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1.
以乙酰二茂铁和氨基三氮唑为原料,合成了两种新型的二茂铁三氮唑Sch iff碱化合物,其结构通过IR,1H-NMR,元素分析和X-射线单晶衍射法确定。X射线单晶结构分析表明,固态时化合物1 a与一分子水通过分子间氢键形成-维无限链状结构,其晶体属单斜晶系,P21/n空间群,M r:312.16,a=11.679(2),b=9.862(2),c=12.717(3),β=108.60(3)0k,v=1388.3(5),Z=4,D c=1.493mg.m-3,μ=0.71073,F(000)=648,最终偏离因子R=0.0454,wR=0.0984。电化学分析表明1 a和1b的电化学性质相似,在电位0.4~1.1V范围内,都只有一对氧化-还原峰,对应于Fc/Fc 电对,且该过程是受扩散控制的可逆过程。 相似文献
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近年来 ,二茂铁金属有机液晶材料因其特异的液晶性能和较高的应用价值 ,引起了人们广泛的研究兴趣 ,得到了迅速的发展 ,使该类液晶材料的种类不断增加[1~ 4] 。本文报道的二茂铁衍生物是一个含有苯基、酯基和Schiffs的金属有机化合物 ,是一种潜在的金属有机液晶材料 ,其合成路线如下 :1 实验1 1 仪器与试剂仪器 :显微熔点测定仪。核磁共振仪为RraKerAVANCE - 30 0G型 ,TMS作为内标。红外光谱仪为Perkin Elmer1 730型 ,KBr压片。单晶测定仪为SiemensP4型衍射仪。试剂均为国产化学纯。1 2… 相似文献
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Kohei Okubo Kouki Oka Keiho Tsuchiya Atsunori Tomimoto Norimitsu Tohnai 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2024,136(15):e202400475
Porous organic salts (POSs) are organic porous materials assembled via charge-assisted hydrogen bonds between strong acids and bases such as sulfonic acids and amines. To diversify the network topology of POSs and extend its functions, this study focused on using 4,4′,4′′,4′′′-(9,9′-spirobi[fluorene]-2,2′,7,7′-tetrayl)tetrabenzenesulfonic acid ( spiroBPS ), which is a tetrasulfonic acid comprising a square planar skeleton. The POS consisting of spiroBPS and triphenylmethylamine ( TPMA ) ( spiroBPS/TPMA ) was constructed from the two-fold interpenetration of an orthogonal network with pts topology, which has not been reported in conventional POSs, owing to the shape of the spirobifluorene backbone. Furthermore, combining tris(4-chlorophenyl)methylamine ( TPMA-Cl ) and tris(4-bromophenyl)methylamine ( TPMA-Br ), which are bulkier than TPMA owing to the introduction of halogens at the p-position of the phenyl groups with spiroBPS allows us to construct novel POSs ( spiroBPS/TPMA-Cl and spiroBPS/TPMA-Br ). These POSs were constructed from a chiral helical network with pth topology, which was induced by the steric hindrance between the halogens and the curved fluorene skeleton. Moreover, spiroBPS/TPMA-Cl with pth topology exhibited circularly polarized luminescence (CPL) in the solid state, which has not been reported in hydrogen-bonded organic frameworks (HOFs). 相似文献
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XuChun Wang JieYing Wu HongPing Zhou YuPeng Tian Lin Li JiaXiang Yang BaoKang Jin ShengYi Zhang 《中国科学B辑(英文版)》2009,52(7):930-936
Two new metal-centered ferrocene complexes Ni(SCN)2(L)4 (1) and Cu(OAc)2(L)2 (2) (L = 1-[1-ferro- cenylmethyl]imidazole) have been synthesized and characterized by elemental analysis, single crystal X-ray diffraction analysis, spectroscopic and cyclic voltammetric measurements. The geometry of Ni(Ⅱ) in 1 is octahedral, with four ligands in the equatorial plan and two thiocyanate anions at the axial site, while that of Cu(Ⅱ) in 2 is a distorted octahedron formed by two chealted OAc- and two ligands. Single c... 相似文献
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Synthesis,CrystalandMolecularStructureof1,1'-Bis(N-phenylhydroxyaminocarbonyl)ferrocene¥ZhangWen;LiFeng-Ze;LiuQi-Wang(Departm... 相似文献
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A coordination polymer of [Zn(BBP)(p-CPOA)]n(where BBP is 2,6-bis(benzimidazolyl)pyridine and p-CPOA is p-carboxylato-phenoxyacetate dianion) has been synthesized and characterized by elemental analysis, IR, TG, and the single crystal structure was determined by X-ray diffraction. The crystal crystallizes in the monoclinic system, space group of P21/n with a=1.397 3(4) nm, b=1.138 4(3) nm, c=1.575 9(5) nm, β=91.805(1)°, V=2.505 4(13) nm3, Z=4, Dc=1.513 g·cm-3, μ=1.030 mm-1 and F(000)=1 168. Zn(Ⅱ) ion is penta-coordinated and surrounded by two carboxylate O atoms from two different p-CPOA groups in a bis-monodentate mode, three N atoms from the 2,6-bis(benzimidazolyl)pyridine ligand, completing a distorted trigonal bipyramidal coordination configuration. The structure is a helix with a long pitch of 1.138 4 nm. Under direction of supramolecular recognition and attraction, the adjacent chains are formed the double-stranded chain through π-π stacking between the 2,6-bis(benzimidazolyl)pyridine ligands and hydrogen-bonding interactions. A three-dimensional supramolecular network is further constructed through these interactions between the helices. The TG shows that its chain skeleton is thermally stable up to 382 ℃. CCDC: 626650. 相似文献
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HUANG Zun-Xing WANG Xiu-Li LIU Shi-Xiong 《结构化学》2002,21(5):505-508
1 INTRODUCTION Transition metal complexes with ferrocene are of considerable interest in the past fifty years because of their novel structures and special properties[1, 2]. The chemistry of ferrocene and its derivatives has become richer and richer in the last decade. Many complexes containing ferrocenyl have been synthesized and characterized[3~5]. Recently we have reported the synthesis and crystal structure of dibromo[1,1?bis(diphenylphosphino)- ferrocene]cadmium (Ⅱ)[6]. Herein we… 相似文献
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《应用有机金属化学》2017,31(7)
tert ‐Butyl‐1′‐methoxycarbonyl‐1‐ferrocenecarbamate ( 1 ) was Boc‐deprotected to give free amine which underwent oxalyl chloride‐mediated dimerization. The structure of the so‐obtained oxalamide‐bridged ferrocene 2 was elucidated using infrared and NMR (1H, 13C, COSY, NOESY, HSQC, HMBC) spectroscopies, crystal structure analysis, and electrospray ionization and high‐resolution mass spectrometry. The preliminary conformational analysis in solution suggested the intramolecular engagement of oxalamide protons, while single‐crystal analysis revealed an intermolecular hydrogen‐bonding pattern. Also, the effect of oxalamide‐bridged ferrocene 2 on cell viability of three human cell lines (HEK293T, HeLa and HepG2) was tested. In vitro screening revealed proliferative as well as cytotoxic effects of the tested compound in the applied concentration range (1–350 μM) on HEK293T and HepG2 cells. Stimulatory effect on cell growth was the most pronounced for normal HEK293T cells, while the highest cytotoxic effect was observed towards HeLa tumour cells and it was dose‐dependent. The observed dual biological activity of 2 implies its potential application in drug development. 相似文献
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We review in this short perspective the history of cholesterol crystals and crystal structures. We address in particular the helical crystals that form in vitro and in pathology from environments rich in bile acids or from phospholipid membranes. We review the known mechanisms leading to crystals with chiral morphology, from screw-dislocation mediated growth to mechanisms involving asymmetric mechanical strain. We propose a mechanism for cholesterol helical crystal development based on the monoclinic cholesterol monohydrate crystal structure. We suggest that curvature arises in few layers thick crystals due to the tension induced between the hydrophobic layer and the ice-like H-bonded lattice of the water molecules with the cholesterol hydroxy groups. Helicity would ensue through a combination of the curvature and the fast growth of a thin ribbon in one crystal direction. 相似文献
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A. Eceiza 《European Polymer Journal》2005,41(12):3051-3059
This third paper in this series regarding the mechanism and kinetics of urethane systems presents the results obtained in the study of the influence of molecular weight and chemical structure of several polycarbonate diols on the polycondensation reaction with 4,4′-diphenylmethane diisocyanate (MDI), comparing them with those obtained previously for condensation reaction with p-tolyl isocyanate (p-TI). The substitution effect induced in the second isocyanate group by the reaction of the first isocyanate group of a symmetric diisocyanate likes MDI has been studied by size exclusion chromatography (SEC) using a model monoalcohol. The condensation reaction kinetics is adequately described by an autocatalyzed third order rate equation. The values obtained for rate constants, using a Runge-Kutta mathematical model, suggest association phenomena by hydrogen bonding implying hydroxyl groups but also urethane groups. In bulk and in stoichiometric conditions, the association phenomena observed increase proportionally on one hand, to the decrease of molecular weight of macrodiol and on the other hand, to the tendency to form intramolecular hydrogen bonds. The activation energies were obtained from the evaluation of kinetic data at different temperatures in the range 45-65 °C. As association phenomena increase, activation energies decrease. The slightly higher activation energies obtained for polycondensation compared to condensation are explained because of the rapid increase of viscosity of the medium. 相似文献
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Two inclusion compounds of dithiobiurea and tetrapropylammonium and tetrabutylammonium are characterized and reported, namely tetrapropylammonium carbamothioyl(carbamothioylamino)azanide, C12H28N+·C2H5N4S2−, (1), and tetrabutylammonium carbamothioyl(carbamothioylamino)azanide, C16H36N+·C2H5N4S2−, (2). The results show that in (1), the dithiobiurea anion forms a dimer via N—H...N hydrogen bonds and the dimers are connected into wide hydrogen‐bonded ribbons. The guest tetrapropylammonium cation changes its character to become the host molecule, generating pseudo‐channels containing the aforementioned ribbons by C—H...S contacts, yielding the three‐dimensional network structure. In comparison, in (2), the dithiobiurea anions are linked via N—H...S interactions, producing one‐dimensional chains which pack to generate two‐dimensional hydrogen‐bonded layers. These layers accommodate the guest tetrabutylammonium cations, resulting in a sandwich‐like layer structure with host–guest C—H...S contacts. 相似文献
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The diol host compound 2 has been synthesised and its behaviour to form crystalline inclusion compounds is discussed in comparison with an analogous ethynylene spaced host compound 1. The rotation around the fluorenol–anthracene bonds in 2 is highly restricted as indicated by solution NMR spectroscopy, molecular mechanics and semi-empirical calculations. Single-crystal X-ray structures of the inclusion complexes of 2 with 1-BuOH (2a), morpholine/H2O (2b) and DMSO (2c) are in agreement with the bent geometry of the anthracene ring system suggested by the calculations. The structures exhibit specific modes of hydrogen bond interactions. 相似文献
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1 INTRODUCTIONTheα ,α ,α′,α′ tetraaryl 1 ,3 dioxolane 4,5 dimethanols (TADDOLS)diolswhicharereadilyavailablefromalkyltartrates ,havebeenwidelyusedaschiralligandsinenantioselectiveadditionreactionsofcarbon centerednucleophilestoaldehy des[1 ] ,in [2 +2 ]cycloadditions[2 ] … 相似文献
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de Souza A. C. Pires A. T. N. Soldi V. 《Journal of Thermal Analysis and Calorimetry》2002,70(2):405-414
Thermogravimetric data and the kinetic interpretation of the curves of mass loss for ferrocene, ferrocenecarboxylic and ferrocenedicarboxylic
acids and a series of ferrocene-containing polyamides are presented. The results indicate that the degradation process occurred
with more than one stage of thermal degradation. The apparent activation energy values and the FTIR spectra of the degradation
products suggest that the degradation mechanism occurred by either scission of weak links or by random scission of the chain.
Apparently, the N-vicinal methylene group was the primary site of attack of oxygen on the polymer chain.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
19.
Vladimir B. Arion Alexey A. Nazarov Christian G. Hartinger Gerald Giester Bernhard K. Keppler 《应用有机金属化学》2003,17(9):723-724
For the unsymmetrical title compound, 1‐bromo‐1′‐[(2S)‐N‐(1‐hydroxy‐3‐methylbutane‐2‐yl)]‐ferroceneamide, two independent molecules were found in the asymmetric unit. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
20.
Ingeborg Csöregh Mátyás Czugler Anne Ertan Edwin Weber Jochen Ahrendt 《Journal of inclusion phenomena and macrocyclic chemistry》1990,8(3):275-287
The crystal structures of four dimethyl sulphoxide (DMSO) inclusion compounds with different carboxylic acid hosts,1–4, have been studied by single crystal X-ray analysis. Crystals of thetrans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid inclusion compound (1a), [1 · DMSO (1: 1)] show monoclinic (P21/n) symmetry with the unit cell dimensionsa = 11.522(4),b = 18.658(2),c = 8.709(1) Å and = 98.92(2)°. The clathrate of the 9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid (2a), [2 · DMSO (1: 2)] is triclinic (P) with the cell dimensionsa = 15.043(7),b =9.657(4),c = 8.118(7) Å, = 101.81(5), = 96.05(4) and = 100.04(4)°. Triclinic (P) symmetry is shown also by the inclusion compound of 9,10-dihydro-9,10-ethanoanthracene-11-monocarboxylic acid (3a) [3 · DMSO (1:1)] with the cell dimensionsa=6.3132(1),b=7.9846(2),c=17.5314(4) Å, = 96.46(2), = 87.08(2) and = 106.02(2)°. The 9,9-bianthryl-2-monocarboxylic acid clathrate (4a) [4 · DMSO (1:1)] is monoclinic (P21/n) and the cell dimensions area = 19.625(18),b = 8.817(1),c = 14.076(8) Å and = 97.92(6)°. In all these structures, the hosts show the same basic recognition pattern for the DMSO guest, involving a strong O-H ... O bond from the COON to the S=O group, and a possible C-H ... O type interaction between the carbonyl O atom of the host and a CH3 group of the guest. The crystals consist of discrete host-guest aggregates which are mainly held together by weak intermolecular interactions of the Van der Waals' type. The stoichiometries of the aggregates are, however, different. 相似文献