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1987 (274)
21Author    Carlos AguileraRequires cookie*
 Title    Frozen Cholesteric Phase of a /J-Estradiol Derivative  
 Abstract    A new /3-estradiol derivative was synthesized. The compound shows LC behaviour (cholesteric phase between 119 and 151 °C). On cooling the LC state, the liquid crystalline structure is preserved. The mesophase persists at room temperature. To our knowledge, such a thermotropic behaviour has only been observed in the case of polymeric liquid crys-tals. 
  Reference    (Z. Naturforsch. 42b, 113—114 [1987]; received July 14 1986) 
  Published    1987 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0113_n.pdf 
 Identifier    ZNB-1987-42b-0113_n 
 Volume    42 
22Author    Gernot Heckmann, Ekkehard Fluck, Peter KuhmRequires cookie*
 Title    A [l,3,4]Thiazaphospholidine, Preparation and NMR Data  
 Abstract    Preparation and properties of a [l,3,4]thiaza-phospholidine are described. The 31 P. 13 C and 'H NMR spectra in double and triple resonance mode are recorded and discussed in detail. 
  Reference    (Z. Naturforsch. 42b, 115—117 [1987]; eingegangen am 29. August 1986) 
  Published    1987 
  Keywords    [l, 3, 4]Thiazaphospholidine, NMR Spectra, Triple Resonance 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0115_n.pdf 
 Identifier    ZNB-1987-42b-0115_n 
 Volume    42 
23Author    Max Herberhold, Karlheinz GuldnerRequires cookie*
 Title    Cyclische Organylarsino-Schwefeldiimide Cyclic Organylarsino Sulfur Diimides  
 Abstract    The reactions of the bifunctional bis(chloro-arsino) compounds MeCH[As(Bu')Cl] 2 and RCH[AsC1 2 ] 2 (R = H, Me) with the salt K 2 SN 2 lead to rings and cages containing arsino-substituted sul-fur diimide units. 
  Reference    (Z. Naturforsch. 42b, 118—120 [1987]; eingegangen am 18. September 1986) 
  Published    1987 
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 Identifier    ZNB-1987-42b-0118_n 
 Volume    42 
24Author    Fritz Preuss, Harald NoichlRequires cookie*
 Title    Oxo-und Thiovanadium(V)-Thiolate Oxo and Thiovanadium(V) Thiolates  
 Abstract    Thiolato Oxovanadium(V), Thiolato Thiovanadium(V), Preparation, 5I V NMR Spectra Syntheses of oxovanadium(V) thiolates such as 0 = V(SR) 3 (R = 'C 4 H g , SiPh 3) and 0=V(0'C 4 H 9)"(S'C 4 H 9) 3 _" (n — 1, 2) are described. The thiovanadium(V) compounds S=V(0'C 4 H 9) 3 , S = V(S'C 4 H 9)(0'C 4 H 9) 2 and S=V(SSiPh 3) 3 have been prepared by various 
  Reference    (Z. Naturforsch. 42b, 121—129 [1987]; eingegangen am 26. August 1986) 
  Published    1987 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0121.pdf 
 Identifier    ZNB-1987-42b-0121 
 Volume    42 
25Author    KurtO. KleppRequires cookie*
 Title    Darstellung und Kristallstruktur von NaCu 3 Te 2 Preparation and Crystal Structure of NaCu 3 Te 2  
 Abstract    The title compound was prepared by reacting a corresponding mixture of Na 2 Te 2 , copper and tellurium at 700 °C. NaCu 3 Te 2 forms crystals of metallic lustre which are rapidly decomposed in humid atmosphere. It crystallizes with a rhombohedral structure, space group R3m, with a — 4.276(3) Ä, c = 23.78(1) Ä. Z = 3. The crystal structure was determined from diffractometer data and refined to a conventional R of 0.050 for 135 independent reflections. The atomic arrangement of NaCu 3 Te 2 is based on a c.c.p. array of tellurium atoms with stacking sequence c 6 . Na and Cu occupy alternatingly the interstitial layers. Na is in an octahedral coordi-nation (d Na _ Te : 3.22 A), the Cu atoms occupy the tetrahedral and the octahedral voids. They are, however, shifted from the centers of these sites, resulting in an 1 + 3 coordination (d Cu _ Te : 2.70 Ä) for Cu on the tetrahedral. and an essentially trigonal coordination (d Cu Xe : 2.575 A) for Cu on the octahedral sites. NaCu 3 Te 2 shows no closer structural relationships to the other alkali-copper-chalcogenides known so far. However, its crystal structure may be interpreted as an ordered defect derivative structure of the CaCu 4 P 2 -type [1]. 
  Reference    (Z. Naturforsch. 42b, 130—134 [1987]; eingegangen am 11. April 1986) 
  Published    1987 
  Keywords    Ternary Chalcogenides, Sodium Copper Telluride, Crystal Structure, Preparation 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0130.pdf 
 Identifier    ZNB-1987-42b-0130 
 Volume    42 
26Author    Dieter Kissel, Rudolf HoppeRequires cookie*
 Title    Zur Kenntnis von KCrF 4 [1], [2] On KCrF 4 [1], [2]  
 Abstract    KCrF 4 has been prepared as yellowish-green single crystals (by heating of KF, CuF 2 , CrF 3 ; Au-tube, 750 °C, 60 d). It crystallizes in the orthorhombic crystal system (Pnma) with: a = 1573.2, b = 743.2, c = 1833.1 pm, Z = 24. The structure shows [Cr 3 F 9 F 6/2 ] 3 ~-columns along [010], The Madelung Part of Lattice Energie, MAPLE, is calculated and discussed, along with Effec-tive Coordination Numbers, ECoN (via Mean Fictive Ionic Radii, MEFIR). The structure is described using SCHLEGEL-diagrams. 
  Reference    Z. Naturforsch. 42b, 135—141 (1987); eingegangen am 12. September 1986 
  Published    1987 
  Keywords    Preparation, Crystal Structure, MAPLE, SCHLEGEL-Diagrams 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0135.pdf 
 Identifier    ZNB-1987-42b-0135 
 Volume    42 
27Author    Hubert Schmidbaur, Jan Ebenhöch, Gerhard MüllerRequires cookie*
 Title    Synthese, Eigenschaften und Struktur einiger Silyl-Ethene Synthesis, Properties, and Structure of Some Silyl-Ethenes  
 Abstract    Silyl-ethene, Silyl-ethine, Alkenyl-silane, Alkinyl-silane rnms-l,2-Dichloro-l,2-bis(trichlorosilyl)ethene (1) was prepared from Cl 3 CSiCl 3 and copper powder, and its structure determined by single crystal X-ray diffraction (monoclinic, space group P2,/n, a = 7.297(1), b = 10.964(1), c = 7.988(1) k, ß = 108.06(1)°; R = 0.037, R w = 0.066). Cl 3 SiC=CSiCl 3 , 2, forms a cobalt cage cluster on reaction with Co 2 (CO) 8 formulated as (CO) 6 Co 2 C 2 (SiCl 3) 2 . Hydrosilylation with HSiCl 3 gives tris(trichlorosilyl)ethene. -Bis(trimethyl-silyl)ethine adds HSiCl 3 to form l-trichlorosilyl-l,2-bis(trimethylsilyl)ethene, which can be con-verted into the hydride with /-BU 2 A1H. All compounds are model systems for CVD production of amorphous silicon a-Si:C. 
  Reference    Z. Naturforsch. 42b, 142—146 (1987); eingegangen am 26. Juni 1986 
  Published    1987 
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 Identifier    ZNB-1987-42b-0142 
 Volume    42 
28Author    H. Schmidbaur, W. Bublak, B. Huber, G. MüllerRequires cookie*
 Title    Cyclophan-Metall-Komplexe: Synthese und Kristallstruktur von ([2](l,4)NaphthaIino[2]paracyclophan)gallium(I)-tetrabromogallat(III) Cyclophane Metal Complexes: Synthesis and Crystal Structure of ([2]( 1,4)Naphthalino[2]paracyclophane)gallium(I) Tetrabromogallate(III)  
 Abstract    (Arene)gallium(I) Complex, Crystal Structure, Naphthalinocyclophane Complex The title complex has been prepared from Ga[GaBr 4 ] and [2](l,4)naphthalino[2]para-cyclophane in toluene as a solvent, and the crystal structure of this adduct determined by single crystal X-ray diffraction. The structure is composed of dimeric units Ga 2 [GaBr 4 ] 2 , which are crosslinked into sheets through Ga(I)-arene coordination. Both the benzene ring and the substi-tuted ring of the naphthalene system are ^-bonded from the outer side of the cyclophane cage, each to an univalent metal. The benzene and the naphthalene form an interplane angle of 49.3°. The distance to the benzene ring (2.67 Ä) is much shorter than the distance to the naphthalene (2.85 Ä), suggesting a stronger complexation with the unperturbed ;r-system of the former. [2.2](l,4)Naphthalinophane forms no adduct with Ga[GaBr 4 ], and with [2](l,5)naph-thalino[2]paracyclophane secondary reactions are observed. 
  Reference    Z. Naturforsch. 42b, 147—150 (1987); eingegangen am 17. November 1986 
  Published    1987 
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 Identifier    ZNB-1987-42b-0147 
 Volume    42 
29Author    Roland Zagler, Brigitte Eisenmann, Herbert SchäferRequires cookie*
 Title    Tritelluride mit komplexierten Kationen: Darstellung und Kristallstruktur von [Ba(en) 3 ]Te 3 und [Ba(en) 4;5 ]Te 3 Tritellurides of Complex Cations: Synthesis and Crystal Structure of [Ba(en) 3 ]Te 3 and [Ba(en) 4 5 ]Te 3  
 Abstract    The two title compounds have been prepared by reaction of appropriate mixtures of the elements in ethylenediamine. The structures have been determined on the basis of single crystal data. [Ba(en) 3 ]Te 3 crystallizes in the monoclinic system, space group P2 (/c with a = 918.0(4), b — 1203.7(6), c = 1639.9(6) pm, ß = 93.4(1)°. In the structure there are bent tritelluride anions Te 3 2 ~ (bond lengths 273.9—278.5 pm, bond angle 105.7°). The Ba 2+ cations are six coordinate by the bidentate ligand ethylenediamine. [Ba(en) 4 5 ]Te 3 crystallizes in the monoclinic system, space group Cc with a = 1752.8(6), b = 938.9(4), c = 3041.7(8) pm, ß = 91.3(1)°. In this structure the bond lengths in the Te 3 2 ~ anions are shorter (272.1—273.1 pm, bond angles 110.9—112.2°). The cations are coordinated by four bidentate ligands, and are connected into pairs by a further ethylenediamine molecule. The resulting dinuclear [Ba(en) 4 ]en[Ba(en) 4 ] 4+ units have the Ba 2+ cations in CN 9. 
  Reference    Z. Naturforsch. 42b, 151—156 (1987); eingegangen am 7. 0ktober/20. November 1986 
  Published    1987 
  Keywords    Tellurides, Polyanions, Crystal Structure 
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 Identifier    ZNB-1987-42b-0151 
 Volume    42 
30Author    F. Seel, J. SchuhRequires cookie*
 Title    Über die Umsetzung von Kupfersulfat mit Carbonsäuren und Carbonsäurederivaten in wäßrigen Lösungen unter hydrothermalen Bedingungen The Reaction of Copper Sulfate with Carboxylic Acids and their Derivatives in Aqueous Solutions under Hydrothermal Conditions  
 Abstract    Under hydrothermal conditions aqueous solutions of copper(II) sulfate (1) are reduced by means of saturated fatty acids with hydrogen at the a-atom to yield crystalline copper. In all cases carbon dioxide is liberated and lower fatty acids and ketones can be identified as reaction prod-ucts. a-Hydroxy and a-aminocarboxylic acids proved to be very effective reducing agents towards 1. The yield of copper varied from 2 to 2.5 mol Cu per 1 mol of amino acid. The reaction of 1 is suppressed by sulfuric acid. The presence of hydrochlorid acid or chlorides leads to the precipita-tion of copper(I) chloride. The mechanisms of the decomposition of the various types of carboxy-lic acids is discussed. It was also possible to precipitate metallic copper by means of various proteins. 
  Reference    Z. Naturforsch. 42b, 157—162 (1987); eingegangen am 19. September 1986 
  Published    1987 
  Keywords    Copper, Copper(II) Sulfate, Carboxylic Acids, Hydrothermal Reactions 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0157.pdf 
 Identifier    ZNB-1987-42b-0157 
 Volume    42 
31Author    Ralf Steudel, Detlef Jensen, Bettina PlinkeRequires cookie*
 Title    Low Temperature Raman Spectra of Dichlorosulfane (SC1 2 ), Tetrachlorosulfurane (SC1 4 ), Dichlorodisulfane (S 2 C1 2 ) and Dichlorodiselane (Se 2 Cl 2 ) [1]  
 Abstract    The Raman spectrum of commercial "sulfur dichloride" shows strong lines due to SC1 2 and S 2 C1 2 and weak Cl 2 lines at 25 °C, but strong SC1 2 and SC1 4 signals at —100 °C (the latter are superimposed on the S 2 C1 2 lines). Thus, the intense Raman effect of SC1 4 can be used to detect small amounts of chlorine in SC1 2 . Mixtures of SC1 2 and Cl 2 (1:15) yield the Raman spectrum of SC1 4 at —140 °C, while at 25 °C not trace of this compound can be detected. The spectra of SC1 4 and a-SeCl 4 are quite different, indicating different molecular and/or crystal structures, although EC1 3 + ions (E — S, Se) are present in both cases. While Se 2 Cl 2 dimerizes reversibly below —50 °C, S 2 C1 2 neither dimerizes nor isomerizes on cooling. The S 2 C1 2 dimer is characterized by a Raman line at 215 cm" 1 the intensity of which was used to calculate an enthalpy of dimerization as of -17 kJ/mol. 
  Reference    Z. Naturforsch. 42b, 163—168 (1987); received September 22 1986 
  Published    1987 
  Keywords    Raman Spectra, Sulfur Chlorides, Selenium Chlorides 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0163.pdf 
 Identifier    ZNB-1987-42b-0163 
 Volume    42 
32Author    Winfried Hinrichs, Peer Berges, Günter KlarRequires cookie*
 Title    Selbststapelnde Systeme, IV [1] 2,3,7,8-Tetramethoxythianthreniumsalze Selfstacking Systems, Part IV [1] 2.3.7.8-Tetramethoxythianthrenium Salts  
 Abstract    2.3.7.8-Tetramethoxythianthrenium Ion, Formation of Dimers and Stacks By addition of solutions of nitrosyl hexachloroantimonate(V) in acetonitrile or of diiodine in /7-hexane to a solution of 2.3.7.8-tetramethoxythianthrene ("Vn 2 S 2 ", 1) in toluene the oxidation products [Vn 2 S 2 ][SbCl 6 ] • CH 3 CN (2) and [Vn 2 S 2 ]I 3 (3), resp., are formed. Crystal structure deter-minations show both compounds to contain the [Vn 2 S 2 ] + ion. In contrast to the folded parent compound Vn 2 S 2 its monocation [Vn 2 S 2 ] T is planar, the short CS and CO distances (172—173 pm and 134—135 pm resp.) indicate an extended mesomeric system. Both compounds crystallize with segregated stacks of cations and anions. In 2 the coplanarly and equidistantly stacked [Vn 2 S 2 ] + ions have an A,B-sequence (distance between the planes of the ions 353 pm, intermolecular S---S distance 366 pm). In 3 the [Vn 2 S 2 ] + ions form dimers by SS contacts (S---S distance 316 pm); these dimers are arranged in a stair-like manner (distances between atoms of adjacent dimers 350-380 pm). The conductivities of 2 and 3 are 9.4 • 10" 9 and 5.3 • 10" 6 Sem" 1 , resp. 
  Reference    Z. Naturforsch. 42b, 169—176 (1987); eingegangen am 2. September 1986 
  Published    1987 
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 Identifier    ZNB-1987-42b-0169 
 Volume    42 
33Author    Sibbele Hietkamp, Thomas Lebbe, GerdU. Spiegel, Othmar StelzerRequires cookie*
 Title    Oligophosphaalkane, XVII [1] Funktionalisierte Tri-, Tetra-und Pentaphosphaalkane mit der Donorsequenz P-C-C-P und P-C-C-C-P Oligophosphaalkanes, XVII [1] Functionalized Tri-, Tetra-and Pentaphosphaalkanes with the Donor Sequence P-C-C-P and P-C-C-C-P  
 Abstract    Starting with the secondary phosphanes R 2 PH (R = Me, Ph, /Pr) and the vinyl-or allylmethyl-phosphinic acid isopropylesters, the triphosphaalkanes R 2 P-[CH 2 ] 3 —PMe —[CH 2 ] 2 —PMeH con-taining one terminal PH-group have been synthesized in a multiple step synthesis. The tertiary-secondary phosphanes R 2 P—[CH 2 ] 3 —PMeH obtained as intermediates may be used for the syn-theses of hybrid donor systems PPN. The P—C-skeletons of the tetra-and pentadentate oligophos-phaalkanes have been built up by a free radical initiated addition of the vinyl or allyl compounds CH,=CH-P(NEt,) 2 or CH 2 =CH-CH,-P(0)(0/Pr)Me to disecondary or disecondary-tertiary phosphanes, HMeP-[CH 2 ]"-PMeH {n = 2, 3) or HMeP-[CH 2 ] 3 -PPh-[CH 2 ] 3 -PMeH, respec-tively. Methanolysis of the tetra-and pentaphosphaalkanes with terminal P—NEt 2 functional groups affords the methoxy derivatives in almost quantitative yield. While the terminal P(NEt 2) 2 groups in the oligophosphaalkanes cannot be reduced by LiAlH 4 , the corresponding methoxy derivatives react immediately to give the primary-tertiary phosphanes. 
  Reference    Z. Naturforsch. 42b, 177—185 (1987); eingegangen am 4. August 1986 
  Published    1987 
  Keywords    Tertiary-Secondary Phosphanes, Triphosphaalkanes, Tetra-and Pentaphosphaalkanes, 31 P{'H} NMR Spectra, 13 C{'H} NMR Spectra 
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 Identifier    ZNB-1987-42b-0177 
 Volume    42 
34Author    Klaus Stumpf, Walter Siebert, Roland Köster, Günter SeidelRequires cookie*
 Title    Reaktionen von 2,3-Dihydro-l,3-diborolen mit Kalium und Iodmethan. Charakterisierung der Produkte als (C 5 H 5 )Co-Komplexe [1]  
 Abstract    The reactions between 2,3-dihydro-l,3-diborole derivatives 1 and potassium in tetrahydrofuran yield dark brown solutions. Without elimination of hydrogen, 1.4 to 1.8 moles of potassium are consumed by one mole of 1. Reduced 1 and iodomethane react to give methylated products, identified by GC/MS studies. Complexation with (C 5 H 5)Co(C 2 H 4) 2 leads to the cyclopentadienyl-cobalt complexes 2, iso-2, 3, and 4, of which iso-2 is a new cobalt-hydride sandwich. Methylation reactions of the cobalt sandwich anions (2-H)~ are reported. 
  Reference    Z. Naturforsch. 42b, 186—190 (1987); eingegangen am 4. Juli 1986 
  Published    1987 
  Keywords    2, 3-Dihydro-l, 3-diboroles, Cobalt Sandwich Complexes, Cobalt-Hydride Complexes 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0186.pdf 
 Identifier    ZNB-1987-42b-0186 
 Volume    42 
35Author    Roland Köster, Günther Seidel, Susanna Kerschl, Bernd WrackmeyerRequires cookie*
 Title    Atropisomerism in Boron-Nitrogen Heterocycles  
 Abstract    Atropisomerism owing to hindered rotation about the N-aryl bond is observed in 4,5-diethyl-2,2,3-trimethyl-l-(o-trifluormethyl)phenyl-2,5-dihydro-lH-l,2,5-azasila-(2) and -azastanna-boroles (5). The compounds 2 and 5 are characterized by elemental analysis, mass spectra and 'H, "B, 13 C, 29 Si and U9 Sn NMR. The orr/zo-trifluoromethyl group serves as an additional NMR spectroscopic probe because of "through space" W F-'H and 19 F-L, C spin spin coupling. Compound 5 is the first derivative of a 2,5-dihydro-lH-l,2,5-azastannaborol. 
  Reference    Z. Naturforsch. 42b, 191—194 (1987); eingegangen am 23. Oktober 1986 
  Published    1987 
  Keywords    Atropisomerism, Boron-Nitrogen Heterocycles, Multinuclear NMR 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0191.pdf 
 Identifier    ZNB-1987-42b-0191 
 Volume    42 
36Author    W. S. Sheldrick, P. BellRequires cookie*
 Title    Interaction of Metal Ions with 7-Deaza-8-aza-and 8-Aza-purines Preparation and X-Ray Structural Analysis of Copper(II) Complexes  
 Abstract    The reaction of 8-aza-and 7-deaza-8-aza-purines with Cu :+ cations in acid solution has been studied. At a pH value of 2, the 8-azaadenine complex [Cu(H 2 0) 4 (AAdH) 2 ](N0 3) 2 (1), which displays Cu-N9 coordination, may be isolated from solution. The reaction of CuCl 2 with 8-aza-hypoxanthine in concentrated HCl solution leads to ring opening at C 2 of the azapurine with subsequent formation of dichlorobis[(5-amino-4-carboxamide)[l — 3]triazole] copper(II) dihydrate 2, in which the triazole ligands display a chelating function, coordinating the metal via N7 and 06. The results for 1 and 2 suggest that copper coordination of the azapurine base is not a prerequisite for opening of the pyrimidine ring. Respectively N9-and N8-coordinated complexes [CUC13(A11H3)]" 3 and [CuCl 2 (H 2 0)(MAllH)] n (4) of allopurinol (A11H 2) and 9-methylallopurinol (MA11H) may be prepared by the reaction of CuCl 2 with the respective bases in HCl solution. In contrast, with the analogous l-methyl-4-aminopyrazolo[3,4-d]pyrimidine MAPP, only the salt (MAPPH)4(CU2C18) (5) could be isolated under similar conditions, indicating that N8 is less attractive as a binding site in this 7-deaza-8-azaadenine derivative. The structures of 1—5 have been established by X-ray structural analysis. A distorted octahedral [4+2]geometry is found for the copper atoms in 1 and 2. Chlorine bridged polymeric chain structures are adopted by the complexes 3 and 4. An intermediate coordination geometry between trigonal bipyramidal and square-pyrami-dal is observed for the metal atoms in 3, a distorted square-pyramidal geometry in 4. 
  Reference    Z. Naturforsch. 42b, 195—202 (1987); received August 18/October 17 1986 
  Published    1987 
  Keywords    8-Azapurines, Allopurinol, Copper(II) Complexes, X-Ray 
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 Identifier    ZNB-1987-42b-0195 
 Volume    42 
37Author    Gertrud Weiler, Gottfried Huttner, Laszlo Zsolnai, Heinz BerkeRequires cookie*
 Title    Phosphordonor-substituierte Formylmangan-Komplexe Phosphorous Donor Substituted Formyl Manganese Complexes  
 Abstract    Phosphonomanganese complexes (CH 3 0) 2 (0)PMn(C0)3[P(0CH 3)3] 2 (lb), (CH 3 0) 2 (0)PMn(C0) 2 [P(0CH 3) 3 ] 3 (lc) are obtained via demethylation of the corresponding cationic substituted carbonylmanganese compounds with KHB(secBu) 3 . The reaction of NaBH 4 in methanol with cationic phosphorus donor substituted carbonyl manganese compounds leads to formyl complexes (OC) 3 L 2 MnCHO (L = P(OCH 3) 3 (3a), L = P(OEt) 3 (3c), L -P(0*Pr) 3 (3d), L = PPh 3 (3e)) and (OC) 2 [P(OCH 3) 3 ] 3 MnCHO (3b). 3d decomposes thermally to give an (OC) 3 [P(OzPr) 3 ] 2 MnH and an (0C) 2 [P(0/Pr) 3 ] 3 MnH complex. The latter has been characterized by an X-ray structure determination. 
  Reference    Z. Naturforsch. 42b, 203—209 (1987); eingegangen am 22. August 1986 
  Published    1987 
  Keywords    Formyl, Hydride Complexes, X-Ray 
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 Identifier    ZNB-1987-42b-0203 
 Volume    42 
38Author    Diazo, Heinrich Heydt, Hans-Werner Breiner, Volker Hell, Manfred RegitzRequires cookie*
 Title    Diazoverbindungen, 65 [1] Isomerisierungen im System 4-Diazo-l-buten/2.3-Diazabicyclo[3.1.0]hex-2-en/1.4-Dihydropyridazin  
 Abstract    Compounds, 65 [1] Isomerization Reactions in the System 4-Diazo-l-butene/2.3-Diazabicyclo[3.1.0]hex-2-ene/1.4-Dihydropyridazine [3+2]-Cycloaddition and Reversion, Allyl-diazo Compounds, 2.3-Diazabicyclo[3.1.0]hexenes, 1.4-Dihydropyridazines (Diazomethyl)diphenylphosphine oxide (2a) adds onto the 1-cyclopropene phosphonates la and c under formation of the 2.3-diazabicyclo[3.1.0]hex-2-enes 3a and c. 3a is easily converted into the 1.4-dihydropyridazine 5a. On the other hand the reaction of lb with 2a directly affords the 1.4-dihydropyridazine 5b. The 2.3-diazabicyclo[3.1.0]hex-2-enes 3a and c isomerize to the allyl diazomethanes 4a and c on heating in benzene. In the case of the reactions 2b+lb as well as 6+1 a the direct formation of allyl diazo compounds (4d and 8a respectively) is observed. In a novel reaction 9-diazofluorene (6) yields the 1.3-butadiene 9 when reacted with the cyclo-propene lb. 
  Reference    Z. Naturforsch. 42b, 210—216 (1987); eingegangen am 28. August 1986 
  Published    1987 
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 Identifier    ZNB-1987-42b-0210 
 Volume    42 
39Author    Requires cookie*
 Title    Heterocyclische Siebenring-Verbindungen, XXX [1] Synthese und Eigenschaften von 4-Methoxy-l,5-benzothiazepin, einem einfachen Vertreter des 1,4-Thiazepin-Ringsystems  
  Reference    Z. Naturforsch. 42b, 217 (1987) 
  Published    1987 
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 Identifier    ZNB-1987-42b-0217 
 Volume    42 
40Author    Horst Küppers, Karl-F Hesse, Ulrike Ashauer-Holzgrabe, Rolf Haller, Roland BoeseRequires cookie*
 Title    Stereochemistry of Substituted Isomeric 3-Oxa-7-aza-bicyclo[3.3.1]nonan-9-ones  
 Abstract    3-Oxa-7-aza-bicyclo[3.3. l]nonan-9-ones, Boat-Chair and Chair-Chair Conformation, Configuration of Ring Substituents Two isomers of 7-methyl-9-oxo-2,4-diphenyl-3-oxa-7-aza-bicyclo[3.3.1]nonan-l,5-ethyl dicarb-oxylate (la and lb) were obtained by condensation of 2,6-diphenyl-l-oxa-4-oxo-cyclohexan-3,5-ethyl dicarboxylate with methylamine and formaldehyde. Their crystal structures were deter-mined by X-ray diffraction. They crystallize in the triclinic space group PI with (for la) a = 12.907(5), b = 11.223(4), c = 8.993(4) Ä, a = 105.82(4), ß = 100.14(5), y = 97.35(4)°, and (for lb) a = 16.400(7), b = 13.062(4), c = 11.336(2) A, a = 94.19(3), ß = 94.74(3), y = 102.56(4)°. This investigation has shown that isomer la has the boat-chair conformation, and isomer lb has the chair-chair conformation. The formation of la causes a configurational change of the phenyl substituents. The two species are characterized by NMR spectroscopy. — Another comparable bicyclononanone with a bulky substituent at the nitrogen atom has been synthesized and was investigated spectroscopically. This compound should have chair-boat conformation (with the boat conformation in the N-heterocyclic ring) whereas la has the boat conformation in the O-heterocyclic ring. 
  Reference    Z. Naturforsch. 42b, 221—228 (1987); received July 14 1986 
  Published    1987 
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 Identifier    ZNB-1987-42b-0221 
 Volume    42 
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