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1.
Naka Seidel Klaus Jacob Piero Zanello Marco Fontani 《Journal of organometallic chemistry》2001,620(1-2)
The reaction of {C,N-[Fe(η5-C5H5)(η5-C5H3(CH2NMe2)-2)]}Li, (FcN)Li, with zinc chloride affords the diorganozinc complex (FcN)2Zn (1). In solution, 1 appears as a mixture of rac and meso diastereomers, whereas in the solid state it crystallizes solely as a rac diastereomer. The ratio of rac/meso diastereomers in solution is solvent-, temperature- and concentration-dependent, consistent with an intermolecular exchange between diastereomers. An intramolecular dynamic phenomenon involving dissociation and recoordination of Zn---N bonds was also observed. The reaction of 1 with zinc chloride yields the monoorganozinc compound (FcN)ZnCl (2) as a slightly soluble yellow microcrystalline powder. 相似文献
2.
It is demonstrated by cyclovoltammetry and ESR spectroscopy that N,N,N,'N,'-tetramethyl; tetraethgl, tetra-n-propyl, tetra-n-butyl-p-phenylenediamine and tetraethyl, tetra-n-propyl-p-benzidine undergo deprotonat ion and two consecutive single electron transfer step CE reaction at electrode in aqueous acetonitrile with the corresponding radical cations as the intermediate. The bivalent cations produced at the electrode react not only with hydroxyl anion in the medium to give quinone but also with the N-alkyl-p-phenylene-diamines or benzidines to produce the corresponding radical cations. 相似文献
3.
The synthesis of a series of new alkoxylated linearly annulated dioxins is described together with their cyclic voltammetric behavior and some preliminary result on their ability to form cation radical salts. Of these dioxins, seven (8, 12, 19, 21, 27, 33, 34) are the first representatives of entirely new heterocyclic systems. Dioxins 8, 21, 22 and 27 gave good quality cation radical salts upon electrocrystallization. 相似文献
4.
The reaction of [Ti](CCR)2 {[Ti] = (η5-C5H4SiMe3)2Ti; 1a, R = Fc, Fc = (η5-C5H4)Fe(η5-C5H5); 1b, R = Ph} with MX {2a, MX = [Cu(NCCH3)4]BF4; M = Ag; 2b, X = ClO4; 2c, X = NO3} in a 2:1 molar ratio produces the trinuclear heterobimetallic (Ti2M) or heptanuclear heterotrimetallic (Ti2MFe4) complexes [{[Ti](μ-σ,π-CCR)2}2M]X (R = Fc: 3a, M = Cu, X = BF4; 3b, M = Ag, X = ClO4. R = Ph: 3c, M = Cu, X = BF4; 3d, M = Ag, X = ClO4: 3e, M = Ag, X = NO3) in high yield. Complexes 3c-3e are also accessible, when {[Ti](μ-σ,π-CCPh)2}MX (M = Cu: 4a, X = FBF3; M = Ag: 4b, X = OClO3; 4c, X = ONO2) is reacted with one equivalent of 1b. Transferring this reaction scheme to [Ti](CCSiMe3)2 (1c) only the formation of the heterobimetallic tweezer complex {[Ti](μ-σ,π-CCSiMe3)2}MX {4d, MX = [Cu(NCCH3)]BF4; 4e, MX = AgOClO3} is observed which is attributed to the bulkiness of the acetylide-bound Me3Si group. The solid-state structure of 3e is reported. In 3e, two [Ti](CCPh)2 tweezer moieties are chelate-bound by their carbon-carbon triple bonds to a silver(I) ion, resulting in a pseudo-tetrahedral environment at the group-11 metal. is acting as counter-ion to cationic [{[Ti](CCPh)2}2Ag]+.Additionally, the result of cyclic voltammetric studies on [{[Ti](μ-σ,π-CCPh)2}2Cu]BF4 (3c) is reported. 相似文献
5.
Syntheses, Structures, Electrochemistry and Optical Properties of Alkyne‐Functionalized 1,3,2‐Diazaboroles and 1,3,2‐Diazaborolidenes The reaction of 2‐bromo‐1,3‐ditert‐butyl‐2,3‐dihydro‐1H‐1,3,2‐diazaborole ( 3 ) with lithiated tert‐butyl‐acetylene and lithiated phenylacetylene affords the 2‐alkynyl‐functionalized 1,3,2‐diazaboroles 4 and 5 as a thermolabile colorless oil ( 4 ) or a solid ( 5 ). Similarly 2‐bromo‐1,3‐diethyl‐2,3‐dihydro‐1H‐1,3,2‐benzodiazaborole ( 6 ) was converted into the crystalline 2‐alkynyl‐benzo‐1,3,2‐diazaboroles 7 and 8 by treatment with LiC≡C–tBu or LiC≡CPh, respectively. 2‐Ethynyl‐1,3‐ditert‐butyl‐2,3‐dihydro‐1H‐1,3,2‐diazaborole ( 2 ) was metalated with tert‐butyl‐lithium and subsequently coupled with 2‐bromo‐1,3,‐ditert‐butyl‐2,3‐dihydro‐1H‐1,3,2‐diazaborole ( 3 ) to afford bis(1,3‐ditert‐butyl‐2,3‐dihydro‐1H‐1,3,2‐diazaborol‐2‐yl)acetylene ( 9 ) as thermolabile colorless crystals. Analogously coupling of the lithiated species with 6 or with 2‐bromo‐1,3‐ditert‐butyl‐1,3,2‐diazaborolidine ( 11 ) gave the unsymmetrically substituted acetylenes 10 or 12 , respectively, as colorless solids. Compounds 4 , 5 , 7 – 10 and 12 are characterized by elemental analyses and spectroscopy (IR, 1H‐, 11B{1H}, 13C{1H}‐NMR, MS). The molecular structures of 5 , 8 and 9 were elucidated by X‐ray diffraction analyses. 相似文献
6.
W. Likussar A. Michelitsch M. Schubert-Zsilavecz D. Gusterhuber 《Monatshefte für Chemie / Chemical Monthly》1991,122(11):987-994
Summary 2-Phenylthio-1,4-benzoquinone (1 a) reacts with azomethine ylide AY-A to give 2-methyl-5-phenylthio-2H-isoindole-4,7-dione (4 f). With 2-(N-methylanilino)-5-methyl-1,4-benzoquinone (1 b), the azomethine ylide AY-B undergoes cycloaddition to yield an inseparable mixture of 5a-methyl-8-(N-methylanilino)-2,3,5,5a,9a,9b-hexahydro-pyrrolo[2,1-a]1H-isoindole-6,9-dione (5 bI) and 9a-methyl-7-(N-methylanilino)-2,3,5,5a,9a,9b-hexahydropyrrolo[2,1-a]1H-isoindole-6,9-dione (5 bII). The structures of5 bI and5 bII were established on basis of two-dimensional-NMR-techniques. The mechanism of the cycloaddition of azomethine ylides to 1,4-quinones was studied on basis of cyclovoltammetric investigations. To determine the electron affinity of the isoindoledione derivatives4 a–f and5 a–b the peak potentials were measured by differential pulse polarography (DPP). 相似文献
7.
A. Bach L. Beyer C. Hennig K. H. Hallmeier J. Sieler 《Monatshefte für Chemie / Chemical Monthly》1997,128(3):217-224
Zusammenfassung Die Molekülstruktur und das cyclovoltammetrische Verhalten von 1,4-Bis-(pyrrol-1-yl-carbonyl)benzol (1) werden beschrieben. Das Röntgenabsorptionsspektrum von1 (NK XANES) wird bezüglich der N1s *-Übergänge im Vergleich mit 1H-Pyrrol untersucht.
Molecular structure, electrochemical behaviour, and NK XANES of 1,4-bis(pyrrol-1-yl-carbonyl)benzene
Summary The molecular structure and the cyclovoltammetric behaviour of 1,4-bis(pyrrol-1-yl-carbonyl)benzene (1) are described. The X-ray absorption spectrum of1 (NK XANES) is investigated with respect to the N1s * transitions in comparison with 1H-pyrrole.
Prof. Dr. Peter Welzel zum 60. Geburtstag gewidmet. 相似文献
8.
(Oligo)phenothiazinyl nitriles were synthesized in good to very good yields from bromo (oligo)phenothiazines via the Beller cyanation protocol either under conductive or under dielectric heating using NMP as a solvent. Their electronic properties were determined by absorption and emission spectroscopy and cyclic voltammetry. Cyano(oligo)phenothiazines display large Stokes-shifts (5800-8300 cm−1) and substantial quantum yields (11-27%). Their reversible oxidation potentials are considerably shifted anodically due to the electron-withdrawing character of the cyano group. 相似文献
9.
The synthesis of biferrocene-bridged NCN pincer palladium and platinum complexes (NCN = [1-C6H2(CH2NMe2)2-3,5]−) is discussed. Sonogashira cross-coupling of [(η5-C5H4)Fe(η5-C5H4CCH)]2 (1) with I-1-NCN-4-X (2a, X = H; 2b, X = Br) produces [(η5-C5H4)Fe(η5-C5H4CC-1-NCN-4-X)]2 (3a, X = H; 3b, X = Br). Homobimetallic 3b further reacts with [Pd2(dba)3 · CHCl3] (4) or [Pt(tol)2(SEt2)]2 (5) (dba = dibenzylidene acetone, tol = 4-tolyl), respectively, to give tetrametallic [(η5-C5H4)Fe(η5-C5H4CC-4-NCN-1-MBr)]2 (6, M = Pd; 7, M = Pt) in which NCN-MBr fragments are connected by a biferrocene unit. Cyclovoltammetric studies show that the ferrocene moieties can independently be oxidized. The difference of the Fe(II)/Fe(III) redox couples amounts to ca. 300 mV and is not affected by the nature of the NCN pincer metal moities. 相似文献
10.
Mehmet Karakus Peter Lnnecke Dmitry Yakhvarov Evamarie Hey‐Hawkins 《无机化学与普通化学杂志》2004,630(10):1444-1450
The reaction of 2,4‐diferrocenyl‐1,3‐dithiadiphosphetane 2,4‐disulfide [FcPS(μ‐S)]2 [Fc = Fe(η5‐C5H4)(η5‐C5H5)] with alcohols ROH gave the corresponding ferrocenyldithiophosphonic acids [FcPS(OR)(SH)], which were treated in situ with Ni(CH3COO)2·4H2O in acetic acid to yield the square‐planar heterobimetallic trinuclear complexes [{FcP(OR)S2}2Ni] (R = Me ( 1 ), Et ( 2 ), Pri ( 3 ), Bus ( 4 ) and Bui ( 5 )). Compounds 1‐5 were characterized by elemental analysis, MS, NMR (1H, 13C and 31P), IR spectroscopy, and 2‐5 also by X‐ray crystallography. Cyclovoltammetric studies on the heterobimetallic nickel(II) complexes 1‐5 showed irreversible reduction to unstable nickel(I) complexes and an irreversible two‐electron oxidation of the sulfur‐containing nickel fragments, followed by a reversible one‐electron oxidation of the two ferrocenyl groups. 相似文献