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1.
X‐ray absorption fine structure study on the role of solvent on polymerization of 3‐hexylthiophene with solid FeCl3 particles
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Tomoyasu Hirai Masanao Sato Makoto Kido Yusuke Nagae Katsuhiro Kaetsu Yudai Kiyoshima Shota Fujii Tomoyuki Ohishi Kevin L. White Yuji Higaki Yasutake Teraoka Maiko Nishibori Kazutaka Kamitani Kenji Hanada Takeharu Sugiyama Ryuichi Sugimoto Kazuhiko Saigo Ken Kojio Atsushi Takahara 《Journal of polymer science. Part A, Polymer chemistry》2015,53(18):2075-2078
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《应用有机金属化学》2017,31(10)
We describe the reaction of anion [RhCl6]3− with a series of hydantoin ligands (HL1, HL2 and HL3 = 5‐methyl‐5‐(2‐, 3‐ and 4‐pyridyl)‐2,4‐imidazolidenedione, respectively). Based on spectroscopic, cyclic voltammetric, elemental and MS analyses, the complexes have the general formula K[RhCl2(L1)2] ( 1 ), cis ‐ and trans ‐K[RhCl4(HL2)2] ( 2a and 2b ) and cis ‐ and trans ‐K[RhCl4(HL3)2] ( 3a and 3b ). Complexes 2a , 2b , 3a and 3b were characterized successfully using infrared, 1H NMR and 13C NMR spectral analyses. Dissolution of complex 1 in dimethylsulfoxide (DMSO) led to elimination of one KL1 ligand and coordination of two DMSO molecules as ligands and transformation of this complex to cis ‐ and trans ‐[RhCl2L1(DMSO)2] ( 1a and 1b ). Recrystallization led to separation and isolation of crystals of 1a from the initial mixture. X‐ray analysis results showed that this complex was crystallized as solvated complex cis ‐[RhCl2L1(DMSO)2]DMSO. The catalytic activity of these complexes was then evaluated for the hydrogenation of various ketones. 相似文献
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Fe K‐Edge X‐ray Absorption Fine Structure Determination of γ‐Al2O3‐Supported Iron‐Oxide Species
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Dr. Atsuko Tomita Dr. Takeshi Miki Takeru Tango Tatsuro Murakami Hideyuki Nakagawa Dr. Yutaka Tai 《Chemphyschem》2015,16(9):2015-2020
The structure of FeOx species supported on γ‐Al2O3 was investigated by using Fe K‐edge X‐ray absorption fine structure (XAFS) and X‐ray diffraction (XRD) measurements. The samples were prepared through the impregnation of iron nitrate on Al2O3 and co‐gelation of aluminum and iron sulfates. The dependence of the XRD patterns on Fe loading revealed the formation of α‐Fe2O3 particles at an Fe loading of above 10 wt %, whereas the formation of iron‐oxide crystals was not observed at Fe loadings of less than 9.0 wt %. The Fe K‐edge XAFS was characterized by a clear pre‐edge peak, which indicated that the Fe?O coordination structure deviates from central symmetry and that the degree of Fe?O?Fe bond formation is significantly lower than that in bulk samples at low Fe loading (<9.0 wt %). Fe K‐edge extended XAFS oscillations of the samples with low Fe loadings were explained by assuming an isolated iron‐oxide monomer on the γ‐Al2O3 surface. 相似文献
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Takayoshi Yamaguchi Kohei Komoriyama Yutaka Ohkoshi Hiroshi Urakawa Yasuo Gotoh Norihisa Terasawa Masanobu Nagura Kanji Kajiwara 《Journal of Polymer Science.Polymer Physics》2005,43(9):1090-1099
Fiber‐structure‐development in the poly(ethylene terephthalate) fiber drawing process was investigated with online measurements of wide‐angle and small‐angle X‐ray scattering with both a high‐luminance X‐ray source and a CO2‐laser‐heated drawing system. The intensity profile of the transmitted X‐ray confirmed the location of the neck‐drawing point. The diffraction images had a time resolution of several milliseconds, and this still left much room for improvement. Crystal diffraction appeared in the wide‐angle X‐ray images almost instantaneously about 20 ms after necking, whereas a four‐point small‐angle X‐ray scattering pattern appeared immediately after necking. With the elapse of time after necking, the four‐point scattering pattern changed into a meridional two‐point shape. © 2005 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 43: 1090–1099, 2005 相似文献
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Mononuclear Co(III), Ni(II) and Cu(II) complexes of tridentate di‐tert‐butylphenylhydrazone: Synthesis,characterization, X‐ray crystal structures,Hirshfeld surface analysis,molecular docking and in vivo anti‐inflammatory activity
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Geeta H. Chimmalagi Umashri Kendur Sunil M. Patil Kalagouda B. Gudasi Christopher S. Frampton Mahantesh B. Budri Chandrashekhar V. Mangannavar Iranna S. Muchchandi 《应用有机金属化学》2018,32(6)
A new hydrazone (LH2) derived from the condensation of 2‐(4‐fluorobenzamido)benzohydrazide with 3,5‐di‐tert‐butyl‐2‐hydroxybenzaldehyde was used to synthesize Co(III), Ni(II) and Cu(II) complexes. These were characterized using various physicochemical, thermal, spectroscopic and single‐crystal X‐ray diffraction techniques. All the complexes crystallize in a monoclinic crystal system with P21/n space group and Z = 4. Structural studies of [Co(L)(LH)]?H2O indicate the presence of both amido and imidol tautomeric forms of the ligand, resulting in a distorted octahedral geometry around the Co(III) ion. On the other hand, in the [Ni(L)(DMF)] and [Cu(L)(H2O)] complexes, the ligand coordinates to the metal through imidol form resulting in distorted square planar geometry, in which the fourth position is occupied by the oxygen of coordinated DMF in [Ni(L)(DMF)] and by a water molecule in [Cu(L)(H2O)]. Hirshfeld surface calculations were performed to explore hydrogen bonding and C―H???π interactions. Molecular docking studies were carried out to study the interaction between the synthesized compounds and proteins (cyclooxygenase‐2 and 5‐lipoxygenase). The complexes along with the parent ligand were screened for their in vivo anti‐inflammatory activity, using the carrageenan‐induced rat paw oedema method. The complexes show significant anti‐inflammatory potencies. 相似文献
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Reaction of Ti(OCH2CH2OR)4 (R?CH3 and C2H5) with 8‐hydroxyquinoline in benzene at room temperature resulted in the formation of Ti(C9H6NO)2(OCH2CH2OR)2, characterized by IR, 1H‐NMR, UV and mass spectroscopies. The molecular structure of Ti(C9H6NO)2(OCH2CH2OCH3)2 has been determined by single‐crystal X‐ray structure analysis. The geometry at titanium is a distorted octahedron, with the nitrogen atoms of quinolinate occupying the trans position with respect to oxygens of the 2‐methoxyethoxy groups. The prepared quinolinate derivatives of titanium alkoxides are very stable towards hydrolysis and harsh conditions are required for hydrolytic cleavage. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
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Dr. Bahia Arezki Dr. Guntram Schwarz Dr. Yves Bodenthin Dr. Dirk Luetzenkirchen‐Hecht Dr. Christian Markert Dr. Ralph Wagner Prof. Ronald Frahm Prof. Dirk G. Kurth Prof. Ullrich Pietsch 《Chemphyschem》2011,12(2):405-410
X‐ray absorption near the iron K edge (XANES) was used to investigate the characteristics of temperature‐induced low‐spin‐to‐high‐spin change (SC) in metallo‐supramolecular polyelectrolyte amphiphile complexes (PAC) containing FeN6 octahedra attached to two or six amphiphilic molecules. Compared to the typical spin‐crossover material Fe(phen)2(NCS)2 XANES spectra of PAC show fingerprint features restricted to the near‐edge region which mainly measures multiple scattering (MS) events. The changes of the XANES profiles during SC are thus attributed to the structure changes due to different MS path lengths. Our results can be interpreted by a uniaxial deformation of FeN6 octahedra in PAC. This is in agreement with the prediction that SC is originated by a structural phase transition in the amphiphilic matrix of PAC, but in contrast to Fe(phen)2(NCS)2, showing the typical spin crossover being associated with shortening of all the metal–ligand distances. 相似文献
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Munehisa Yasuniwa Shinsuke Tsubakihara Kazuhito Ohoshita Shin'Ichi Tokudome 《Journal of Polymer Science.Polymer Physics》2001,39(17):2005-2015
The double melting behavior of poly(butylene terephthalate) (PBT) was studied with differential scanning calorimetry (DSC) and wide‐angle X‐ray analysis. DSC melting curves of melt‐crystallized PBT samples, which we prepared by cooling from the melt (250 °C) at various cooling rates, showed two endothermic peaks and an exothermic peak located between these melting peaks. The cooling rate effect on these peaks was investigated. The melt‐crystallized PBT sample cooled at 24 K min?1 was heated at a rate of 1 K min?1, and its diffraction patterns were obtained successively at a rate of one pattern per minute with an X‐ray measurement system equipped with a position‐sensitive proportional counter. The diffraction pattern did not change in the melting process, except for the change in its peak height. This suggests that the double melting behavior does not originate from a change in the crystal structure. The temperature dependence of the diffraction intensity was obtained from the diffraction patterns. With increasing temperature, the intensity decreased gradually in the low‐temperature region and then increased distinctly before a steep decrease due to the final melting. In other words, the temperature‐dependence curve of the diffraction intensity showed a peak that is interpreted as proof of the recrystallization in the melting process. The peak temperature was 216 °C. The temperature‐dependence curve of the enthalpy change obtained by the integration of the DSC curve almost coincided with that of the diffraction intensity. The double melting behavior in the heating process of PBT is concluded to originate from the increase of crystallinity, that is, recrystallization. © 2001 John Wiley & Sons, Inc. J Polym Sci Part B: Polym Phys 39: 2005–2015, 2001 相似文献
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Evidence of CuI/CuII Redox Process by X‐ray Absorption and EPR Spectroscopy: Direct Synthesis of Dihydrofurans from β‐Ketocarbonyl Derivatives and Olefins
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Hong Yi Zhixiong Liao Guanghui Zhang Guoting Zhang Chao Fan Xu Zhang Prof. Dr. Emilio E. Bunel Dr. Chih‐Wen Pao Prof. Dr. Jyh‐Fu Lee Prof. Dr. Aiwen Lei 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(52):18925-18929
The CuI/CuII and CuI/CuIII catalytic cycles have been subject to intense debate in the field of copper‐catalyzed oxidative coupling reactions. A mechanistic study on the CuI/CuII redox process, by X‐ray absorption (XAS) and electron paramagnetic resonance (EPR) spectroscopies, has elucidated the reduction mechanism of CuII to CuI by 1,3‐diketone and detailed investigation revealed that the halide ion is important for the reduction process. The oxidative nature of the thereby‐formed CuI has also been studied by XAS and EPR spectroscopy. This mechanistic information is applicable to the copper‐catalyzed oxidative cyclization of β‐ketocarbonyl derivatives to dihydrofurans. This protocol provides an ideal route to highly substituted dihydrofuran rings from easily available 1,3‐dicarbonyls and olefins. 相似文献
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Syntheses and Structures of New Trinuclear MIILnMII (M = Ni,Co; Ln = Gd,Ce) Complexes with 2, 6‐Bis(acetobenzoyl)pyridine
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One‐pot reactions of 2, 6‐bis(acetobenzoyl)pyridine (H2L) with a mixture of LnCl3 (Ln = Ce, Gd) and Ni(CH3COO)2 (ratio 2:1:2) in CH2Cl2/MeOH in the presence of a supporting base like Et3N give trinuclear complexes with the general composition [Ni2Ln(L)2(CH3COO)3(MeOH)2/3] ( 1 ) in high yields. Trinuclear [Ni2Ln(L)2(PhCOO)3(MeOH)2] ( 2 ) complexes are formed when similar reactions are performed starting from NiCl2, and benzoic acid (PhCOOH) is added subsequently. Under the same conditions, reactions with the corresponding cobalt(II) salts result in the formation of a neutral [Co8(μ3‐O)2(L)6] complex, which has a bis(triple‐helical) structure. The cobalt(II) analogues to compounds 1 and 2 , however, can be synthesized by a pre‐treatment of the lanthanide salts with H2L and subsequent addition of the cobalt salts, and benzoic acid (in the case of 2 ). 相似文献
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Pedro Álvarez‐Boo José S. Casas Eduardo E. Castellano M. Delfina Couce Rosa Farto Eduardo Freijanes José Sordo 《应用有机金属化学》2007,21(1):49-53
Reaction of 3‐(2‐methoxyphenyl)‐2‐sulfanylpropenoic acid [H2(o‐mpspa)] with SnPh3OH in the presence of di‐isopropylamine resulted in the formation of the complex [HQ][SnPh3(o‐mpspa)] (where HQ = di‐isopropylammonium cation and o‐mpspa = 3‐(2‐methoxyphenyl)‐2‐sulfanylpropenoato), which was characterized by mass spectrometry and vibrational spectroscopy, as well as by 1H, 13C and 119Sn NMR spectroscopy. The single‐crystal X‐ray structural analysis of the new complex shows a trigonal‐bipyramidal coordination geometry around the Sn atom where o‐mpspa behaves as a bidentate chelating ligand. Dimeric units arise from the existence of N? H…O hydrogen bonds between the NH2 group of the di‐isopropylammonium cation and the oxygen atoms of the two neighbouring carboxylato groups. The bacteriostatic activity of the complex is also reported. Copyright © 2007 John Wiley & Sons, Ltd. 相似文献
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Sabine Schuster Prof. Dr. Elias Klemm Prof. Dr. Matthias Bauer 《Chemistry (Weinheim an der Bergstrasse, Germany)》2012,18(49):15831-15837
The metal–organic framework (MOF) [Pd(2‐pymo)2]n (2‐pymo=2‐pyrimidinolate) was used as catalyst in the hydrogenation of 1‐octene. During catalytic hydrogenation, the changes at the metal nodes and linkers of the MOF were investigated by in situ X‐ray absorption spectroscopy (XAS) and IR spectroscopy. With the help of extended X‐ray absorption fine structure and X‐ray absorption near edge structure data, Quick‐XAS, and IR spectroscopy, detailed insights into the catalytic relevance of Pd2+/Pd0 in the hydrogenation of 1‐octene could be achieved. Shortly after exposure of the catalyst to H2 and simultaneously with the hydrogenation of 1‐octene, the aromatic rings of the linker molecules are hydrogenated rapidly. Up to this point, the MOF structure remained intact. After completion of linker hydrogenation, the linkers were also protonated. When half of the linker molecules were protonated, the onset of reduction of the Pd2+ centers to Pd0 was observed and the hydrogenation activity decreased, followed by fast reduction of the palladium centers and collapse of the MOF structure. Major fractions of Pd0 are only observed when the hydrogenation of 1‐octene is almost finished. Consequently, the Pd2+ nodes of the MOF [Pd(2‐pymo)2]n are identified as active centers in the hydrogenation of 1‐octene. 相似文献
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C. A. Furtado A. O. Porto G. G. Silva R. A. Silva M. A. Pimenta M. C. Martins‐Alves P. J. Schilling 《Journal of Polymer Science.Polymer Physics》2001,39(21):2572-2580
X‐ray absorption spectroscopy [extended X‐ray absorption fine structure (EXAFS) and X‐ray absorption near‐edge structure (XANES)], differential scanning calorimetry, and Raman spectroscopy measurements were performed for a series of liquid polyether/salt systems prepared with poly(tetramethylene glycol) (PTMG) and the copolymer poly(tetramethylene glycol‐co‐ethylene glycol) as matrices and zinc and cobalt chlorides as dopants in the concentration range of n = 30–90, where n is the molar ratio of oxygen to metal cation. According to EXAFS, XANES, and Raman results, even in diluted solutions, these complexes exist mostly as undissociated ZnCl2 and CoCl2 species, presenting a weak cation–polymer interaction. EXAFS results indicate that for polymer/ZnCl2 systems, the nearest metal neighbors are only chlorine atoms. However, for polymer/CoCl2 samples, oxygen is also observed coordinating the metal. Raman spectra do not support any feature related specifically to the cation–polymer interaction. Nevertheless, for both salts the symmetric stretching vibrations are located in frequencies characteristic of salt in solution, which means that the polymer solvating action is effective. Differential scanning calorimetry data show an increase in the glass‐transition temperature for all polymer/salt systems in relation to the pure polymer samples, a consequence of the increase in the macromolecular chain stiffening produced by the presence of the salt. This result corroborates the existence of polymer–salt interactions. © 2001 John Wiley & Sons, Inc. J Polym Sci Part B: Polym Phys 39: 2572–2580, 2001 相似文献
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Namik Özdemi̇r Bi̇lge Eren Muharrem Di̇nçer Yunus Bekdemi̇r 《International journal of quantum chemistry》2011,111(12):3112-3124
The title molecule, 2‐(4‐chlorophenyl)‐1‐methyl‐1H‐benzo[d]imidazole (C14H11ClN2), was prepared and characterized by 1H NMR, 13C NMR, IR, and single‐crystal X‐ray diffraction. The molecular geometry, vibrational frequencies, and gauge including atomic orbital (GIAO) 1H and 13C NMR chemical shift values of the title compound in the ground state have been calculated by using the Hartree‐Fock (HF) and density functional theory (DFT/B3LYP) method with 6‐31G(d) basis sets, and compared with the experimental data. The calculated results show that the optimized geometries can well reproduce the crystal structural parameters, and the theoretical vibrational frequencies and GIAO 1H and 13C NMR chemical shifts show good agreement with experimental values. The energetic behavior of the title compound in solvent media has been examined using B3LYP method with the 6‐31G(d) basis set by applying the Onsager and the polarizable continuum model (PCM). Besides, molecular electrostatic potential (MEP), frontier molecular orbitals (FMO) analysis, and nonlinear optical (NLO) properties of the title compound were investigated by theoretical calculations. © 2010 Wiley Periodicals, Inc. Int J Quantum Chem, 2011 相似文献
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Sulfonamide‐derived new ligands, 4‐({[(E)‐(5‐bromo‐2‐hydroxyphenyl)methylidene]‐amino}methyl)benzenesulfonamide and 4‐bromo‐2‐((E)‐{4‐[(3,4‐dimethylisoxazol‐5‐yl)sulfamoyl]phenyl}iminiomethyl)phenolate and their transition metal [cobalt(II), copper(II), nickel(II) and zinc(II)] complexes were synthesized and characterized. The nature of bonding and structure of all the synthesized compounds were deduced from physical (magnetic susceptibility and conductivity measurements), spectral (IR, 1H and 13C NMR, electronic, mass spectrometry) and analytical (CHN analysis) data. The structure of the ligand, 4‐bromo‐2‐((E)‐{4‐[(3,4‐dimethylisoxazol‐5‐yl)sulfamoyl]phenyl} iminiomethyl)phenolate was also determined by X‐ray diffraction method. An octahedral geometry was suggested for all the complexes. In order to evaluate the biological activity of the ligands and the effect of metals, the ligands and their metal complexes were screened for in vitro antibacterial, antifungal and cytotoxic activity. The results of these studies revealed that all compounds showed moderate to significant antibacterial activity against one or more bacterial strains and good antifungal activity against various fungal strains. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
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Helle Svendsen Jacob Overgaard Dr. Marie A. Chevallier Eric Collet Prof. Dr. Yu‐Sheng Chen Dr. Frank Jensen Prof. Dr. Bo B. Iversen Prof. Dr. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2010,16(24):7215-7223
Single‐crystal X‐ray diffraction measurements have been carried out on [Nd(dmf)4(H2O)3(μ‐CN)Fe(CN)5]?H2O ( 1 ; dmf=dimethylformamide), [Nd(dmf)4(H2O)3(μ‐CN)Co(CN)5]?H2O ( 2 ), [La(dmf)4(H2O)3(μ‐CN)Fe(CN)5]?H2O ( 3 ), [Gd(dmf)4(H2O)3(μ‐CN)Fe(CN)5]?H2O ( 4 ), and [Y(dmf)4(H2O)3(μ‐CN)Fe(CN)5]?H2O ( 5 ), at 15(2) K with and without UV illumination of the crystals. Significant changes in unit‐cell parameters were observed for all the iron‐containing complexes, whereas 2 showed no response to UV illumination. Photoexcited crystal structures have been determined for 1 , 3 , and 4 based on refinements of two‐conformer models, and excited‐state occupancies of 78.6(1), 84(6), and 86.6(7) % were reached, respectively. Significant bond‐length changes were observed for the Fe–ligand bonds (up to 0.19 Å), the cyano bonds (up to 0.09 Å), and the lanthanide–ligand bonds (up to 0.10 Å). Ab initio theoretical calculations were carried out for the experimental ground‐state geometry of 1 to understand the electronic structure changes upon UV illumination. The calculations suggest that UV illumination gives a charge transfer from the cyano groups on the iron atom to the lanthanide ion moiety, {Nd(dmf)4(H2O)3}, with a distance of approximately 6 Å from the iron atom. The charge transfer is accompanied by a reorganization of the spin state on the {Fe(CN)6} complex, and a change in geometry that produces a metastable charge‐transfer state with an increased number of unpaired electrons, thus accounting for the observed photomagnetic effect. 相似文献
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Yu‐Quan Feng Yu‐Long Hu Hong‐Wei Wang Feng‐Pu Cao 《Acta Crystallographica. Section C, Structural Chemistry》2015,71(8):679-682
A new linear bismuth(III) coordination polymer, catena‐poly[[chloridobismuth(III)]‐μ3‐1,10‐phenanthroline‐2,9‐dicarboxylato‐κ6O2:O2,N1,N10,O9:O9], [Bi(C14H6N2O4)Cl]n, has been obtained by an ionothermal method and characterized by elemental analysis, energy‐dispersive X‐ray spectroscopy, IR spectroscopy, thermal stability studies and single‐crystal X‐ray diffraction. The structure is constructed by Bi(C14H6N2O4)Cl fragments in which each BiIII centre is seven‐coordinated by one Cl atom, four O atoms and two N atoms. The coordination geometry of the BiIII cation is distorted pentagonal–bipyramidal (BiO4N2Cl), with one bridging carboxylate O atom and one Cl atom located in the axial positions. The Bi(C14H6N2O4)Cl fragments are further extended into a one‐dimensional linear polymeric structure via subsequent but different centres of symmetry (bridging carboxylate O atoms). Neighbouring linear chains are assembled via weak C—H...O and C—H...Cl hydrogen bonds, forming a three‐dimensional supramolecular architecture. Intermolecular π–π stacking interactions are observed, with centroid‐to‐centroid distances of 3.678 (4) Å, which further stabilize the structure. In addition, the solid‐state fluorescence properties of the title coordination polymer were investigated. 相似文献
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A number of alkyltin(IV) paratoluenesulfonates, RnSn(OSO2C6H4CH3‐4)4?n (n = 2, 3; R = C2H5, n‐C3H7, n‐C4H9), have been prepared and IR spectra and solution NMR (1H, 13C, 119Sn) are reported for these compounds, including (n‐C4H9)2Sn(OSO2X)2 (X = CH3 and CF3), the NMR spectra of which have not been reported previously. From the chemical shift δ(119Sn) and the coupling constants 1J(13C, 119Sn) and 2J(1H, 119Sn), the coordination of the tin atom and the geometry of its coordination sphere in solutions of these compounds is suggested. IR spectra of the compounds are very similar to that observed for the paratoluenesulfonate anion in its sodium salt. The studies indicate that diorganotin(IV) paratoluenesulfonates, and the previously reported compounds (n‐C4H9)2Sn(OSO2X)2 (X = CH3 and CF3), contain bridging SO3X groups that yield polymeric structures with hexacoordination around tin and contain non‐linear C? Sn? C bonds. In triorganotin(IV) sulfonates, pentacoordination for tin with a planar SnC3 skeleton and bidentate bridging paratoluenesulfonate anionic groups are suggested by IR and NMR spectral studies. The X‐ray structure shows [(n‐C4H9)2Sn(OSO2C6H4CH3‐4)2·2H2O] to be monomeric containing six‐coordinate tin and crystallizes from methanol–chloroform in monoclinic space group C2/c. The Sn? O (paratoluenesulfonate) bond distance (2.26(2) Å) is indicative of a relatively high degree of ionic character in the metal–anion bonds. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献