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1985 (316)
21Author    Bernhard Czeska, Kurt DehnickeRequires cookie*
 Title    [P(C 6 H 5 ) 4 ] 2 S 8 : Synthesis and IR Spectrum  
 Abstract    [P(C 6 H 5)4] 2 S g was prepared from Na 2 S 4 and PPh 4 Cl in ethanol solution and characterized by its IR spectrum. 
  Reference    (Z. Naturforsch. 40b, 120—121 [1985]; eingegangen am 28. September 1984) 
  Published    1985 
  Keywords    Tetraphenylphosphonium Octasulfide, Synthesis, IR Spectra 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0120_n.pdf 
 Identifier    ZNB-1985-40b-0120_n 
 Volume    40 
22Author    Horst Sabrowsky, Petra Mertens, FritzOtto DönhoffRequires cookie*
 Title    Neues über ternäre Interalkalimetalloxide und AlkaIithallium(I)-oxide News About Ternary Inter Alkaline Metal Oxides and Alkalinethallium(I)oxides  
 Abstract    Ternary Inter Alkaline Metal Oxides, Alkalinethallium(I)oxides, X-Ray Besides KNaO and RbNaO, KLiO is the third example of hitherto unknown and unexpected in-teralkaline metal oxides. The X-ray investigation of the orthorhombic KLiO (Z=8) shows a new struc-ture with separated layers of 2 [LiO]^ anions in which every lithium atom is co-ordinated by a triangle of three oxygens. The compounds KTIO, RbTIO and CsTIO are al-ready known. Now serveral new ternary alkaline oxides with monovalent thallium have been ob-tained. In the Na 2 0—T1 2 0 system the red com-pounds NaTIO and Na 3 T10 2 were found. Further-more KT1 3 0 2 , RbTl 3 0 2 and CST1 3 0 2 have been pre-pared. Their unit cells (Z=3) correlate to the unit cell of hexagonal T1 2 0 (Z—6). 
  Reference    (Z. Naturforsch. 40b, 122—123 [1985]; eingegangen am 12. September 1984) 
  Published    1985 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0122_n.pdf 
 Identifier    ZNB-1985-40b-0122_n 
 Volume    40 
23Author    Synthesis, Crystal Structure Of, HerbertW. Roesky, Hartmut Hofmann, Mathias Noltemeyer, GeorgeM. SheldrickRequires cookie*
 Title    Synthese und Kristallstruktur von l,l,l,3,3»3-Hexafluor-2-propylamino- l-thiooxamid +-Hexafluoro-2-propylamino- 1-thiooxamide"  
 Abstract    Dithiooxamide 1 reacts with hexafluoroacetone 2 at room temperature to yield 1,1,1,3,3,3-hexafluoro-2-propylamino-l-thiooxamide 3 and sulfur. The modes of formation of the bis(trifluoromethyl)-methyl group from hexafluoroacetone, the migra-tion of oxygen and the elimination of sulfur are not clear. Crystals of 3 are monoclinic, space group Cc, with a = 2865.3(13), b = 924.4(9), c = 702.9(6) pm, ß = 93.3(7)°. The structure was re-fined to R — 0.067 from 614 reflections. 
  Reference    (Z. Naturforsch. 40b, 124—126 [1985]; eingegangen am 13. August 1984) 
  Published    1985 
  Keywords    Dithiooxamide, Hexafluoroacetone, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0124_n.pdf 
 Identifier    ZNB-1985-40b-0124_n 
 Volume    40 
24Author    Udo Kunze, Andreas BrunsRequires cookie*
 Title    Phosphinsubstituierte Chelatliganden, XII [1] Metallinduzierte E/Z-Isomerisierung an Rheniumcarbonyl-Komplexen mit Phosphinothioformamid-und -thioformimidat-Liganden Phosphine-Substituted Chelate Ligands, XII [1] Metal-Induced E/Z-Isomerisation of Rheniumcarbonyl Complexes with Phosphino- thioformamide and -thioformimidate Ligands  
 Abstract    The coordination of tertiary phosphinothioform-amides and the isomeric S-alkyl phosphinothioform-imidates to BrRe(CO) 5 gives the /ac-bromotricar-bonylrhenium complexes la, b and 2a, b with P,S-chelate ligands. Unlike the analogous manganese complexes, the NMR spectra of dissolved lb and 2a, b show a splitting of the N-alkyl ('H, 13 C) and phosphorus signals indicating E/Z isomerisation of the ligands. 
  Reference    (Z. Naturforsch. 40b, 127—128 [1985]; eingegangen am 7. August/5. September 1984) 
  Published    1985 
  Keywords    E/Z-Isomerisation, NMR Spectra, Rhenium Complexes, Tertiary Phosphinothioform-amides, S-Alkyl Phosphinothioformimidates 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0127_n.pdf 
 Identifier    ZNB-1985-40b-0127_n 
 Volume    40 
25Author    Nadia Sobhy, Ibrahim, Usef Kamal, SuzanIbrahim Sadek, Mohamed Aziz, Elnagdi HilmyRequires cookie*
 Title    A Novel Synthesis of Heterocyclic /?-Enaminoamides: The Reaction of Halomethyl Acet-p-toluidide with Isothiocyanates and with Isocyanates  
 Abstract    A novel synthesis of thiophene and furan /3-enaminoamides via the reaction of halomethyl acet-p-toluidide with isothiocyanates and isocya-nates were reported. 
  Reference    (Z. Naturforsch. 40b, 129—131 [1985]; received April 4 1984) 
  Published    1985 
  Keywords    Bromomethyl Acet-p-toluidide, Isocyanate, Isothiocyanates, Enaminothiophene, Enaminofuran 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0129_n.pdf 
 Identifier    ZNB-1985-40b-0129_n 
 Volume    40 
26Author    Francesco Ciardelli, Paolo PerticiRequires cookie*
 Title    Structure and Reactivity of Aromatic Polymers/Ruthenium Catalysts  
 Abstract    Previously prepared (J. Mol. Catalysis 11, 353 (1981)) polystyrene/ruthenium systems have been examined by EXAFS, TEM, IR and Raman spectroscopy. A structure based on small metal clusters bound to the polymer by single ruthenium-arene binding is proposed. The general validity of the approach has been confirmed by preparing a similar product when starting with poly-1-vinylnaphthalene in the place of polystyrene. Both systems are active for the hydrogenation of a large variety of unsaturated groups such as olefinic double bonds, mononuclear aromatic hydrocarbons, ketones, nitriles, nitroaromatic com-pounds and oximes. Catalytic activity, chemio-and stereoselectivity are discussed in terms of the proposed structure. 
  Reference    Z. Naturforsch. 40b, 133—140 (1985); received September 13 1984 
  Published    1985 
  Keywords    Hydrogenations, Heterogeneous Catalysts, Ruthenium/Aromatic Vinyl Polymer Systems, Ruthenium/Arene Systems 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0133.pdf 
 Identifier    ZNB-1985-40b-0133 
 Volume    40 
27Author    Wilhelm Volker, Dahlhoff, Angelika GeisheimerRequires cookie*
 Title    Organoboron-Monosaccharides, XIV [1] Routes to a-and /3-D-Mannofuranosyl ß-D-Mannofuranosides  
 Abstract    a/y3-D-Mannofuranosyl yß-D-Mannofuranosides, Sodium-organooxytriethylborate, Organooxy-tri-n-butylstannane Intermediates Stereoselective glycosylations of 2,3:5,6-di-0-ethylboranediyl-a-D-mannofuranosyl bromide (1) by two independent routes involving 1-O-tri-n-butyl-stannyl and 1-O-triethylborate a-D-man-nofuranosyl derivatives give a-D-mannofuranosyl /3-D-mannofuranoside (8a) after deprotection. /3-D-Mannofuranosyl ß-D-mannofuranosides can be prepared by reaction of 1 with the sodium triethylborate derivative of 2,3:5,6-di-0-isopropylidene-/3-D-mannofuranose (11) and by reacting 1 with hexabutyldistannoxane. The latter approach allows the synthesis of /3-D-mannofuranosyl ß-D-mannofuranoside (8b) after total deprotection. 
  Reference    Z. Naturforsch. 40b, 141—149 (1985); received October 15 1984 
  Published    1985 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0141.pdf 
 Identifier    ZNB-1985-40b-0141 
 Volume    40 
28Author    Gerhard Erker, Klaus Engel, Carl Krüger, Yi-Hung Tsay, Edmond Samuel, Pierre VogelRequires cookie*
 Title      
 Abstract    ,3-Bis(methylen)bicycIo[2.2.2]octan)zirconocen: Synthese, Struktur und elektrochemische Reduktion (2,3-Bis(methylene)bicyclo[2.2.2]octane)zirconocene: Synthesis, Structure, and Electrochemical Reduction (s-cw-Conjugated diene)zirconocene Complexes, Diene Metallocene Automerization, Diene Zirconocene Electrochemical Reduction Photolysis of diphenylzirconocene and 2,3-bis(methylene)bicyclo[2.2.2]octane in toluene at —25 °C yields biphenyl and (2,3-bis(methylene)bicyclo[2.2.2]octane)zirconocene (lg) (67.5% isolated yield), lg exhibits dynamic NMR spectra indicating rapid alternation of diene faces coordinated to zirconium (ring-flip mechanism). This degenerate intramolecular rearrangement is characterized by an extremely low activation barrier (JG 4= _ 131 « C = 7.1 ± 0.3 kcal/mol). lgcrystal-lizes in space group PI with a = 7.215(1) A, b = 9.654(1) A, c = 11.831(1) A, a = 94.97(1)°, ß = 91.81(1)°, and y = 103.22(1)°. The X-ray structure determination reveals a pronounced metal alkyl character of the (diene)ZrCp 2 moiety. Accordingly, lg is easily reduced electrochemically to give a Zr(III) radical anion (7) observed by esr (g = 1.990; a(H) -2.976 G; a(Zr) = 18.36 G). Dienkomplexe "früher" Übergangsmetalle unter-scheiden sich in vielen Eigenschaften von den Ver-bindungen konjugierter Diolefine der elektronen-reicheren Elemente der rechten Seite des Perioden-systems [1, 2]. Eine besondere Stellung nehmen da-bei die Komplexe der gewinkelten Metallocene Bis(?7-cyclopentadienyl)zirconium und -hafnium ein. Sie zeichnen sich nicht nur durch die Bildung stabi-ler, isolierbarer einkerniger (s-£ram , -?7 4 -Dien)metall-Komplexe aus, auch die (s-c/5-Dien)metallocen-Iso-meren zeigen sehr ungewöhnliche Struktureigen-schaften und Chemie [3, 4], Die bisher bekannten substituierten (s-c/s-Buta-dien)zirconocen-und -hafnocen-Verbindungen (1) besitzen sämtlich einen ausgeprägten Metallalkyl-charakter. Von den für Dien-Übergangsmetallkom-plexe möglichen Strukturalternativen decken sie das Kontinuum zwischen den Grenzen eines 
  Reference    Z. Naturforsch. 40b, 150—157 (1985); eingegangen am 17. September 1984 
  Published    1985 
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 Identifier    ZNB-1985-40b-0150 
 Volume    40 
29Author    Gerhard Fink, RichardWolfgang Fenzl, MynottRequires cookie*
 Title    Ethylene Insertion with Soluble Ziegler Catalysts: Direct Insight into the Reaction Using Enriched 13 C 2 H 4 and 13 C NMR Spectroscopy II. The System Cp2TiMeCl/AlMeCl 2 / 13 C 2 H4  
 Abstract    The elementary processes involved in the polymerization of ethylene by soluble Ziegler cata-lysts of the type Cp 2 TiMeCl/AlMeCl 2 have been studied by 13 C NMR spectroscopy. Using 13 C-enriched ethylene, detailed information was obtained directly on the system in the course of the polymerization. No spectroscopic evidence was found for precoordination of the monomer. The development of the oligomer distribution, which could be followed spectroscopically, proves that the mechanism proposed by Olive cannot be correct. These experiments show conclusively that the ethylene is inserted into the titanium-carbon bond. 
  Reference    Z. Naturforsch. 40b, 158—166 (1985); received October 25 1984 
  Published    1985 
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 Identifier    ZNB-1985-40b-0158 
 Volume    40 
30Author    Thomas Kuhlmann, Walter SiebertRequires cookie*
 Title    Synthese eines Hexadecker-Sandwichkomplexes [1] Synthesis of a Hexadecker Sandwich Complex [1]  
 Abstract    Allylnickel Tripledecker, Bis(2,3-dihydro-l,3-diborol)nickel, Hexadecker Two routes have been studied to obtain the first hexadecker sandwich complexes 4. The reaction between the ^ 3 -allyl tetradecker 2 b and the cobalt sandwich 3 b in refluxing mesitylene leads to red-violet diamagnetic 4bb in 7% yield. Bis(allyl)nickel and the cyclopentadienylcobalt(2,3-dihydro-l,3-diborol) 3b form the triple-decker ?/ 3 -allylnickel(w,^ 5 -dihydro-l,3-diborolyl)-cobalt(?; 5 -cyclopentadienyl) 9b, which reacts at 160 °C with the bis(2,3-dihydro-l,3-diborol)nickel sandwich 10c to give 4bc (21%) and the tetra-decker 7b (69%). The constitution of the new complexes is derived from NMR and mass spectra. 
  Reference    Z. Naturforsch. 40b, 167—170 (1985); eingegangen am 28. September 1984 
  Published    1985 
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 Identifier    ZNB-1985-40b-0167 
 Volume    40 
31Author    Herbert Lehmkuhl, Johannes Elsäßer, Reinhard Benn, Barbara Gabor, Anna Rufińska, Richard Goddard, Carl KrügerRequires cookie*
 Title    Ein-und zweikernige Phosphorinylnickel-Komplexe Mono-and Binuclear Phosphorinylnickel Complexes  
 Abstract    [Bis(2-4?7-phosphorinyl)nickel]-P,P'-(77 2 -alkene)nickel, Valence Isomerization, Alkene Rotation, A 5 -Phosphorin-l-ylnickel Complexes The ethylene molecule in the binuclear complex [bis(2-4?7-phosphorinyl)nickel](?7 2 -ethylene)-P,P'-nickel (1) is displaced by 1-alkenes in an equilibration reaction to give the corresponding (rj 2 -l-alkene)nickel complexes 2—5. The NMR spectra of the octene complex 3 and the propene complex 6 are temperature dependent because of valence isomerization in the phosphorinyl group and rotation of the olefin. The binuclear structure is not maintained upon displacement of the ethylene by butadiene or isoprene. One nickel atom is displaced as the dodecatrienediylnickel complex 9 and the remaining bis(phosphorinyl)nickel fragment B reacts with insertion of the diene into one allyl-Ni bond to give 7 resp. 8. The molecular structure of 7 was determined by X-ray crystallography. 
  Reference    Z. Naturforsch. 40b, 171—181 (1985); eingegangen am 12. Juni 1984 
  Published    1985 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0171.pdf 
 Identifier    ZNB-1985-40b-0171 
 Volume    40 
32Author    Heinz Martin, Helmut BretingerRequires cookie*
 Title    Bis-und Tris-aluminiumalkan-Verbindungen als Zwischenprodukte bei der Auflösung von Aluminium mit Olefinen in Gegenwart von Aluminiumtrichlorid oder Alkylaluminiumdichlorid Bis-and Tris-aluminum-alkane Compounds as Intermediates During the Dissolution of Aluminum Metal with Olefins in the Presence of Aluminum Trichloride or Alkyl Aluminum Dichloride  
 Abstract    Bis-and Tris-aluminum-alkane Compounds, Aluminum Aluminum can be dissolved by ethylene in the presence of aluminum trichloride to form primarily bis-(dichloro-aluminum)-ethanes (1) and (2) or in the presence of ethyl aluminum dichloride to form chloro-aluminum-ethyl-(dichloroaluminum)-ethane (3) and/or a tris-aluminum compound C1 2 A1-C 2 H4-A1(C1)-C2H4-Al(Cl)Et (4). 1-4 react further with olefins, with elimi-nation of alkyl aluminum dichloride and/or dialkyl aluminum chloride, which are practically inert towards olefins. The C 2 H 4 -bridge is available to the growth and displacement reaction with olefins. 
  Reference    Z. Naturforsch. 40b, 182—186 (1985); eingegangen am 30. Oktober 1984 
  Published    1985 
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 Identifier    ZNB-1985-40b-0182 
 Volume    40 
33Author    Roberto Millini, Horst Kisch, Carl KrügerRequires cookie*
 Title    Iron Carbonyl Assisted Synthesis of l,2-Diazepin-3-ones from Cyclic Diazenes and Alkynes [1]  
 Abstract    , 2a, c are prepared by an iron carbonyl mediated reaction sequence from alkynes and cyclic 1,2-diazenes. The latter are first converted into hexacarbonyl diiron complexes which react with two molecules of an alkyne to afford tricyclic carbonyl iron compounds I —III. Oxidative degradation with bromine leads to these novel heterocycles whose structure is confirmed by an X-ray analysis of lb. 
  Reference    Z. Naturforsch. 40b, 187—192 (1985); received October 15 1984 
  Published    1985 
  Keywords    Diazepinones, Diazenes, Alkynes, Carbonyl-Iron Assistance Bicyclic l, 2-diazepin-3-ones la—c 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0187.pdf 
 Identifier    ZNB-1985-40b-0187 
 Volume    40 
34Author    Richard Neidlein, Reiner Gottfried, Alfred Gieren, Carsten-P Kaerlein, Thomas HübnerRequires cookie*
 Title    Kupplungsreaktionen von Diazoniumsalzen mit 3-ferf-Butoxy- l,6-methano[10]annulen und Röntgenstrukturanalyse eines Vertreters Coupling Reactions of Diazonium Salts with 3-terr-Butoxy-l,6-methano[10]annulene and X-Ray Structure Analysis of one Compound  
 Abstract    The syntheses of 5a—c by coupling reactions of 3-terr-butoxy-l,6-methano[10]annulene with different aryldiazonium salts as well as their spectroscopic properties are described; an X-ray structure analysis of 5c is reported. 
  Reference    Z. Naturforsch. 40b, 193—198 (1985); eingegangen am 20. August 1984 
  Published    1985 
  Keywords    Syntheses with Coupling Reactions, 1, 6-Methano[10]annulenylarylhydrazones, X-Ray, Bonding Relationships 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0193.pdf 
 Identifier    ZNB-1985-40b-0193 
 Volume    40 
35Author    KlausR. Pörschke, Richard Mynott, Klaus Angermund, ++, Carl KrügerRequires cookie*
 Title    Neue Bis(phosphan)-nickel(0)-alkin-Komplexe New Bis(phosphane)-nickel(0)-alkyne Complexes  
 Abstract    (Me 3 P)2Ni(C 2 H4) (5) and (dmpe) 2 Ni2(C 2 H4)3 (6) react with various alkynes including ethyne (acetylene) and 1-alkynes to form the crystalline compounds (Me 3 P) 2 Ni(C 2 RR'), (dmpe)Ni(C 2 RR'), and (dmpe)2Ni 2 (C 2 R2) 2 (R.R' = H, Me, Ph). Structural assignments were made on the basis of : H, I3 C, and 31 P NMR data. The crystal and molecular structure of (dmpe)Ni(C 2 Ph 2) (17) has been determined by X-ray crystallography. 
  Reference    Z. Naturforsch. 40b, 199—209 (1985); eingegangen am 15. Oktober 1984 
  Published    1985 
  Keywords    Alkynes, Nickel(O), Phosphanes, NMR Spectra, X-Ray 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0199.pdf 
 Identifier    ZNB-1985-40b-0199 
 Volume    40 
36Author    Kenji Sano, Takakazu Yamamoto, Akio YamamotoRequires cookie*
 Title    Preparation and Reactions of i7 3 -Allylcarboxylatoruthenium(II)  
 Abstract    ?7 3 -Allyl, Metallacyclic Compound, Ruthenium Complex Reactions of (l,5-cyclooctadiene)(l,3,5-cyclooctatriene)ruthenium(0) with 3-butenoic acid in the presence of tertiary phosphines, PR 3 , afford ^ 3 -allylcarboxylatoruthenium(II) complexes for-mulated as (PR3)2RUCH2HI:CH^CHCOÖ (1 (PR3 = PPh 3), 2 (PR3 = P(C6H4-P-OCH3)3). The reaction of 1 with carbon monoxide gives the complex (PPh 3) 2 (CO)RuCH 2 in:CH—CHCOO while reaction with Br 2 or I 2 leads to ring closure of the organic ligand to afford 2-butenolide. 
  Reference    Z. Naturforsch. 40b, 210—214 (1985); received September 25 1984 
  Published    1985 
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 Identifier    ZNB-1985-40b-0210 
 Volume    40 
37Author    Nien Man, Henryk Schuchmann, Zegota, Clemens Von SonntagRequires cookie*
 Title    Acetate Peroxyl Radicals, 0 2 CH 2 C0;: A Study on the y-Radiolysis and Pulse Radiolysis of Acetate in Oxygenated Aqueous Solutions  
 Abstract    Hydroxyl radicals from the radiolysis of N 2 0/0 2 (4:1 v/v)-saturated aqueous solutions have been reacted with acetate ions (1CT 2 M). As measured by pulse radiolysis, the resulting "CH 2 C0 2 radicals react with oxygen yielding the corresponding peroxyl radicals, 0 2 CH 2 C0 2 (k = 1.7 x 10 9 M-V 1). These peroxyl radicals decay bimolecularly (2k = 1.5 x 10 8 M _1 s _1) giving rise to the products (G values in brackets) glyoxylic acid (2.7), glycolic acid (0.7), formaldehyde (1.4), carbon dioxide (1.4), organic hydroperoxide (0.7) and hydrogen peroxide (2.5). Oxygen is consumed with a G value of 5.3. Aided by data from pulse radiolysis it is concluded that the intermediate tetroxide formed upon the bimolecular decay breaks down by various routes to yield: (i) hydrogen peroxide and two molecules of glyoxylic acid (ca. 27%); (ii) oxygen, glycolic acid and glyoxylic acid (ca. 25%); (iii) hydrogen peroxide and two molecules of formaldehyde, carbon dioxide and OH~ (25%). These reactions do not involve free radicals as intermediates; (iv) There is some 0 2 (G = 0.5) formed in the decay of the peroxyl radicals, which is attributed to the decay of intermediate oxyl radicals (tetroxide —* • 0 2 + 2 0CH 2 C0 2) by 1,2-H shift, oxygen addition and H0 2 elimination, a reaction sequence which gives rise to glyoxylic acid (10%); (v) The reaction of 0 2 with the organic peroxyl radical yields the hydroperoxide (13%). Reaction (iii) is a novel peroxyl radical reaction. 
  Reference    Z. Naturforsch. 40b, 215—221 (1985); received October 24 1984 
  Published    1985 
  Keywords    Acetic Acid, Peroxyl Radicals, Oxyl Radicals, Superoxide Radicals, Pulse Radiolysis 
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 Identifier    ZNB-1985-40b-0215 
 Volume    40 
38Author    Mohamed Yalpani, WernerE. KlotzbücherRequires cookie*
 Title    Transformations in Thin Solid Layers: The Reversible Polymerization-Depolymerization of 2,6-Di-n-propyl- l,3>5,7-tetraoxa-2,6-dibora-4,8-octalindiones at Low Temperatures  
 Abstract    The course of Aggregation of molecules of the title compound (lb) through different, spectro-scopically discernible and chemically identifiable forms of associations could be followed by matrix isolation and thin film infrared and UV-visible spectroscopy. It was found that molecules of lb in thin films form clusters which at low temperatures interact weakly, probably through the carbonyl oxygens of one and the boron atoms of the neighbouring molecules. On warming to 260 K this association gradually takes the form of more defined chelate bonds, probably with ordered three-dimensional intermolecular structures. Above this temperature spontaneous for-mation of crystallites of the previously reported 'hot' and 'cold' modifications was observed. Studies with films of varying thickness indicate an interdependence of crystallite size and lattice energies. 
  Reference    Z. Naturforsch. 40b, 222—228 (1985); received September 24 1984 
  Published    1985 
  Keywords    Solid State Reaction, Matrix Isolation, Aggregation, Phase Transformation, Microcrystals 
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 Identifier    ZNB-1985-40b-0222 
 Volume    40 
39Author    KurtO. KleppRequires cookie*
 Title    Darstellung und Kristallstruktur von Tl 2 TiS 4 : Ein Perthiotitanat(IV) mit i-[TiS 4 2 "]-Ketten Preparation and Crystal Structure of Tl 2 TiS 4 : A Perthiotitanate(IV) with ^-[TiS 4 2 ~]-Chains  
 Abstract    Tl 2 TiS 4 is orthorhombic, space group Pbca, with a = 22.176(7), b = 9.484(4), c = 6.3977(9) A, Z = 8. The crystal structure was solved by direct methods and refined to a conventional R of0.058 for 704 reflections with I^3a(I). The crystal structure is characterized by infinite perthioanions, i-[TiS 4/2 (S 2) 2 -], which are separated by Tl + -cations. The anion chains are built up by distorted octahedra which share two skew edges to form infinite cis-chains running along [001], The two unshared S-atoms of each octahedron are connected via a S —S-single bond of 2.10 A length. The crystal structure is described as a mixed packing of TI-and S-atoms, composed of puckered T1S 2 -layers, in which the Ti-atoms occupy the octahedral interstices. The relationship of the ^-[XiS^ -]-chains to the anionic groups of Cs 2 TiS 3 is discussed. 
  Reference    Z. Naturforsch. 40b, 229—234 (1985); eingegangen am 27. September 1984 
  Published    1985 
  Keywords    Thallium Perthiotitanate, Preparation, Crystal Structure 
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 Identifier    ZNB-1985-40b-0229 
 Volume    40 
40Author    Klaus Wolfer, Hans-Dieter Hausen, Herbert BinderRequires cookie*
 Title    Ein neues borhaltiges Anion mit dem Adamantangerüst CB 5 S 4 A New Boron-Containing Anion with the Adamantane Skeleton CB 5 S 4  
 Abstract    Boron-Sulfur-Carbon-Adamantane Hydroboration of CS 2 with NaB 3 H 8 yields the new compound Na[CH 2 (BH 2)5S 4 ], isolated as the tri-dioxanat. The anion has the adamantane skeleton CB 5 S 4 . The crystal structure of the analog-ous compound (C 6 H 5) 4 P[CH 2 (BH 2) 5 S 4 ] was determined from diffractometer data and refined to R = 0.043. The tetragonal unit cell (space group P 4In) contains two formula units (a — b — 1351.7 pm; c = 790.0 pm). 
  Reference    Z. Naturforsch. 40b, 235—239 (1985); eingegangen am 8. Oktober 1984 
  Published    1985 
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 Identifier    ZNB-1985-40b-0235 
 Volume    40 
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