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1999[X]
101Author    G. Erhard Bringm, DanielaH. Erzberga, Geo Adam, Friedhelm Balkenhohlb, Joachim PaustbRequires cookie*
 Title    A Short and Productive Synthesis of (R)-«-Lipoic Acid  
 Abstract    Lipoic Acid, Yeast Reduction, Enantioselective Hydrogenation, Regioselective Reduction (R)-a-Lipoic acid is synthesized in seven steps from the base chemicals methyl acetoace-tate or M eldrum's acid and monom ethyl adipate. The key steps are the introduction of the stereogenic center by fermentative or hom ogeneously catalyzed hydrogenation of 3-oxo-octanedioic acid diester to (3S)-3-hydroxyoctanedioic acid diester and its regioselective re­ duction to (6S)-6 ,8-dihydroxyoctanoic acid ester. The overall yield of (R)-a-lipoic acid, start­ ing from 3-oxooctanedioic acid diester, is 40%. Results and Discussion The 3-oxo diesters 4 have not been employed 
  Reference    Z. Naturforsch. 54b, 655—661 (1999); received Decem ber 4. 1999 
  Published    1999 
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 Identifier    ZNB-1999-54b-0655 
 Volume    54 
102Author    Steffen Runge3, MathiasO. Senge3, Karin Ruhlandt-SengebRequires cookie*
 Title    5,10,15,20-Tetrakis(diphenylmethyl)porphyrin -A Nonplanar Porphyrin with Intermediate Degree of Ruffling  
 Abstract    The title compound was prepared by condensation of pyrrole and diphenylacetaldehyde in 16% yield. Based on spectroscopic data, the free base porphyrin exhibits a nonplanar macrocycle in solution with a degree of distortion between that of 5,10,15,20-tetracyclohexyl-porphyrin and 5,10,15,20-tetra(r-butyl)porphyrin. A crystal structure determination of the cobalt(II) complex reveals a ruffled macrocycle conformation with an average out-of-plane displacement of the m eso carbon atoms by 0.55 A. 
  Reference    Z. Naturforsch. 54b, 662 (1999); received February 17 1999 
  Published    1999 
  Keywords    Porphyrins, Steric Strain, Cobalt Porphyrins, Crystal Structure, Conformation 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0662.pdf 
 Identifier    ZNB-1999-54b-0662 
 Volume    54 
103Author    Thomas Kurz, D. Etlef GeffkenRequires cookie*
 Title    Synthesis of 3-Amino(alkoxy)-2,4-dioxo-l,3-oxazolidine-5-carboxylates from Tartronic Esters  
 Abstract    Tartronic Esters, l,l'-C arbonyl-di-(l,2,4-triazole), 3-A m ino-2,4-dioxo-l,3-oxazolidine-5-carboxylates, 3-A lkoxy-2,4-dioxo-l,3-oxazolidine-5-carboxylates The reaction of tartronic esters (la-d) with l,l'-carbonyl-di-(l,2,4-triazole), hydrazines or hydroxylamines produces 3-amino/3-alkoxy(aralkoxy)-2,4-dioxo-l,3-oxazolidine-5-carboxylic esters (5,6) which are structurally related to the fungicides Famoxadone (I) and Chlozolinate (II). Under suitable conditions the carboxylic ester of 6 can be converted to a carboxamide (7), carbohydrazide (8) or carbohydroxamic acid (9). 
  Reference    Z. Naturforsch. 54b, 667—6 (1999); eingegangen am 30. Dezem ber 1998 
  Published    1999 
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 Identifier    ZNB-1999-54b-0667 
 Volume    54 
104Author    SanaaM. EldinRequires cookie*
 Title    Cyanothioacetamide and its Derivatives in Heterocyclic Synthesis: A New Route for the Synthesis of Several Pyridine and Thieno[2,3-b]pyridine Derivatives and their Biological Evaluation  
 Abstract    Several new pyridine and thieno[2,3-b]pyridine derivatives were synthesized via the reac­ tions of some pyridinethiones, obtained by the action of acetylacetone on some thiocarbox-amidocinnamonitriles, with halogenated esters and ketones. Structures were established based on elemental and spectral data. All the synthesized compounds were tested for their biological activity. 
  Reference    Z. Naturforsch. 54b, 674 (1999); received N ovem ber 9 1998 
  Published    1999 
  Keywords    Pyridines, Thieno[2, 3-b]pyridines, Cyanothioacetamide, Thiocarboxamido-cinnamonitriles, Michael Condensations 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0674.pdf 
 Identifier    ZNB-1999-54b-0674 
 Volume    54 
105Author    Axel Lifferth3, IsabelB. Ahnera, Ut Helm, Lackner, M. Artina SchäferbRequires cookie*
 Title    Synthese und Struktur von Prolinring-modifizierten Actinomycinen des X-Typs Synthesis and Structure of Proline Ring Modified Actinomycins of the X-Type  
 Abstract    The first total synthesis o f actinomycins containing L-4-hydroxyproline (1) and the separa­ tion and NM R spectroscopic assignment o f the regioisomers X (V* and iso-X0/i (lc, le) are described. The synthetic X 0/j proves, that the oxidized proline ring of the natural actinomycins 
  Reference    Z. Naturforsch. 54b, 681—6 (1999); eingegangen am 15. Januar 1999 
  Published    1999 
  Keywords    Antibiotics, Actinomycins, Synthesis, Crystal Structure, NM R Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0681.pdf 
 Identifier    ZNB-1999-54b-0681 
 Volume    54 
106Author    Hong Zhanga, Yali Wanga, Rene Thiirmera, Khalid Parvez, Iqbal Choudhary, A. Tta-, Ur-R Ahm Anb, Wolfgang Voelter3Requires cookie*
 Title    Neighbouring Group Participation of C-6 Substituents of Glucose Derivatives on the Stereoselectivity of the N-Glycosidic Linkage of Glycopeptides  
 Abstract    The first example of a glycopeptide with a direct /V-a-glycosidic linkage between the trisac­ charide and the amino acid residue was found in the glomerular basement membrane of rats. In connection with the total synthesis of nephritogenoside, glycosyl azides with different protecting groups and carbohydrate chain lengths are synthesized, reduced to the corre­ sponding glycosyl amines and coupled with Z-Asp-O Bzl. Remarkable differences in the a:ß ratio of the condensation products are observed, caused by neighbouring group participation. 
  Reference    Z. Naturforsch. 54b, 692—6 (1999); received February 2. 1999 
  Published    1999 
  Keywords    Oligosaccharide Synthesis, Glycopeptides, Neighbouring Group Participation 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0692.pdf 
 Identifier    ZNB-1999-54b-0692 
 Volume    54 
107Author    N. Orbert Kuhn, Heike Kotowski, Manfred SteimannRequires cookie*
 Title    Synthese und K ristallstruktur von 3.6-Di-terf-butylpyridazin Synthesis and Crystal Structure of 3.6-Di-rm-butylpyridazine  
 Abstract    Heterocycles, Pyridazines, X-Ray Data 3,6-Di-rm-butylpyridazine (4) is obtained from 2,2,7,7-tetramethyloctan-3,6-dione (2) and anhy­ drous hydrazine in good yield. Its X-ray structure is reported. 
  Reference    Z. Naturforsch. 54b, 699—7 (1999); eingegangen am 5. Februar 1999 
  Published    1999 
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 Identifier    ZNB-1999-54b-0699_n 
 Volume    54 
108Author    Bernd Aechter, Kurt Polborn, Volker Weinrich, Wolfgang BeckRequires cookie*
 Title    /?-Tolyl(trimethylsiIylethynyl)sulfone as Synthon for the Synthesis of Cp(OC)2M -C =C SiM e3 (M = Fe, Ru). Molecular Structure of Cp(OC)2Fe-C =C SiM e3  
 Abstract    Alkynyl Complexes, X-Ray Data, /?-Tolyl(trimethylsilylethynyl)sulfone The alkynyl complexes Cp(OC)2M -C = C S iM e 3 (M = Fe, Ru) are formed from p -to ly lS 0 2C = CSiMe3 and [Cp(OC)2M ]'N a +. The structure of Cp(OC)2F e-C = C S iM e 3 was determined by X-ray diffraction. 
  Reference    Z. Naturforsch. 54b, 701 (1999); received February 4 1999 
  Published    1999 
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 Identifier    ZNB-1999-54b-0701_n 
 Volume    54 
109Author    BemdW. Rackm, SergeiV. PonomarevbRequires cookie*
 Title    Decomposition of Ethoxyethynyl(trimethyl)tin -Studied by 119Sn and 13 C NMR Spectroscopy  
 Abstract    A The thermally induced decomposition o f ethoxyethynyl(trimethyl)tin (1) was studied by ll9Sn NM R which revealed the formation o f bis(trimethylstannyl) ketene (2) as the major product, bis(trimethylstannyl) acetic acid ethyl ester (3) as a minor product, and a small amount o f tetramethyltin (4). Full NM R data sets, including coupling constants and isotope induced chemical shifts 1 _ \ 12 13C(1 l9Sn) are provided for 1 -3 . The first example o f ultra-high resolution " 9Sn NM R is shown. 
  Reference    Z. Naturforsch. 54b, 705 (1999); received February 23 1999 
  Published    1999 
  Keywords    lkynes, Ketenes, Tin, NMR Data 
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 Identifier    ZNB-1999-54b-0705 
 Volume    54 
110Author    Rolf-Dieter Hoffmann3, Dirk Kußmanna, Ute Ch, Rainer Rodewald3, Pöttgen3, Carsten Rosenhahnb, BerndD. MoselbRequires cookie*
 Title    New Stannides CaTSn2 (T = Rh, Pd, Ir) and Ca2Pt3 Sn5 -Synthesis, Structure and Chemical Bonding  
 Abstract    New stannides CaTSm (T = Rh, Pd, Ir) and Ca2P hSn5 were prepared as single phase materials by a reaction o f the elements in glassy carbon crucibles under flowing purified argon. The four compounds were investigated by X-ray diffraction both on powders and single crystals and their structures were refined from single crystal data. The stannides CaTSn2 (T = Rh, Pd, Ir) adopt 
  Reference    Z. Naturforsch. 54b, 709 (1999); received February 25 1999 
  Published    1999 
  Keywords    Intermetallic Calcium Compounds, Crystal Structure, Mössbauer Spectroscopy, Chemical Bonding 
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 Identifier    ZNB-1999-54b-0709 
 Volume    54 
111Author    Isabel Díaza, Vicente Fernández3, VitalyK. Belskyb, Jose Luis, M. Artínez0Requires cookie*
 Title    Synthesis and Structural Study of the Thermochromic Compounds Bis(2-amino-4-oxo-6-methylpyrimidinium) Tetrachlorocuprate(II) and Bis(2-amino-4-chloro-6-methylpyrimidinium) Hexachlorodicuprate(II)  
 Abstract    The compound bis(2-am ino-4-oxo-6-methylpyrimidinium) tetrachlorocuprate(II) 1 contains CuCU2-square-planar anions, and bis(2-am ino-4-chloro-6-m ethylpyrim idinium) hexachlorod-icuprate(II) 2 quasi-planar CU2CI62-anions. Both compounds show thermochromic behaviour. This phenomenon has been studied by X-ray crystallography at variable temperature, with the result that no major change is observed in the geometry o f the copper atom. Thus it is possible to assume som e influence o f the hydrogen bonds and o f the different geometries o f interme­ diate states on the color o f the compounds due to the modifications provoked in the L —>M charge transfer and in the energy o f the metal d-d transitions. Magnetic measurements o f the compounds give information on magneto-structural correlations. Compound 1 is ferromagnetic (Tc = 20 K) due to the perpendicular arrangement o f the square anions that allows exchange pathways only via Cu-Cl -Cu , H-bonding or cationic n electron interactions. Compound 2 shows a very complicated behavior at low temperature with local antiferromagnetic fluctua­ tions. Crystal data: 1 CioHioNftC^CUCu, triclinic, P i; 393(2) K: a = 11.053(2), b = 11.334(2), c = 14.038(3) (Ä), a = 95.76(3), ß = 101.35(3), 7 = 9 0 .1 5 (3) 0 ; 293(2) K: a = 11.022(2), b = 11.289(2), c = 14.001(3) (A), a = 95.86(2), ß = 101.34(2), 7 = 9 0 .0 9 (3) 0 ; 155(2) K: a = 11.008(2), b = 11.231 (2), c = 13.967(3) (A), a = 95.86(2), ß = 101.37(2), 7 = 8 9 .9 9 (2) 0 ; Z = 4. 2 (C5H7N 3C l3Cu)2, monoclinic, P 2,/c; 293(2) K: a = 5.998(1), b =18.669(4), c = 9.466(2) (A), ß = 1 0 0 .9 3 (3)0 ; 150(2) K: a = 5.971(1), b = 18.655(4), c = 9.3 8 3 (2) (Ä), ß = 1 0 1 .6 4 (1) 0 ; Z = 4. 
  Reference    Z. Naturforsch. 54b, 718 (1999); received March 1 1999 
  Published    1999 
  Keywords    Thermochromic Compounds, Copper, Chloride 
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 Identifier    ZNB-1999-54b-0718 
 Volume    54 
112Author    M. Fernanda, N. N. Carvalho3, ArmandoJ L Pombeiro3, Gabriele Wagner3, Bj0m Pedersenb, Rudolf HerrmannRequires cookie*
 Title    Cascade Reaction of Camphor-Derived Diynes with Transition Metal Compounds  
 Abstract    Platinum(II) catalyzes the isomerization o f camphor sulfonamide diynes in a cascade reaction involving annulation o f a five-membered ring to the camphor skeleton, ring-enlargement by C-C bond cleavage, reduction o f sulfur(VI) to sulfur(IV), and oxidation o f a hydroxy group to a ketone. The reactions o f the diynes with other transition metal compounds were also studied. Copper, gold and rhenium give final products similar to those obtained with simple Br0nsted acids or halogens, mainly by annulation o f a five-membered ring to the camphor moiety, accompanied by reduction o f a sulfonamide to a sulfinamide group, but lacking the ring-enlargement step. Palladium(II) occupies an intermediate position as both types o f products are obtained. The reaction mechanism and intermediates are discussed. 
  Reference    Z. Naturforsch. 54b, 725—733 (1999); received March 18 1999 
  Published    1999 
  Keywords    Camphor Diyne, Ring Enlargement, Transition Metals, Catalysis, Alkyne 
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 Identifier    ZNB-1999-54b-0725 
 Volume    54 
113Author    Winfried Hoffmüller, Kurt Polborn, Wolfgang BeckRequires cookie*
 Title    Ein tetraedrischer Zink-Komplex (L-terf-Leucin)2ZnCl2 mit Carboxylat-koordiniertem L-terf-Leucin in der Zwitterform Metal Complexes of Biologically Important Ligands, CXIX [1]. A Tetrahedral Zinc Complex (L-terf-Leucine)2ZnCl2 of Carboxylate Coordinated L-terr-Leucine in the Zwitterionic Form  
 Abstract    Zinc, L-terr-Leucine From an aqueous solution o f ZnCl2 and L-terMeucine the complex (L-r^rr-leucine)2ZnCl2 • 2 CH3OH with a distorted tetrahedral structure is formed in which, according to an X-ray structure analysis, the zwitterionic form o f the amino acid is coordinated through the carboxylate group. Metallkomplexe mit biologisch wichtigen Liganden, CXIX [1]. 
  Reference    Z. Naturforsch. 54b, 734—7 (1999); eingegangen am 1. April 1999 
  Published    1999 
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 Identifier    ZNB-1999-54b-0734 
 Volume    54 
114Author    Snte, PbteO. Bosholm, H. OppermannRequires cookie*
 Title    Untersuchungen zum chemischen Transport intermetallischer Phasen, I: GeTe, SnTe, PbTe Investigations on the Chemical Transport of Intermetallic Phases, I: GeTe  
 Abstract    GeTe, SnTe, and PbTe have been prepared by chemical transport reactions with iodine as transport agent in the temperature range between T2 (800 -700 °C) and T , (700 -500 °C). The effective transport equilibria were determineted. Total pressure measurements in the system Ge-Te-I give the coexistence equlibria for condensed phases, and also for the gasphase equilibra. GeTe4 exists only as a metastable phase at lower temperatures and decom poses near 260 °C in GeTe and Te. Thermodynamic calculations show satisfactory agreement between calculation and experi­ ment. 
  Reference    Z. Naturforsch. 54b, 737 (1999); eingegangen am 26. Februar 1999 
  Published    1999 
  Keywords    Chemical Transport Reactions, Total Pressure Measurement, Calculation o f CTR, Thermodynamic Data 
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 Identifier    ZNB-1999-54b-0737 
 Volume    54 
115Author    Joachim Pickardt, Pirka WischlinskiRequires cookie*
 Title    Kristallstruktur des "supramolekularen" Komplexes [K(Benzo-18-krone-6)][Zn(CN)3]*H20 mit einem polymeren kettenförmigen Tricyanozincat-Anion Crystal Structure of the "Supramolecular" Complex [K(benzo-18-crown-6)][Zn(CN)3] *H20 with a Polymeric Tricyano Zincate Anion with Chain Structure  
 Abstract    Crystals o f the com plex [K (benzo-18-crown-6][Zn(CN)3] H20 were obtained from a solution o f Z n(C N)2, KCN, and b en zo-18-crown-6 in water/methanol. The compound crystallizes in the triclinic space group PI (no. 2),: Z = 2, a = 818,6(5), b = 1236,7(8), c = 1359,6(6) pm, a = 67,02(4), ß = 87,38(4), 7 = 75,46(5). Each Zn atom is bonded to one bridging cyanide ion to give chains -Z n (C N)Z n -, and to two terminal CN groups. The N atom o f one o f the terminal CN groups interacts with a potassium ion o f the [K (benzo-18-crow n-6)]+ unit. The coordination spheres o f the K ions are completed by water molecules, which in turn form hydrogen bonds to N atoms o f terminal CN groups o f neighbouring chains, whereby puckered sheets are formed. 
  Reference    Z. Naturforsch. 54b, 747 (1999); eingegangen am 10. Februar 1999 
  Published    1999 
  Keywords    Zinc Cyanide C om plex, Crown Ether Complex, Crystal Structure 
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 Identifier    ZNB-1999-54b-0747 
 Volume    54 
116Author    Karin Brüning, Bettina Lühmann, Heinrich LangRequires cookie*
 Title    .2-Verzweigte Carbosiloxan-Dendrimere mit Hauptgruppenelement- und Übergangsmetall-modifizierten Oberflächen 1.2-Branched Carbosiloxane-Dendrimers with Main-Group Element and Transition-Metal Modified Surfaces  
 Abstract    The preparation o f the first and second generation carbosiloxane dendrimers Si[O C H ,-C h L C H ,S iM e(O C fL C = C H),]4 (3) and Si{O C H X H ,C H ,SiM e[O C H ,C FL C fL SiM e(O C F L -C = C H)2]2}4 (5) by the reaction o f Si(O C H ,C H ,C H ,SiM eC L)4 (1) or S i[O C H X H ,C H ,S iM e-(OCH2CH2CH2SiM eC l2)2]4 (4) with HOCH2C = C H (2) in the presence o f NEt3 is descri­ bed. Dendrimers 3 and 5 contain propargyloxy units as terminal groups, which can be trans­ ferred to Co2(C O)8 (6) to give the hexacarbonyldicobalt functionalized dendritic m olecu­ les S i{O C H ,C H X H ,S iM e [(/72-O C H ,C = C H)C o,(C O)6] , } 4 (7) and S i{ O O L O L C H ,S iM e -(OCH2CH2CH2S'iMe[(?72-OCH2C = C H)C o 2(CO)6]2)2} 4 (8). All compounds were characterized by elemental analyses, spectroscopic studies (IR, 'H-, 13C { 1H }-, -9S i{ 1H } N M R) as w ell as GPC investigations. 
  Reference    Z. Naturforsch. 54b, 751 (1999); eingegangen am 21. Januar 1999 
  Published    1999 
  Keywords    Carbosiloxane, Dendrimer, Propargyloxy Unit, Hexacarbonyldicobalt, Coordination Ability 
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 Identifier    ZNB-1999-54b-0751 
 Volume    54 
117Author    Christiane Leben, Martin JansenRequires cookie*
 Title    Darstellung und Kristallstruktur von Triammonium-trisulfimid (NH4)3(N S02)3 Preparation and Crystal Structure of Triammonium-trisulfimid (NH4)3(N S 0 2)3  
 Abstract    The preparation and crystal structure o f (N H 4N S 0 2)3 (a = 11.720(2), b = 6.156(6), c = 14.030(2) A ,ß = 96.69(8)°) is reported. The structure reveals a chair-conformation o f the anions, which are arranged to form a hexagonal rod stacking. Compared to cyclometatriphosphates the cations are coordinated differently due to the different basicities o f the bridging nitrogen and oxygen atoms, respectively. 
  Reference    Z. Naturforsch. 54b, 757 (1999); eingegangen am 24. Februar 1999 
  Published    1999 
  Keywords    Sulfimide, Ammonium, Preparation, Single-Crystal Structure Determination 
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 Identifier    ZNB-1999-54b-0757 
 Volume    54 
118Author    Tjark Siedentop, Ion Neda, Holger Thönnessen, PeterG. Jones, Reinhard SchmutzlerRequires cookie*
 Title    Synthese und Röntgenstrukturanalyse der ersten terf-Butylcalix[4]arensalze mit einem Phosphonium-Kation Synthesis and X-Ray Structure Analysis of the First rm-Butylcalix[4]arene Salts with a Phosphonium Cation  
 Abstract    terr-Butylcalix[4]arene A nions, rm -Butylcalix[4]arenes (Phosphorus-Substituted), Phospho­ nium Salts (Tetramethylguanidine-Substituted), X-Ray Data The reactions o f ter/-butylcalix[4]arene (1) and the phosphorus-substituted rm -butylcalix-[4]arene (2), respectively, with terf-butylbis[N-(N',N',N",N"-tetramethyl)guanidinyl]phosphine (3) led to the first calix[4]arene-anions with the protonated phosphonium cations 4 and 5. N o protonation o f the imino nitrogen atom was observed. In the case o f compound 4, a single­ crystal X-ray structure analysis has been conducted. In compound 5, phosphorus atoms in the oxidation states +III and +V are present in one molecule. 
  Reference    Z. Naturforsch. 54b, 761—7 (1999); eingegangen am 11. Februar 1999 
  Published    1999 
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 Identifier    ZNB-1999-54b-0761 
 Volume    54 
119Author    L. Homolya, S. Strueß, W. PreetzRequires cookie*
 Title    Kristallstrukturen und Normalkoordinatenanalyse von fraws-(w -Bu4N)2 [ReCl4IX], X = NCS, NCSe Crystal Structures and Normal Coordinate Analyses of trans-(n-Bu4 N)0 [ReCl4 IX], X = NCS, NCSe  
 Abstract    rra«s-Tetrachloromonoiodothiocyanato(N)-rhenate(IV), rrans-Tetrachloro-monoiodoselenocyanato(N)-rhenate(IV), Crystal Structure, Normal Coordinate Analysis The crystal structures o f rrafls-(n-Bu4N)2 [ReCl4I(NCS)] (triclinic, space group PI, a = 11.268(3), b = 11.696(2), c = 18.109(3) A , a = 98.68(2) ß = 106.40(2), 7 = 97.58(2)°, Z = 2)andrrans-(«-B u4N)2 [ReCl4 I(NCSe)] (orthorhombic, space group P 2)2 ,2,, a = 11.839(2), b = 12.2679(10), c = 31.136(5) A, Z = 4) have been determined by single crystal X-ray diffraction analysis. Based on the molecular parameters o f the X-ray determinations the low temperature (10 K) IR and Raman spectra o f the (n-Bu4N) salts have been assigned by normal coordinate analysis. The valence force constants are fd(R eN) = 1.69(N CS) and 1.65(N CSe) mdyn/A. 
  Reference    Z. Naturforsch. 54b, 767—771 (1999); eingegangen am 11. Februar 1999 
  Published    1999 
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 Identifier    ZNB-1999-54b-0767 
 Volume    54 
120Author    C. Drewes, W. PreetzRequires cookie*
 Title    Darstellung, n B-NMR-und Schwingungsspektren  
 Abstract    von c/s-Monoethyl-m0n0nitr0tetrahydr0-c/050-hexab0rat(2-) sowie Kristallstruktur von cM P h 4As)2[B6H4(C2H5)(N 0 2)] Synthesis, 11B NMR and Vibrational Spectra of ds-Monoethylmononitrotetrahydro-c/<m>-hexaborate(2 -) and Crystal Structure of c/5'-(Ph4 As)2 [B6 H4 (C2H5)(NO-,)] c/5-Monoethylmononitrotetrahydro-c/o5o-hexaborate(2 -), Crystal Structure, n B NMR Data, Vibrational Spectra By electrochemical oxidation of (n-Bu4N)[B6H5H^!'(C2Hs)] in the presence of nitrite ions and of the base DBU in dichloromethane solution c/\HB6H4(C2H5)(N02)]2_ is formed. X-ray diffraction analysis has been performed on a single crystal of c/s-(Ph4As)2[B6H4(C2H5)(N0 2)] (triclinic, space group PI; a = 10.673(4). b = 10.907(4), c = 21.237(4) A, a = 80.789(4), ß = 83.117(4), 7 = 66.548(2)°, Z = 2). The MB NMR spectrum is consistent with a disubstituted octahedral B6 cage with local Cs symmetry. The IR and Raman spectra exhibit characteristic CH3, CH2, N 02, BN, BH and B6 vibrations. 
  Reference    Z. Naturforsch. 54b, 772—776 (1999); eingegangen am 26. Februar 1999 
  Published    1999 
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 Identifier    ZNB-1999-54b-0772 
 Volume    54 
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