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1988 (283)
101Author    Ralf Steudel, Birger HolzRequires cookie*
 Title    Detection of Reactive Sulfur Molecules (S 6 , S 7 , S 9 , S^) in Commercial Sulfur, in Sulfur Minerals, and in Sulfur Melts Slowly Cooled to 20 °C [1]  
 Abstract    HPLC, Sulfur Molecules Quantitative analysis by high-pressure liquid chromatography shows that all commercial sam-ples of elemental sulfur besides S 8 contain traces of S 7 (up to 0.56%) and in some cases also S 6 , S 9 , and polymeric sulfur (S«,). Pure S 8 can be obtained by recrystallization from CS 2 . Elemental sulfur minerals also quite often contain traces of S 7 (up to 0.3%). Since neither irradiation by daylight at 20 °C nor heating to 90 °C for 41 days did convert a-S 8 into S 7 , the reactive sulfur molecules S" (n=£8) are believed to origin from liquid or gaseous sulfur which are known to be complex equilibrium mixtures of many S" species. Sulfur melts slowly cooled (within 0.6 to 145 h) from 122 to 20 °C in fact contain S 7 (minimum 0.2%) and at cooling rates of <24 h also other non-S 8 molecules. Solid solutions of S 7 in a-S 8 have also been prepared by cocrystallization of the compounds from CS 2 . In contrast to pure a-S 8 , these solid solutions are pale-yellow at 77 K, and the implications of these findings for the surface composition of Jupiter's satellite Io and for the mechanical properties of "formed sulfur" (Prills, Rotoform, Slates, etc.) are discussed. 
  Reference    Z. Naturforsch. 43b, 581—589 (1988); received December 4 1987 
  Published    1988 
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 Identifier    ZNB-1988-43b-0581 
 Volume    43 
102Author    ManfredL. Ziegler, Klaus Blechschmitt, Harald Bock, Ernst Guggolz, RichardP. KorswagenRequires cookie*
 Title    Über die Reaktivität von [(CH 3 ) 2 N] 6 W 2 (W=W) gegenüber CS 2 /S 8 und CS 2 /Se, Röntgenstrukturanalyse von [(CH 3 ) 2 NCS 2 ] 2 W(S)(S 2 ) Reactivity of [(CH 3 ) 2 N] 6 W 2 (W=W) Towards CS 2 /S 8 and CS 2 /Se 8 . X-Ray Structure Analysis of [(CH 3 ) 2 NCS 2 ] 2 W(S)(S 2 )  
 Abstract    In this paper we report two improved preparation methods for [(CH 3) 2 N] 6 W 2 (W=W) (1), one starting from WC1 4 (yield 51%), and a second one starting from W 2 C1 6 (THF) 4 (ca. 60% yield). We have studied the reactions of 1 with different nucleophiles, among them triphenylalkylidenphos-phoranes (like Ph 3 P=CH 2 and Ph 3 P=CHPh • LiCl; Ph = phenyl), sulfur and CS 2 . 1 reacts with S 8 and CS 2 in hexane to yield the two new compounds (Me 2 NCS 2) 2 WS(S 2) (4) and W(CS 2 H)(Me 2 NCS 2) 2 (5), both containing dithiocarbamato ligands formed by insertion of CS 2 into the W-N bond. The two mononuclear compounds were characterized spectroscopically, in the case of 4 an X-ray diffraction structure analysis was performed. The reaction of 1 with Se and CS 2 , leads to the compounds 4, (Me 2 NCS 2) 2 W 2 S 4 (6) and [(Me 2 N) 2 C]CS 2 (7), which were also characterized spectroscopically. No Se-containing compounds could be isolated. 4 crystallizes monoclinically, C 5 2h -P2Jn, with a = 648.6(3), b = 1346.7(6) and c = 1745.9(7) pm, ß = 91.85(3)°, V = 1524xl0 6 pm 3 , Z = 4. The structure of the seven-coordinate tungsten compound is discussed and compared to complexes with similar ligands and geometry. 
  Reference    Z. Naturforsch. 43b, 590—598 (1988); eingegangen am 28. Dezember 1987 
  Published    1988 
  Keywords    Reactivity, Synthesis, X-Ray 
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 Identifier    ZNB-1988-43b-0590 
 Volume    43 
103Author    Günter KlarRequires cookie*
 Title    Elementorganische Verbindungen mit o-Phenylenresten, XV [1] Hexamethoxy-tetrachalcogena-tetrahydropentacene Organometallic Compounds with o-Phenylene Substituents, Part XV [1] Hexamethoxy-tetrachaleogena-tetrahydropentaeenes Peer Berges  
  Reference    Z. Naturforsch. 43b, 599—604 (1988); eingegangen am 21. Januar 1988 
  Published    1988 
  Keywords    tetrahydropentacene, Synthesis, 'H NMR Spectra, X-Ray 
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 Identifier    ZNB-1988-43b-0599 
 Volume    43 
104Author    Reiner Radeglia, Helmut Poleschner, Werner SchrothRequires cookie*
 Title    NMR-spektroskopische Untersuchung des Problems der Valenzisomerie zwischen 1,2-Dithiin und (Z)-But-2-en-l,4-dithion NMR Spectroscopic Investigation Concerning the Problem of Valence Isomerism between 1,2-Dithiine and (Z)-But-2-ene-l,4-dithione  
 Abstract    -Bis(organylthio)-buta-l,3-diene, 1,2-Dithiines, (Z)-But-2-ene-l,4-dithione. Valence Isomerism, 13 C NMR Spectra 3,6-Diaryl-l,2-dithiines and their precursors, (Z,Z)-l,4-bis(organylthio)-buta-l,3-dienes, are investigated by 'H and 13 C NMR spectroscopy. The chemical shifts and coupling constants, which are relevant to the investigated problem, are determined and assigned, respectively, by different techniques (shift increments, spectrum simulation, heteronuclear 2D J-resolved and hetero-nuclear shift correlated 2D NMR spectra, anomalous off-resonance splittings and selective de-coupling experiments). The NMR parameters are discussed in relation to the molecular structure. The l3 C shift values prove the ring structure of 1,2-dithiines and exclude existence of the valence isomer (Z)-but-2-ene-l,4-dithione (absence of thiocarbonyl resonances). The vicinal 'H,'H cou-pling constants of the C4 unit of the investigated compounds verify (1) the (Z,Z) configuration of the organylthio groups in 1,4 position of butadiene, (2) the s-transoid conformation of acyclic butadienes and (3) the forced s-eis structure in the cyclic 1,2-dithiines. 
  Reference    Z. Naturforsch. 43b, 605—610 (1988); eingegangen am 4. Januar 1988 
  Published    1988 
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 Identifier    ZNB-1988-43b-0605 
 Volume    43 
105Author    T. Sogo, J. Romero, A. Sousa, A. De Blas, M. L. Durán, E. E. CastellanoRequires cookie*
 Title    The Electrochemical Synthesis of Neutral Zinc(II) Complexes of Schiff Base Ligands: The Crystal Structure of Bis[N-(4-methylphenyl)salicylaldiminato]zinc(II)  
 Abstract    The electrochemical synthesis and physico-chemical properties of neutral zinc(II) complexes of bidentate Schiff bases derived from salicylaldehydes are presented together with the X-ray struc-ture of bis[N-(4-methylphenyl)salicylaldiminato]zinc(II). The crystal is monoclinic, a = 21.877(3), b = 8.801(2), c = 12.027(5) Ä, ß = 96.55(3)°, space group C2/c. The complex is a monomer, and the zinc atom is tetrahedrally coordinated. 
  Reference    Z. Naturforsch. 43b, 611—615 (1988); received November 5 1987/January 28. 1988 
  Published    1988 
  Keywords    X-Ray, Zinc, Schiff Bases, Electrochemical Synthesis 
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 Identifier    ZNB-1988-43b-0611 
 Volume    43 
106Author    Hermann Poschenrieder, Hans-Dietrich StachelRequires cookie*
 Title    Synthese von 5-Alkyliden-2,3-pyrrolidindionen Synthesis of 5-Alkylidene-2,3-pyrrolidinediones  
  Reference    Z. Naturforsch. 43b, 616—618 (1988); eingegangen am 22. Dezember 1987 
  Published    1988 
  Keywords    Spirooxiranes, Retro-Aldol Cleavage, 5-Alkylidene-2, 3-pyrrolidinediones, a-Tetramic Acids 
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 Identifier    ZNB-1988-43b-0616 
 Volume    43 
107Author    Ernst Küsters, Willy RahmenRequires cookie*
 Title    Alio-Verbindungen mit ungewöhnlichem Verhalten bei der Gaschromatographie an chiraler stationärer Phase Allo-Compounds with Unusual Behaviour in Gas Chromatography Using Chiral Stationary Phase  
 Abstract    The Separation of the enantiomers of D,L-allo-threoninol, necessary in racemization studies of peptide hydrolysates, gave a surprising result with respect to the elution series of the antipodes. Contrary to the rule (L before D on Chirasil-L-Val) D-allo-threoninol is eluted before its mirror image. This behaviour can only be explained by the differing importance of the asymmetric centres contained in the molecule. As a result of this and taking into account the chromatographic behaviour of allo-compounds refined model concepts of enantiomer separation must be devel-oped in future. The separation of allo-compounds of threonine, isoleucine and cystathionine is considered from this aspect. 
  Reference    Z. Naturforsch. 43b, 619—622 (1988); eingegangen am 15. April/30. November 1987 
  Published    1988 
  Keywords    Enantiomeric Separation, Gaschromatography, Chirasil-Val, Allo-Compounds, Chiral Recognition 
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 Identifier    ZNB-1988-43b-0619 
 Volume    43 
108Author    Kaeko Kikuchi, Yoshio Taniyama, Ryuji MarumotoRequires cookie*
 Title    Evaluation of the 2 NH 2 A—T Pair in Hybridization, I Synthesis of the DNA/RNA Hybrid Oligomers Containing 2-Aminoadenosines  
 Abstract    DNA decamers containing 2-aminoadenosine were synthesized. Oligonucleotide duplexes in-cluding the 2 NH2A—T base pairs were prepared and their Tm profile examined. Contrary to expectation, elevation of the Tm value by the 2 NH2 group is very small in DNA/RNA duplexes. From the CD spectra measurement, we assume that the distortion of the B-DNA structure caused by scattered DNA/RNA base pairing diminishes the efficient hydrogen bonding and base stacking of the duplexes. It was also found that the DNA duplexes containing 2-aminoadenosine hybrids are considerably resistant to ribonuclease T2 or nuclease PI digestion. 
  Reference    Z. Naturforsch. 43b, 623—630 (1988); received October 12 1987/February 1 1988 
  Published    1988 
  Keywords    DNA Probe, Hybridization, 2-Aminoadenosine, CD Spectra, DNA/RNA Hybrid Oligomer 
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 Identifier    ZNB-1988-43b-0623 
 Volume    43 
109Author    H. Wagner, D. NusserRequires cookie*
 Title    Nachweis von Corticosteroiden im Fett von Dachs und Murmeltier Detection of Corticosteroids in Fat of Badger and of Alp-Marmot  
 Abstract    In our search for the antiinflammatory activ principles of fat of badger and alp-marmot, used in folk-medicine as remedies against rheumatism and arthritis, eight known corticosteroids have been detected and identified in the lipophilic fraction of body fats of both animals. Enrichment and detection succeeded by using TLC, straight phase HPLC with diode array equipment, HR-GC on OV-1 capillary columns and GC/MS of the methyloxime-trimethylsilylated steroids. The amount of the detected steroids ranges from 30-40 mg/kg. The whole antiinflammatory activity of the fat, as measured in the rat paw edema test, results from these and further hitherto unidentified cortico-steroids. 
  Reference    Z. Naturforsch. 43b, 631—633 (1988); eingegangen am 7. Januar 1988 
  Published    1988 
  Keywords    Fat, Badger, Alp-Marmot, Steroids, Corticosteroids 
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 Identifier    ZNB-1988-43b-0631 
 Volume    43 
110Author    Dieter Fenske, Hollnagel Achim, Kurt MerzweilerRequires cookie*
 Title    Reaction of [(^ 3 -C 4 H 7 )PdCl] 2 with Se(SiMe 3 ) 2 The Crystal Structure of [(>/ 3 -C 4 H 7 ) 6 Pd 6 Se 3 ]  
 Abstract    Synthesis, X-Ray, Crystal Structure of [(V 3 -C4H7)f,Pd6Se3], Trigonal Prismatic Pd-Se Cluster [(?7 3 -C4H7)PdCl]2 reacts with Se(SiMe3)2 to form [(?7 3 -C4H7)6Pd6Se3j (1). 1 has been characterized by X-ray crystal structure analysis. It contains a dis-torted trigonal prismatic Pd6-cluster. Three faces of the Pd-prism are occupied by jU4-Se ligands. 1 crys-tallizes in the space group Pnma with 4 formula units per unit cell. The lattice constants at 200 K are: a — 1175.1(8), b = 1611.4(12), c = 1720.3(12) pm. 
  Reference    Z. Naturforsch. 43b, 634—636 (1988); eingegangen am 25. Januar 1988 
  Published    1988 
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 Identifier    ZNB-1988-43b-0634_n 
 Volume    43 
111Author    Yuzo Nishida, Naoko Oshino, Tadashi TokiiRequires cookie*
 Title    Preparation and ESR Spectra of Manganese(III) Complexes with 2-[Bis(benzimidazol-2-ylmethyl)- amino] ethanol  
 Abstract    Manganese(III) Complexes, //-Oxo-di-^-acetato Bridges, ESR Spectra Manganese(III) complexes with 2-[bis(benz-imidazol-2-ylmethyl)amino]ethanol were prepared. Based on the analytical data, IR, magnetic and ESR ("16-line ESR signal" was observed in the frozen state) properties, these complexes are assumed to be of the binuclear structure with ,w-oxo and di-w-acetato bridges. 
  Reference    Z. Naturforsch. 43b, 637—638 (1988); received January 4 1988 
  Published    1988 
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 Identifier    ZNB-1988-43b-0637_n 
 Volume    43 
112Author    Jörg Adel, Christina Ergezinger, Reiner Figge, Kurt DehnickeRequires cookie*
 Title    Das Infrarotspektrum des Tetraselentetranitrids, Se 4 N 4 The Infrared Spectrum of Tetraseleniumtetranitride, Se 4 N 4  
 Abstract    The IR spectrum of solid Se4N4 has been recorded in the region of 100— 4000 cm -1 . The assignment has been made on the basis of slightly deformed D2d symmetry, which is in agreement with the X-ray structure determination. Abb. 1. IR-Spektrum von festem Se4N4. N = Absorption des Einbettungsmittels Nujol. 
  Reference    Z. Naturforsch. 43b, 639—640 (1988); eingegangen am 5. November 1987 
  Published    1988 
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 Identifier    ZNB-1988-43b-0639_n 
 Volume    43 
113Author    D. Sellmann, G. Binker, F. KnochRequires cookie*
 Title      
  Reference    Z. Naturforsch. 43b, 641 (1988) 
  Published    1988 
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 Identifier    ZNB-1988-43b-0641_e 
 Volume    43 
114Author    Wolfgang Bernhardt, Heinrich VahrenkampRequires cookie*
 Title    Hydrierungen und Dehydrierungen im System Benzonitril/Ru 3 (CO)i 2 /Benzylamin Hydrogenations and Dehydrogenations in the System Benzonitrile/Ru 3 (CO) 12 /Benzylamine  
 Abstract    The stepwise interconversions between benzonitrile and benzylamine have been realized in both directions via Ru3 cluster intermediates. The hydrogenation/dehydrogenation system can be entered from Ph-CN, Ru3(CO)12, and H2 yielding HRu3(CO),n(NCHPh) or from PhCH2NH2 and Ru3(CO)12 yielding HRu3(CO)10(NHCH2Ph). These two clusters can be interconverted by thermal hydrogenation and dehydrogenation, with H2Ru3(CO)9(NCH2Ph) as a CO and H2 depen-dent intermediate. The system can be left only towards benzylamine which is formed in small yields from HRu3(CO)10(NHCH2Ph) at high temperatures and under high CO or H2 pressures. 
  Reference    Z. Naturforsch. 43b, 643—647 (1988); eingegangen am 29. Januar 1988 
  Published    1988 
  Keywords    Hydrogenations, Dehydrogenations, Benzonitrile, Benzylamine 
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 Identifier    ZNB-1988-43b-0643 
 Volume    43 
115Author    Bernd Breilochs, Herbert BinderRequires cookie*
 Title    Neue Synthesewege zu B 4 H 10 und B 5 H 9 New Synthetic Routes to B 4 H 10 and B 5 H 9  
 Abstract    Syntheses of B4HIÜ and B5H9 The boron hydride B4H10 is prepared in high yields (90%) through hydride-ion abstraction reactions when a mixture of BH4~/B,HK is treated with CH,I or L. respectively. A high yield (96%) method for the conversion of B3H8~ to B4H10 is the reaction of B?HS with A1C1, in solvents which do not have any Lewis base character. The solvents are assumed to react as electron acceptors with the intermediate [B2H5~] to form B4H10, R and H2(R-H -solvent). A 1:1 mixture of B4H1(1and B5Hyis obtained when B3H8~ is treated with CH3I or I2. The reaction can be viewed to involve an initial step in which unstable "B,H7" is generated which immediately undergoes decomposition to give B4Hin, B5H9 and H2. Treatment of B4H,0 with (>z-Bu)4NBr results in the formation of B3H7Br~ which decomposes slowly at 0 °C to form B5H9. An alternative synthesis of BSH9 via hydride-ion abstraction is possible through the reaction of («-Bu)20-BF3 with B3H8~ in ether solvents. 
  Reference    Z. Naturforsch. 43b, 648—653 (1988); eingegangen am 27. November 1987 
  Published    1988 
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 Identifier    ZNB-1988-43b-0648 
 Volume    43 
116Author    AlexanderConstantin Filippou, ErnstOtto Fischer, Guido Helmut, AltRequires cookie*
 Title    Übergangsmetall-Carbin-Komplexe, XC [1] Synthese neuer, siebenfach-koordinierter, kationischer Carbin-Komplexe des Wolframs in einer höheren Oxidationszahl Transition Metal Carbyne Complexes, XC [1] Synthesis of New, Seven Coordinated, Cationic Tungsten Carbyne Complexes in a Higher Oxidation State  
 Abstract    Diiodo(dwm-butylisonitrile)(2.2'-bipyridyl)(diethylaminocarbyne)tungsten Iodide, Diiodo(di-terr-butylisonitrile)(l. 10-phenanthroline)(diethylaminocarbyne)tungsten Iodide 
  Reference    Z. Naturforsch. 43b, 654—657 (1988); eingegangen am 8. Dezember 1987 
  Published    1988 
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 Identifier    ZNB-1988-43b-0654 
 Volume    43 
117Author    Herbert Fisch, Hans Pritzkow, Walter SiebertRequires cookie*
 Title    Enthalogenierung von Bis(diisopropylamino-chlorboryl)methan: Lösungsmittelabhängige Bildung eines 1,2,4,5-Tetraborinan-und eines l-Aza-2,4-diborolidin-Derivats Dehalogenation of Bis(diisopropylamino-chloroboryl)methane: Solvent-dependent Formation of a 1,2,4,5-Tetraborinane and of a l-Aza-2,4-diborolidine Derivative  
  Reference    Z. Naturforsch. 43b, 658—664 (1988); eingegangen am 7. Dezember 1987 
  Published    1988 
  Keywords    l, 2, 4, 5-Tetrakis(diisopropylamino-chloroboryl)-l, 2, 4, 5-tetraborinane, l-Aza-2, 4-diborolidine Derivatives 
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 Identifier    ZNB-1988-43b-0658 
 Volume    43 
118Author    PeterM. Fritz, Wolfgang Beck, Ulrich Nagel, Kurt Polborn, WolfgangA. Herrmann, Christian Hecht, Jürgen RohrmannRequires cookie*
 Title    Metallorganische Lewis-Säuren, XXXV [1]  
 Abstract    Bildung und Struktur chalkogenverbrückter Metallkomplexe: [{(f/ 5 -C 5 H 5)(OC) 2 Fe} 2 SeSe{Fe(CO) 2 (i/ 5 -C 5 H 5)}] + BF 4 -und [(i/ 5 -C 5 H 5)(OC) 2 FeS(R)Re(CO) 5 ] + BF 4 -(R = Me, Ph) Organometallic Lewis Acids, XXXV [1] Formation and Stucture of Chalcogen Bridged Metal Complexes: [{(^ 5 -C 5 H 5)(OC) 2 Fe} 2 SeSe{Fe(CO) 2 (?; 5 -C 5 H5)}] + BF4-and [(^ 5 -C 5 H 5)(OC) 2 FeS(R)Re(CO)5] + BF4-(R = Me, Ph) The cationic diselenium bridged title compound 2 and [{(^-CsH^XCO^Fej^SeLBF.,' have been isolated from the reaction of (OC) 5 ReFBF 3 with (/< 2 -Se")[(^ 5 -C 5 H 5)(CO) 2 Fe] 2 (w = 1, 2). The heterometallic ^-thiolato title complex has been prepared from (OC) 5 ReFBF 3 and (?7 5 -C 5 H 5)(OC) 2 FeSR (R = Me. Ph; 4). The structures of 2 and 4a have been determined by X-ray diffraction analyses. 
  Reference    Z. Naturforsch. 43b, 665—670 (1988); eingegangen am 18. Januar/3. März 1988 
  Published    1988 
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 Identifier    ZNB-1988-43b-0665 
 Volume    43 
119Author    HeinzP. Fritz, Peter DavidRequires cookie*
 Title    Alkali-Polyketenenolat, ein Polyacetylen-Derivat Alkali-Polyketene-Enolate, a Polyacetylene Derivative  
 Abstract    An alkali-polyketene-enolate was made from polyketene by using aqueous bases MOH (M = Li, Na, K, Rb, Cs). The structure is proposed on the basis of IR and 13 C NMR spectra, the paramagnetic properties were investigated by EPR spectroscopy. AC conductivity measurements show a maximum conductivity of 1CT 2 Sern -1 (at 115 °C), where marked ionic participation is expected. Doping of the polyacetylene backbone with iodine gives no increase of conductivity; CV measurements indicate the presence of triiodide anions. 
  Reference    Z. Naturforsch. 43b, 671—676 (1988); eingegangen am 8. November 1987 
  Published    1988 
  Keywords    Alkali-Polyketene-Enolate, Polyketene, 13 C NMR Spectra, EPR Spectra, Conductivity 
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 Identifier    ZNB-1988-43b-0671 
 Volume    43 
120Author    Astrid Görge, Kurt Dehnicke, Dieter FenskeRequires cookie*
 Title    N-Chlornitrenokomplexe des Wolframs: WC1 4 (NC1) und [CH 3 CN-WC1 4 (NC1)] N-Chloro-Nitrene Complexes of Tungsten: WC1 4 (NC1) and [CH 3 CN-WC1 4 (NC1)]  
 Abstract    WC1 4 (NC1) has been prepared as a red-brown crystal powder by the reaction of tungsten hexacarbonyl with excess nitrogen trichloride in boiling CC1 4 . The complex is associated via chloro bridges, forming dimeric units, according to the IR spectrum. Thermal decomposition at 200 °C leads to tungsten nitride trichloride, WNC1,. With acetonitrile, WC1 4 (NC1) reacts with formation of the monomeric complex [CH,CN-WC1 4 (NC1)], which was characterized by its IR spectrum as well as by an X-ray structure determination. Crystal data: space group P2,/m, Z = 2 (1387 independent observed reflexions, R — 0.07). Lattice dimensions at 20 °C: a = 590.4(3), b = 729.0(3), c = 1124.6(4) pm, ß = 100.63(2)°. The complex forms monomeric molecules, in which the tungsten atom has a distorted octahedral environment of four chlorine atoms in equatorial positions, and the acetonitrile molecule in fram-position to the W=N —Cl group. Bond lengths WN = 172 and NCI -161 pm; bond angle WNC1 = 175.5°. 
  Reference    Z. Naturforsch. 43b, 677—681 (1988); eingegangen am 26. Januar 1988 
  Published    1988 
  Keywords    Synthesis, IR Spectra, X-Ray, N-Chloro-Nitrene-Tungsten Tetrachloride, Acetonitrile Adduct 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-0677.pdf 
 Identifier    ZNB-1988-43b-0677 
 Volume    43 
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