlier.  相似文献   

7.
Abstract

A new preparation method of the fibrous organic-inorganic nanohybrids was established by the reaction of Zn(OH)2 with various organic carboxylic acids. Interlayer spacings of the reaction products of Zn(OH)2 with benzoic acid and p-phenyl azobenzoic acid were 1.46 and 2.04 nm, and these reaction products have layered structure. In IR spectra, new peaks of RCOO-Zn band appeared at around 1400 cm?1 and 1550 cm?1 indicating that hydroxyl groups reacted with organic carboxylic acids. SEM images of these reaction products showed fibrous morphology. The TEM image showed that the layer structure was constructed along the fiber direction.  相似文献   

8.
Two 1D polymeric complex, [Cu(CBC)2(Dabco)(H2O)] n (1) and [Ag2(HBC)2(Dabco)] n (2) have been synthesized and characterized by X-ray single crystal analysis, where CBCH is p-chlorobenzoic acid, HBCH 2 is 2-hydroxybenzoic acid and Dabco is 1,4-diazabicyclo[2.2.2]octane. Complex 1 has been obtained in high yield by hydrothermal synthesis from CuO and CBCH and Dabco, and complex 2 has been obtain by evaporation of the solvent from silver salicylate and Dabco, 1 crystallizes in the orthorhombic space group Pmn2 1 with a = 24.3310(5) ?, b = 6.9050(6) ?, c = 5.9980(5) ?, Z = 2, V = 1007.70(4) ?3 and Dx = 1.657 g cm−3, 2 crystallizes in the monoclinic space group P2 1 /m with a = 10.292(3) ?, b = 6.913(2) ?, c = 14.417(4) ?, β = 95.660(5), Z = 2, V = 1020.8(5) ?3 and Dx = 1.959 g cm−3. The final R value is 0.0302 for 1323 measured reflections for 1 and the final R value is 0.0684 for 1545 measured reflections for 2. The atomic arrangement is built by infinite one-dimensional polymeric chain in both complexes. These chains are cross-linked by hydrogen bonds involving the coordinated water molecules to form a two-dimensional framework in complex 1.  相似文献   

9.
The synthesis and X-ray structure analysis of Sn2(HL)Cl · H2O, where HL 3? is the anion of 1-hydroxyethane-1,1-diphosphonic acid, are reported. The coordination polyhedra of two independent tin(II) atoms are the Sn(1)O2Cl and Sn(2)O3 trigonal pyramids, in which one of the vertices is occupied by a lone electron pair (Sn-O, 2.144–2.218 Å and Sn-Cl, 2.573 Å). The pyramids are complemented by weaker Sn?O and Sn?Cl contacts to form severely distorted (3 + 3) octahedra. The SnO2Cl and SnO3 pyramids are linked by the HL 3? bridging ligands into the [Sn2(HL)Cl]6 cyclic molecules, which, in turn, are joined by additional Sn?O, Sn?Cl, O(H2O)?O(L), and O(H2O)?Cl contacts with each other and with crystallization water molecules into a three-dimensional framework.  相似文献   

10.
The first titled compound, 1, was obtained by treating [Ru(bpy)(η2-tpy)(CO)CH2OH]PF6 with acetic anhydride. Heating 1 in acetonitrile afforded 2, [Ru((η3-tpy)(MeCN)(CO) CH2OAc]PF6. Allowing 2 to stand in CH2Cl2 followed by concentration and precipitation afforded the second titled compound, 3 ([Ru((η3-tpy)(CO)–CH2OAc]PF6), in which the acetoxymethyl group had become bidentate. Crystal data for 1, monoclinic crystal system, space group C2/c, a=26.001(4) ?, b=13.0395(18) ?, c=20.718(3) ?, β=107.700(2)°, V=6691.7(16) ?3, Z=8; for 3, monoclinic crystal system, space group P21/n, a=10.864(2) ?, b=16.922(4) ?, c=11.127(2) ?, β=90.907(3)°, V=2045.4(8) ?3, Z=4.  相似文献   

11.
The molecular bis(2-N-H-pyrrolylcarbaldimine)nickel(II) and palladium(II) complexes are isolated in moderate yield (30–35%) from in situ assembly of the Schiff base with metal(II) salt, base, and pyrrole-2-carbaldehyde in aqueous ammonia solution. The nickel(II) complex, 1, is monoclinic, space group P21/c, with a=11.289(6) ?, b=5.611(3) ?, c=8.287(5) ?, β=111.620(6)°, and V=488.0(5) ?3 with Z=2, for d calc=1.667 Mg/m3. The palladium analog, 2, is isomorphous, space group P21/c, with a=11.481(3) ?, b=5.5738(10) ?, c=8.276(2) ?, β=110.923(12)°, and V=494.7(2) ?3 with Z=2, for d calc=1.965 Mg/m3. In both crystal structures, the metal resides on an inversion center. In the IR spectra, ν(C=N) appears at 1561 cm−1 in 1, and 1557 cm−1 in 2, while ν(N–H) shows at 3345 cm−1 and 3335 cm−1, respectively. The 1H-nmr spectra reveal the C–H and N–H protons of the imine group as sharp and broad doublets, respectively, at 7.62 and 8.38 δ in 1 and at 7.92 and 9.73 δ in 2.  相似文献   

12.
Two complexes (H2bipy)[M2(TB)2(H2O)8]·5H2O (M = Mn 1, Zn 2) (bipy = 4,4′-bipyridine, H3TB = 1,3,5-tris(carboxymethoxyl)benzene) were synthesized by the reaction of the corresponding metal salt with ligand H3TB and 4,4′-bipy in an aqueous methanol solution at room temperature, respectively. Their structures were determined by single crystal X-ray diffraction analysis. Both complexes 1 and 2 crystallize in the triclinic space group with the crystal parameters of 1: a = 9.725(12) ?, b = 10.651(13) ?, c = 10.882(13) ?, α = 91.72(2)°, β = 96.41(2)°, γ = 97.72(2)°, V = 1109(2) ?3, Z = 1 and 2: a = 9.610(10) ?, b = 10.55(2) ?, c = 10.83(2) ?, α = 91.60(4)°, β = 95.32(2)°, γ = 97.73(4)°, V = 1082(3) ?3, Z = 1. Complexes 1 and 2 have the same dinuclear structure, in which each metal atom is six coordinated with distorted octahedral geometry by two oxygen atoms from two different TB3− ligands and four ones from four coordinated water molecules. The dinuclear units are further linked by hydrogen bonding and π–π interactions to form the three-dimensional framework structure.  相似文献   

13.
Two new nickel(II)(cyclen) coordination polymers, {[Ni(cyclen)·(bipy)]·(ClO4)2}n (1) and [Ni(cyclen)]2·(squa)·(ClO4)2 (2) have been synthesized and characterized structurally, where cyclen is 1,4,7,10-tetraazadodecane. Compound 1 crystallizes in the monoclinic system, space group C2/c, with a = 10.5339(17) ?, b = 14.565(2) ?, c = 16.133(3) ?, β = 102.799(2)°, V = 2413.4(7) ?3. Compound 2 crystallizes in the orthorhombic system, space group P nm a with a = 25.722(3) ?, b = 11.1168(12) ?, c = 11.4580(13) ?, V = 3276.3(6) ?3. In both compounds, each NiII center is in a distorted octahedral coordinated environment with four Ncyclen atoms and two Npyridine atoms from 4,4′-bipyridine linker for 1 and two Oaqueou atoms from the coordinated water for 2, respectively. The complex 1 exhibits infinite zigzag 1D chains by linking of 4,4′-bipyridine coordinated. In complex 2, 2D sheet supramolecule generated through self-assembling by hydrogen bond.  相似文献   

14.
Abstract

Two new semiconducting organic small molecules, namely BDTQ-BDT(EH) and BDTQ-BDT(OC), were prepared by attaching electron accepting 2,3-didodecyl-6,7-difluoro-5,8-di(thiophen-2-yl)quinoxaline (DTQ) unit on 2,6-position of electron donating 4,8-bis(2-ethylhexyloxy)benzo[1,2-b:4,5-b']dithiophene (BDT(EH)) and 4,8-bis(octyloxy)benzo[1,2-b:4,5-b']dithiophene (BDT(OC)) units. Molecule BDTQ-BDT(EH) showed higher thermal stability (5% weight loss temperature, Td “349 оC), slightly lower band-gap (Eg “2.10?eV) and deeper highest occupied molecular orbital energy level (HOMO “–5.36?eV) level compared to those (Td “336 оC, Eg “2.11?eV, and HOMO “–5.30?eV, respectively.) of the molecule BDTQ-BDT(OC). The organic solar cells (OSCs) made with the synthesized molecules as an electron donor and [6,6]-phenyl C71 butyric acid methyl ester (PC70BM) as an electron acceptor gave a maximum power conversion efficiency (PCE) of 1.20% and 0.83%, respectively, for BDTQ-BDT(EH) and BDTQ-BDT(OC). This study confirmed that the substituents attached on the 4,8-position of BDT unit greatly alter the properties of the resulting molecules.  相似文献   

15.

Abstract  

The reaction of [Ni(L)]Cl2·2H2O (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.18,07.12]docosane) with pyrazine-2-carboxylic acid (H-pyc) yields mononuclear nickel(II) complex, [Ni(L)(pyc)2]·2H2O (1). This complex has been characterized by X-ray crystallography, electronic absorption and cyclic voltammetry. The crystal structure of 1 exhibits a distorted octahedral geometry with four nitrogen atoms of the macrocycle and two pyrazine-2-carboxylate ligands. It crystallizes in the triclinic system P-1 with a = 9.6643(17), b = 10.116(3), c = 16.99(4) ?, V = 1633(3) ?3, Z = 2. Electronic spectrum of 1 also reveals a high-spin octahedral environment. Cyclic voltammetry of 1 undergoes two waves of a one-electron transfer corresponding to NiII/NiIII and NiII/NiI processes.  相似文献   

16.
Silica samples with embedded SnO2 nanoparticles have been produced by sol–gel method with a synthesis modified by the introduction of fluorinated silicon precursors. The structural features of silica network and SnO2 nanophase have been mapped inside the samples by means of confocal micro-Raman scattering spectroscopy. The results show that the detection of residual fluorine into the matrix as Si–F groups is accompanied by network dehydration, by intensity depletion of the D2 peak assigned to three-member rings of coordinated tetrahedra, and by SnO2 nanoparticles with much larger sizes than in fluorine-free material.  相似文献   

17.
The title compounds 3,3,6,6-tetramethyl-9-(2,4-dichlorophenyl)-3,4,6,7,9,10-hexahydro-2H,5H-acridine-1,8-dione 1 (C23H25Cl2NO2, Mr = 418.34) and 3,3,6,6-tetramethyl-9,10-di(4-methoxy-phenyl)-3,4,6,7,9,10-hexahydro-2H,5H-acridine-1,8-dione 2 (C31H35NO4, Mr = 485.60) were synthesized and crystallized. The crystals of compound 1 are monoclinic, space group P21/c, a = 9.826(3), b = 19.866(5), c = 11.471(3) ?, β = 111.929(4)°, Z = 4, V = 2077(1) ?3; The compound 2 crystallizes in space group P21/c, with cell parameters a = 12.089(2), b = 11.447(2), c = 19.742(3) ?, β = 101.00(1)°, V = 2681.8(8) ?3 and D calc = 1.203 g/cm3 for Z = 4. X-ray analysis reveals that atoms C(1), C(6), C(7), C(8), C(13) and N(1) form a 1,4-dihydropyridine ring in compound 1, which adopts half-chair conformation. In compound 2 the atoms C(1), C(6), C(7), C(8), C(13) and N form a 1,4-dihydropyridine ring which adopts boat conformation. In addition, the two outer six-membered rings display half-chair conformations in the crystal structures 1 and 2.  相似文献   

18.
The single crystal structure of NH4[UO2(CH3COO)3] (I), K[UO2(CH3COO)3] (II), and Cs[UO2(CH3COO)3] (III) is studied by X-ray diffraction. I and II crystallize in the tetragonal crystal system. The crystal data are as follows: a = 13.6985(3) and c = 27.5678(14) ?, V = 5173.1(3) ?3, space group I41/a, Z = 16, and R = 0.023 for I; a = 13.8890(5) and c = 26.0839(18) ?, V = 5031.7(4) ?3, space group I41/a, Z = 16, and R = 0.037 for II. Crystals III are orthorhombic, a = 18.176(2), b = 13.119(2), and c = 22.088(4) ?, V = 5267(1)?3, space group Pbca, Z = 16, and R = 0.0424. In structures I–III, the uranium-containing structural units are represented by discrete mononuclear [UO2(CH3COO)3] groups, which belong to the AB 301 (A = UO22+, B 01=CH3COO) crystal chemical group of uranyl complexes.  相似文献   

19.
Abstract The synthesis of the PPN (PPN=Ph3P=N=PPh3) salt of di-μ-iodo-dichlorocuprate (I) anion [Cu2I2Cl2]2− is described and the crystal and molecular structures of this compound are reported. It was found that the compound has the formula [PPN]2[Cu2I2Cl2]0.7[Cu2I4]0.3 (3). Compound 3 crystallizes in an orthorhombic crystal system, space group Pbca, with a = 19.654(3), b = 16.130(2), c = 20.108(3) ?, V = 6374.3(16) ?3 and Z = 4. The crystal contains 70% [Cu2I2Cl2]2− anions and 30% [Cu2I4]2− anions. This was also confirmed by MSES spectroscopy. The anion [Cu2I2Cl2]2− is planar and the Cu atoms have a trigonal planar configuration. Graphical abstract Synthesis and Crystal Structure of the Salt [PPN + ] 2 [Cu 2 I 2 Cl 2 ] 2− Andrey A. Yakovenko, Tatiana V. Timofeeva and Mikhail Yu. Antipin The title compound was synthesized and structurally investigated. The crystal contains 70% [Cu2I2Cl2]2− anions and 30% [Cu2I4]2− anions. This was confirmed by MS ES spectroscopy.   相似文献   

20.
Three Sr2+ compounds with the Edta 4− and H2 Edta 2− ligands—Sr2(Edta) · 5H2O (I), Sr2(H2 Edta)(HCO3)2 · 4H2O (II), and Sr2(H2 Edta)Cl2 · 5H2O (III)—are synthesized, and their crystal structures are studied. In I, the Sr(1) atom is coordinated by the hexadentate Edta 4− ligand following the 2N + 4O pattern and by two O atoms of the neighboring ligands, which affords the formation of zigzag chains. The Sr(2) atom forms bonds with O atoms of five water molecules and attaches itself to a chain via bonds with three O atoms of the Edta 4− ligands. The Sr(1)-O and Sr(2)-O bond lengths fall in the ranges 2.520(2)–2.656(3) and 2.527(3)–2.683(2) ?, respectively. The Sr(1)-N bonds are 2.702(3) and 2.743(3) ? long. In II and III, the H2 Edta 2− anions have a centrosymmetric structure with the trans configuration of the planar ethylenediamine fragment. The N atoms are blocked by acid protons. In II, the environment of the Sr atom is formed by six O atoms of three H2 Edta ligands, two O atoms of water molecules, and an O atom of the bicarbonate ion, which is disordered over two positions. In III, the environment of the Sr atom includes six O atoms of four H2 Edta 2− ligands and three O atoms of water molecules. The coordination number of the Sr atoms is equal to 8 + 1. In II and III, the main bonds fall in the ranges 2.534(3)–2.732(2) and 2.482(2)–2.746(3) ?, whereas the ninth bond is elongated to 2.937(3) and 3.055(3) ?, respectively. In II, all the structural elements are linked into wavy layers. The O-H…O interactions contribute to the stabilization of the layer and link neighboring layers. In III, hydrated Sr2+ cations and H2 Edta anions form a three-dimensional [Sr2(H2 Edta)(H2O)3] n 2n+ framework. The Cl anions are fixed in channels of the framework by hydrogen bonds with four water molecules. In II and III, the N-H groups form four-center N-H…O3 hydrogen bonds, which include one intermolecular and two intramolecular components. PACS numbers: 61.66.Hq Original Russian Text ? I.N. Polyakova, A.L. Poznyak, V.S. Sergienko, 2009, published in Kristallografiya, 2009, Vol. 54, No. 2, pp. 262–267.  相似文献   

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