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1992[X]
1Author    K. Arin Ruhlandt-Senge, AlfredDirk Bacher, G. Ertraude Koellner, Birgit Siewert, Ulrich MüllerRequires cookie*
 Title    Tetraphenylphosphonium-nonachlorodivanadat(III), (PPh4)3[V2Cl9l * 7 CH2C12 Tetraphenylphosphonium Nonachlorodivanadate(III), (PPh4)3[V2Cl9] * 7 C H 2C12  
  Reference    Z. Naturforsch. 47b, 814—818 (1992); eingegangen am 14. O ktober 1991 
  Published    1992 
  Keywords    N onachlorodivanadate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0814.pdf 
 Identifier    ZNB-1992-47b-0814 
 Volume    47 
2Author    A. Dalbert Lossin, Gerd Meyer, R. Obert Fuchs, Joachim SträhleRequires cookie*
 Title    [Sm(CH3C 0 0 )3 (H 20)2] * CH 3COOH, ein Essigsäureaddukt des Samarium(III)-acetatdihydrates [Sm(CH3C0 0 )3(H 20 )2] * CH 3COOH, an Acetic Acid Adduct o f Sam arium (III) Acetate Dihydrate  
 Abstract    The crystal structure o f the acetic acid adduct o f the so far unknown samarium(III) acetate dihydrate was determined from single-crystal four-circle diffractometer data. It has the com ­ position [Sm (CH 3C 0 0)3 (H 20) 2] C H 3C 0 0 H containing {[Sm (CH3C 0 0)3 (H 20) 2]}2 dimers and crystallizes in the trigonal system, R 3, a = 2695.1(3), c = 1030.8(4) pm, Vm = 216.97(5) cm 3/m ol, R = 0.041, Rw = 0.030. 
  Reference    Z. Naturforsch. 47b, 179—182 (1992); eingegangen am 5. September 1991 
  Published    1992 
  Keywords    Samarium Acetate, Acetic Acid Adduct, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0179.pdf 
 Identifier    ZNB-1992-47b-0179 
 Volume    47 
3Author    Volker Müller, Gerlinde Frenzen, K. Urt Dehnicke, Dieter FenskeRequires cookie*
 Title    Synthese, FIR-Spektren und Kristallstrukturen der Pentaselenide K2Se5 und [Na(15-Krone-5)l2Se5 Syntheses, F IR Spectra, and Crystal Structures of the Pentaselenides K 2Se5 and [Na( 15-crown-5)]2Se5  
 Abstract    K2Se5 has been prepared by crystallization from a potassium polyselenide solution in D M F. In a similar way [Na(15-crown-5)]2Se5 can be prepared by crystallization from a sodium p oly­ selenide solution in D M F in the presence o f 15-crown-5. Both com pounds were characterized by FIR spectroscopy as well as by X-ray structure determinations. K2Se5: Space group P 2,2,2,, Z -4, 1659 observed independent reflections, R = 0.061. Lat­ tice dim ensions at -9 0 °C; a = 671.5(5), b = 694.9(5), c = 1776.4(9) pm. The com pound crys­ tallizes with the K2S5 type structure. [Na(15-crown-5)]2Se5: Space group P 1, Z = 2, 3026 observed indenpendent reflections, R = 0.140. Lattice dim ensions at -1 0 0 °C: a = 853.7(5), b = 1042.8(10), c = 2011.0(10) pm; a = 88.95(5)°, ß = 79.42(5)°, y = 66.15(5)°. The compound forms an ion triple, in which the sodium ions are coordinated by the five oxygen atoms o f the crown ether molecules as well as by the terminal selenium atom s o f the pentaselenide chain. The rather high R value is a result o f the disordered crown ether molecules. 
  Reference    Z. Naturforsch. 47b, 205 (1992); eingegangen am 23. August 1991 
  Published    1992 
  Keywords    Pentaselenides, Syntheses, FIR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0205.pdf 
 Identifier    ZNB-1992-47b-0205 
 Volume    47 
4Author    Stefan Vogler, K. Urt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur des Dichloroselenonitren-Komplexes (PPh4)2[WCl5(N SeC l2)| Synthesis and Crystal Structure of the Dichloro-selenonitrene Complex (PPh4)2[WCl5(NSeCl2)]  
 Abstract    The title com pound has been prepared by the reaction o f [WCl4(N SeCl)]2 with PPh4Cl in CH2C12 solution. It forms red crystals, which were characterized by an X-ray structure deter­ 
  Reference    Z. Naturforsch. 47b, 301 (1992); eingegangen am 27. September 1991 
  Published    1992 
  Keywords    Dichloro-selenonitren Complex o f Tungsten, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0301.pdf 
 Identifier    ZNB-1992-47b-0301 
 Volume    47 
5Author    Irina Sens, AlfredDirk Bacher, Ulrich MüllerRequires cookie*
 Title    Natrium-tetraethylammonium-tetrasulfid, N a+NEt4+S42 Synthese und Kristallstruktur Synthesis and Crystal Structure  
 Abstract    N aN E t4S4 was obtained from an equimolar solution of N a2S4 and N E t4Cl in ethanol. Its crystal structure was determined by X-ray diffraction with 4175 observed unique reflexions, R = 0.044. Crystal data: a = 713.4(4), b = 1744.5(9), c = 1204.0(5) pm, ß = 105.8(3)°, space group P 2 ,/«, Z = 4. In the structure, chains consisting of N a + and S42~ ions run in the a direc­ tion, every N a+ being coordinated by four terminal S atom s of S42~ ions (two terminal, one chelating). The chains are separated by the N E t4+ ions. 
  Reference    Z. Naturforsch. 47b, 819—822 (1992); eingegangen am 16. Januar 1992 
  Published    1992 
  Keywords    Sodium Tetraethylammonium Tetrasulfide, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0819.pdf 
 Identifier    ZNB-1992-47b-0819 
 Volume    47 
6Author    Henry StrasdeitRequires cookie*
 Title    Synthesis, Spectroscopic and X-Ray Structural Characterization of |Cd(linpen)l2+, a Model for M etal Complexes of the Chelating Polymer Polyethyleneimine (linpen = Linear Pentaethylenehexamine)  
 Abstract    The isolation of 3,6,9,12-tetraazatetradecane-l,14-diam ine (linear isomer o f pentaethylene­ hexamine, linpen) from a technical polyamine mixture is described. In methanol, linpen acts as a hexadentate ligand tow ards cadmium(II). The solid compounds [Cd(linpen)](BPh4)2 (1), [Cd(linpen)](BPh4)2-2D M SO (2) and [Cd(linpen)](BF4)2 (3) have been isolated and character­ ized by elemental analysis, spectroscopy and X-ray powder diffraction. The 113Cd N M R reso­ nance of 1 is at 351 ppm (0.30 M in DM SO -d6, standard: 0.10 M Cd(C104)2 in D 20). 2 and 3 have been structurally characterized by single-crystal X-ray diffraction. 2: C2/c; a = 19.337(1) A, b = 17.937(1)Ä, c = 18.584(1)Ä, ß = 1 1 1.54(1)°; Z = 4, R = 0.034, Rw = 0.033. 3: P2,/h; a = 8.607(1)Ä, b = 14.851(2)Ä, c = 15.703(2)Ä, ß = 91.21(2)°; Z = 4, R = 0.083, R" = 0.072. Both com pounds contain discrete [Cd(linpen)]2+ complexes. The hexamine wraps ar­ ound the metal ion in a helical manner. This results in a strong distortion of the coordination polyhedron. The mean C d -N bond lengths are 2.38Ä and 2.37Ä for 2 and 3, respectively. Models for M N 6 centers in metal-polyethyleneimine (PEI) complexes are derived from the structure of [Cd(linpen)]2+. F or example, loops at the M N 6 site in molecules of linear PEI are proposed. 
  Reference    Z. Naturforsch. 47b, 829—836 (1992); received December 12 1991 
  Published    1992 
  Keywords    Pentaethylenehexamine, Cadmium Complex, Synthesis, Crystal Structure, Polyethyleneimine 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0829.pdf 
 Identifier    ZNB-1992-47b-0829 
 Volume    47 
7Author    Alfred-Dirk Bacher, Ulrich MüllerRequires cookie*
 Title    Synthese und Kristallstruktur von INa(15-Krone-5)]2S6 Synthesis and Crystal Structure of [Na(15-crown-5)]2S6  
 Abstract    [Na(15-crown-5)]2S6 was obtained from N a 2S4 und 15-crown-5 in acetonitrile. Its crystal structure was determined by X-ray diffraction with 2968 observed reflexions, R = 0.119. Crys­ tal data: a = 861.4(9), 6 = 1006(1), c = 2097(1) pm, a = 89.7(1), ß = 100.20(8), y = 114.6(1)°, Z = 2, space group P 1. The chain-like S62-ion has transoid conform ations, each o f its terminal atom s is in contact with one N a + ion which in turn is coordinated with one crown ether m ole­ cule. 
  Reference    Z. Naturforsch. 47b, 1063—1066 (1992); eingegangen am 6. Februar 1992 
  Published    1992 
  Keywords    Sodium -Crown Hexasulfide, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-1063.pdf 
 Identifier    ZNB-1992-47b-1063 
 Volume    47 
8Author    Dieter Sellmann, W. Olfgang, Soglowek, M. Atthias, MollRequires cookie*
 Title    Übergangsmetallkomplexe mit Schwefelliganden, XCI+ Fen-Komplexe des fünfzähnigen Thioether-Thiolat-Aminliganden 'buN HS4'-H2: Synthese, Charakterisierung, Reaktivität und Stereochemie ('buNHS4'-H2 = 2 ,2 -Bis(2-mercapto-3,5-di-tertiärbutyl-phenylthio)diethylamin)  
 Abstract    Transition M etal Complexes with Sulfur Ligands, X C I+ Fe11 Complexes o f the Pentadentate Thioether-Thiolate-Amine Ligand 'buN HS4'-H 2: Synthesis, Characterization, Reactivity and Stereochemistry (,buN HS4'-H 2 = 2,2'-Bis(2-mercapto-3,5-di-tertiarybutyl-phenylthio)diethylamine) In search o f m odel com pounds for the active centers o f nitrogenases, [Fe(L)('buN HS4')] complexes o f the pentadentate thioether-thiolate-amine ligand 'buN HS4'2-('buN HS4'-H2 = 2,2'-bis(2-mercapto-3,5-di-tertiarybutyl-phenylthio)diethylamine) were obtained. A lkylation o f 'buS2'-H2 with (BrC2H4),N H yielded the new ligand 'buN HS4'-H2 as a mixture o f positional isomers. Isolation o f single isomers was achieved by reacting the mixture with FeCl2-4 H 20 and CO in order to give the corresponding [Fe(CO)] complexes which were se­ parated and hydrolyzed to yield the free ligands. R eaction o f 'buN HS4'-H2 with FeCl2 -4 H 20 led to the high-spin complex [Fe('buN HS4')] which is extremely air-sensitive in solution. It rapidly reacts with L = CO, NO, PM e3, and N 2H4, and is the m ost suitable starting material for syntheses o f [Fe(L)('buN HS4')l complexes which were characterized for L = CO, N O +, N O , PM e3 and N 2H4. All complexes are considerably better soluble in organic solvents than the corresponding parent compounds [Fe(L)('NHS4')], ('N hS4'-H 2 = 2,2'-bis(2-mercaptophenylthio)diethylamine), but have similar properties in most other respects. In the oxidation o f [F e(N 2H 4)('buN HS4')] at low temperatures, there is evidence for the form ation o f the diazene com plex [u-N 2H2{Fe('buN HS4')}2]. 
  Reference    Z. Naturforsch. 47b, 1105 (1992); eingegangen am 10. April 1992 
  Published    1992 
  Keywords    Iron Complexes, Thioether-Thiolate Ligand, Synthesis 
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 Identifier    ZNB-1992-47b-1105 
 Volume    47 
9Author    Rene Wollert, SigridW. Ocadlo, K. Urt Dehnicke, Helmut Goesmann, Dieter FenskeRequires cookie*
 Title    Die Kristallstrukturen von (PPh4)2 [TiCl3 (NSiMe3) ] 2 * CH3CN und (PPh4)2 [TiCl4(OSPCl2) ] 2 The Crystal Structures of (PPh4)2[TiCl3(NSiM e3)]2 -C H 3CN and (PPh4)2[TiCl4(OSPCl2)]2  
 Abstract    (PPh4)2[TiCl3(N SiM e3)]2 C H 3CN has been prepared from [TiCl^NSiM ej)]^ with PPh4Cl in acetonitrile solution as yellow crystals. The com pound crystallizes in the triclinic space group P 1 with one formula unit per unit cell, 3447 observed unique reflections, R = 0.053. Lattice dimensions at 200 K: a = 1030(1), b = 1253(1), c = 1374(1) pm, a = 77.46(8)°, ß = 73.93(8)°, y = 69.99(9)°. The structure consists o f PPh4+ ions and centrosymmetric dimeric anions [TiCl3(N SiM e3)]2~, in which pentacoordinate titanium atom s are associated via the nitrogen atoms o f the silylimido groups. (PPh4)2[TiCl4(OSPCl2)]2 has been prepared by the reaction o f PPh^fOSPClJ with titanium tetrachloride in C H 2C12 solution as orange crystals. (Space group P I , Z = 1, 3242 observed unique reflections, R = 0.033). Lattice dim ensions at 193 K: a = 1114.8(2), b = 1190.6(2), c = 1218.7(2) pm, a = 72.18(1)°, ß = 85.45(1)°, y = 69.19(1)°. The structure consists o f PPh4+ ions and centrosymmetric dimeric anions [TiCl4(O SPCl2)]^~, in which hexacoordinate titanium atom s are associated via two chlorine atoms. The OSPCl2_ group is coordinated via the oxygen atom. 
  Reference    Z. Naturforsch. 47b, 1386—1392 (1992); eingegangen am 9. März 1992 
  Published    1992 
  Keywords    Dimeric Titanium Complexes, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1992-47b-1386 
 Volume    47 
10Author    Wolfgang Tremel, Bernt Krebs, Klaus Greiwe, Wolfgang Simon, Hans-Oscar Stephan, Gerald HenkelRequires cookie*
 Title    [Mn(SPh)3Cl]2-, [Mn(SPh)3Br)2_, [Mn(SePh)4]2-, [Mn(TePh)4]2-, and ICo4(SPh)6Cl4l2-: New Mixed Halide/Thiolate and Chalcogenolate Complexes of Manganese and Cobalt  
 Abstract    The reactions of 1:1:1 m olar ratio mixtures of N aSPh/M nC l2/E t4NBr and N aSPh/CoCl2/ Et4NCl in methanol afford the com pounds [Et4N]4[Mn(SPh)3Br][Mn(SPh)3Cl] (1) and 
  Reference    Z. Naturforsch. 47b, 1580—1592 (1992); received February 7 1992 
  Published    1992 
  Keywords    Transition Metal Chalcogen Complexes, Synthesis, X-Ray Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-1580.pdf 
 Identifier    ZNB-1992-47b-1580 
 Volume    47 
11Author    Adalbert Lossin, Gerd MeyerRequires cookie*
 Title    Dimere und Ketten in Praseodym(III)acetat-sesquihydrat, Pr(CH3COO)3 * 1,5 H20 Dimers and Chains in Praseodymium(III)acetate-sesquihydrate, Pr(C H 3C OO)3-1.5 H20  
 Abstract    Pr(C H 3COO)3-1.5H-,0 crystallizes with the triclinic system. P i (no. 2), Z = 4, a = 844.2(4), b = 1009.8(5), c = 1340.1(7) pm, a = 87.10(5), ß = 76.25(6), y = 75.65(2)°, Vm = 161.9(1) cm3/ mol, R = 0.049, Rw = 0.035. The crystal structure contains centrosymmetric dimers {[Pr(CH3C 0 0) 4(H 20)]~}2 and one-dimensional chains i,[Pr(CH3C 0 0) 2(H 20)]+ along the [100] direction. Both units are built up by bridging acetate groups. The chains are linked by the dimers to layers parallel (101) sharing oxygen atoms. Crystal water molecules between these planes form hydrogen bonds to neighbouring layers. 
  Reference    Z. Naturforsch. 47b, 1602—1608 (1992); eingegangen am 14. April 1992 
  Published    1992 
  Keywords    Praseodymium Acetate, Sesquihydrate, Synthesis, Crystal Structure, Thermal Behaviour 
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 Identifier    ZNB-1992-47b-1602 
 Volume    47 
12Author    Alfred-Dirk Bacher, Ulrich Müller, K. Arin Ruhlandt-SengeRequires cookie*
 Title    Synthese und Kristallstruktur von [K(18-Krone-6)]2S6 * 2 CH3CN Synthesis and Crystal Structure of [K( 18-Crown-6)]2S6 * 2 C H 3CN  
 Abstract    [K(18-crown-6)]2S6-2 C H 3CN was obtained from K2S5 and 18-crown-6 in acetonitrile. The crystalline com pound easily loses the incorporated acetonitrile. Its crystal structure was deter­ 
  Reference    Z. Naturforsch. 47b, 1673—1676 (1992); eingegangen am 11. August 1992 
  Published    1992 
  Keywords    Potassium-Crown Hexasulfide, Synthesis, Crystal Structure 
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 Identifier    ZNB-1992-47b-1673 
 Volume    47 
13Author    Z. NaturforschRequires cookie*
 Title    Synthese und Kristallstrukturen von  
 Abstract    Tris(glykolato)molybdän(VI) und T ris(pinakolato)molvbdän(VI) Syntheses and C rystal Structures o f T ris(glycolato)m olybdenum (V I) and T ris(pinacolato)m olybdenum (V I) Silke B uth, Sigrid W ocadlo, B ernhard N eum üller, F ra n k W eller und K u rt Dehnicke* PPh4[M oN (O Ph)4] has been prepared by reaction o f PPh4[M oN C l4] with sodium phenolate, as an orange-red crystal powder. The reactions o f glycole and pinacole, respectively, with M oN (0-r-B u)3 and M oN C 13, the latter in the presence o f a base, lead to the /rä-chelate com ­ plexes M o(O C 2H40) 3 and M o(OC:M e40) 3, respectively. The complexes were characterized by 'H and l3C N M R spectroscopy, the chelate complexes in addition by X-ray structure analysis. [Mo(OC-,H40) 3]: Space group P 2,/c, Z = 4, 2177 observed unique reflections. R = 0.047. Lattice dim ensions at -4 0 °C: a = 1168.3(2), b = 716.0(1), c = 1206.1(2) pm, ß = 92.84(1)°. [M o(OC2Me40) 3] • 2 C H 2C12: Space group Pbcn, Z = 4, 1860 observed unique reflections, R = 0.049. Lattice dimensions at -8 0 °C: a = 1772.3(1), b = 1023.8(1), c = 1600.0(2) pm. Both complexes form monomeric molecules, in which the molybdenum atom s are surround­ ed in a distorted octahedral fashion by the six oxygen atom s o f the chelates. 
  Reference    Z. Naturforsch. 47b, 706 (1992); eingegangen am 24. Oktober 1991 
  Published    1992 
  Keywords    Chelate Complexes o f M olybdenum, Synthesis, N M R Spectra, Crystal Structure 
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 Identifier    ZNB-1992-47b-0706 
 Volume    47 
14Author    JörgN. Euhausen+, Karl-Ludwig Stork, ElisabethP. Otthoff, W. Olfgang, TremelRequires cookie*
 Title    Synthese und Struktur von Nb0 89Fe0 93Te2 und Ta0,77Fe0990Te2 Synthesis and Structure of N b0 89Fe093Te2 and Ta077Fe090Te2  
 Abstract    N b0g9Fe093Te2 and T a0 77Fe0 90Te2 were prepared by chemical transport reactions. The crys­ tal structures of both com pounds were determined using X-ray single crystal methods. The structures of the layer com pounds N b0g9Fe093Te2 (P mna, Z = 2, a = 7.951(1) Ä, b = 7.241(1) Ä, c = 6.233(1) Ä) and T a077Fe0 90Te2 (P mna, Z = 2, a = 7.890(2) Ä, b = 7.252(2) Ä, c = 6.192(1) Ä) are based on a hexagonal close packing of Te atoms. Approximately one-half of the octahedral holes in this packing are occupied by N b (Ta) atoms, about one-quarter of the tetrahedral holes are occupied by Fe atoms. The relationship to the NiAs structure type is discussed. 
  Reference    Z. Naturforsch. 47b, 1203—1212 (1992); eingegangen am 21. April 1992 
  Published    1992 
  Keywords    Synthesis, X-Ray, M etal-Rich Layer Compounds, Early Transition Metal Tellurides 
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 Identifier    ZNB-1992-47b-1203 
 Volume    47 
15Author    M. Artina Andratschke, Klaus-Jürgen Range, Heinz Haase, Ulrich KlementRequires cookie*
 Title    Die Kristallstruktur von a-K Z nP04 The Crystal Structure o f a  
  Reference    Z. Naturforsch. 47b, 1249—1254 (1992); eingegangen am 21. Februar 1992 
  Published    1992 
  Keywords    Potassium Zinc O rthophosphate, Low-Temperature M odification, Synthesis, Crystal Structure 
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 Identifier    ZNB-1992-47b-1249 
 Volume    47 
16Author    Harald Maelger, Falk Olbrich, Jürgen Kopf, Dirk Abein, Erwin WeissRequires cookie*
 Title    Synthese und Struktur der Basenaddukte von Kupfer(I)-Halogeniden mit Dimethylsulfid und Tetrahydrothiophen Synthesis and Crystal Structure of Lewis Base Adducts of Copper(I)-Halides with Dimethylsulfide and Tetrahydrothiophene  
 Abstract    Copper complexes o f the general formula [(CuX)a(L)J" with L = tetrahydrothiophene (THT) or dimethylsulfide (D M S) and X = Cl, Br or I are formed by direct reaction o f copper(I)halides with the corresponding ligands. All com pounds have been characterized by 
  Reference    Z. Naturforsch. 47b, 1276—1280 (1992); eingegangen am 20. Februar 1992 
  Published    1992 
  Keywords    X-Ray, Lewis Base Adducts, Copper(I)-Halides, Thioethers, Synthesis 
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 Identifier    ZNB-1992-47b-1276 
 Volume    47 
17Author    Peter Willershausen, Andrea Höfner, Jürgen Allwohn, M. Onika Pilz, W. Erner Massa, Armin BerndtRequires cookie*
 Title    Zum Einfluß von Substituenten auf o— ^--Wechselwirkung: Winkelverzerrungen in C-Borylmethylenboranen Effect of Substituents on <r-7r-Interaction: D istortion of Angles in C-Borylmethyleneboranes  
 Abstract    C -Borylmethyleneboranes with one or two O-Aryl substituents in the boryl group, 3 a and 4b, are obtained by cleavage o f B -C single bonds in the presence o f a B -C double bond. The duryl(methyl)borylmethyleneborane 7 is formed by thermal rearrangement o f the vinylborane 
  Reference    Z. Naturforsch. 47b, 983—9 (1992); eingegangen am 30. Oktober 1991/6. Februar 1992 
  Published    1992 
  Keywords    Synthesis, Crystal Structure, "B N M R Spectra, l3C N M R Spectra 
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 Identifier    ZNB-1992-47b-0983 
 Volume    47 
18Author    N. Orbert Auner, Erika Penzenstadler, Eberhardt HerdtweckRequires cookie*
 Title    Silaheterocyclen, XX Aminosubstituierte Vinylchlorsilane und Silaethene: Bausteine zur Synthese von l,3-Diaza-2-silacyclopentanen [1] Silaheterocycles, XX Am inosubstituted Vinylchlorosilanes and Silenes: Building Blocks for the Synthesis of l,3-Diaza-2-silacyclopentanes [1]  
 Abstract    The amino-substituted vinylchlorosilanes 4 -7 are synthesized from N ,N ,N '-trim ethyl-ethylenediamine (8 a) or tris(trimethylsilyl)ethylenediamine (8 b), LiBu" and organodichloro-vinylsilanes. 5 eliminates trimethylchlorosilane when distilled and yields 1,3-diaza-2-silacyclopentane 9, whereas the com pounds 6 and 7 show a great tendency to oligomerize. The reaction o f 4 with LiBu1 gives a neopentylsilene intermediate 10 a which can be trapped by isoprene or 1,3-butadiene yielding small amounts o f the Diels-Alder products 11 and 12, re­ spectively. The main reaction pathway for 10 a is rearrangement with migration o f a M e3Si-group from nitrogen to the silene's carbon atom and a new N —Si bond formation to give the diazasilacyclopentane 10 which has been characterized by X-ray diffraction analysis. This in­ tramolecular rearrangement appears to involve a pentacoordinated silene Si-atom. N o dimer-isation o f 10a to a disilacyclobutane is observed. The introduction o f a second Si-tris(tri-methylsilyl)ethylenediamine substituent at the SiC frame work does not result in silene stabili­ sation: there is no evidence for Si-hexacoordination in silene 15 nor in the [4+2] cyclo-addition product with isoprene (14). 
  Reference    Z. Naturforsch. 47b, 1377—1385 (1992); eingegangen am 6. Mai 1992 
  Published    1992 
  Keywords    Silaheterocycles, Synthesis, Form ation o f Silenes, Cycloaddition Reactions, Highly C oordinated Silicon 
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 Identifier    ZNB-1992-47b-1377 
 Volume    47 
19Author    N. Orbert Auner, Erika PenzenstadlerRequires cookie*
 Title    Silaheterocyclen, XVII Synthese und Cycloadditionsreaktionen neuartiger, aminocyclischer Silaethene [1] Silaheterocycles, XVII Synthesis and Cycloaddition Reactions of Novel Amino Cyclic Silenes [1]  
 Abstract    The silene 2 is formed by reacting 2-chloro-l,3-bis(trimethylsilyl)-2-vinyl-1,3-diaza-2-silacyclopentane (5) with LiBu' in «-pentane in the tem perature range from -1 0 to +10 °C. The reaction primarily leads to the corresponding a-lithio adduct 6 by addition of the Li-organyl to the vinyl group o f 5; subsequent 1,2-LiCl elimination yields 2 as an intermediate. 2 can be trapped by polar reagents M e3SiX (X = OMe, 0 S 0 2C F 3) as well as by organic dienes which add across the Si = C bond; in the absence of trapping agents, trisilacyclohexane 7 is isolated. The cycloaddition behaviour of 2 is best described by the two mesomeric formulae (a) and (ß), with competitive [4+2] and [2 + 2] addition routes: While with butadienes and norbor-na-2,5-diene the [2 + 2] products are formed mainly in a multiple step reaction via zwitterionic intermediates (1,4 dipoles), the ratio o f the [4+2]/[2 + 2] derivatives from 2 and cyclohexa-1,3-diene becomes nearly equivalent. 2 is thus quite com parable in its reactivity to dichloro-neopentylsilene, Cl2Si = C H C H 2Bu'. 
  Reference    Z. Naturforsch. 47b, 795—804 (1992); eingegangen am 25. November 1991 
  Published    1992 
  Keywords    Silaheterocycles, Synthesis, 1, 3-Bis(trimethylsilyl)-1, 3-diaza-2-silacyclopentane, F orm ation o f Silenes, Cycloaddition Reactions 
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 Identifier    ZNB-1992-47b-0795 
 Volume    47 
20Author    H. Hillebrecht, G. Thiele, P. Hollm, Ann, W. PreetzRequires cookie*
 Title    Darstellung, Charakterisierung und Normalkoordinatenanalyse von gemischtvalentem Dodekabromotriplatinat(IV,II,IV) [Pt3Br12]2~ und Kristallstruktur von (Ph3P =N =P P h3)2[Pt3Br12] * 2 CH2C12 Preparation, Characterization and Norm al Coordinate Analysis o f the Mixed Valence Dodecabrom otriplatinat(IV ,II,IV ) [Pt3Br12]2~ and Crystal Structure of (Ph3P = N = PPh3)2[Pt3Br 12] * 2 C H 2C12  
 Abstract    Heating a mixture (2:1) o f the tetrabutylammonium salts (TBA^JPtBrJ and (T B A)2[PtBr4] with trifluoroacetic acid leads to the mixed valence dodecabromotriplatinate(IV,II,IV) (T B A)2[Pt3Br12], The X-ray structure determination o f (Ph3P = N = PPh3)2[Pt3Br12] • 2C H 2C12 (triclinic, P 1, Z = 1) shows trinuclear groups with nearly D 2h symmetry for the anions, formed o f two PtBr6 octahedra and one planar PtBr4 group sharing edges. U sing the structural data a normal coordinate analysis based on a general valence force field for [Pt3Br12]2-has been per­ formed, which gives good agreement o f the calculated frequencies with the bands observed in the IR and Raman spectra. 
  Reference    Z. Naturforsch. 47b, 1099—1104 (1992); eingegangen am 10. Februar 1992 
  Published    1992 
  Keywords    Dodecabrom otriplatinate(IV, II, IV), M ixed-Valence C om pound, Synthesis, Crystal Structure, Raman Spectra 
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 Identifier    ZNB-1992-47b-1099 
 Volume    47