| 3 | Author
| Johannes Rott, Ernst Guggolz, Albert Rettenmeier, ManfredL. Ziegler | Requires cookie* | | Title
| Darstellung und Charakterisierung von Spezies der Zusammensetzung ?? Synthesis, Structure, Mono-and Binuclear Chromium Complexes  | | | Abstract
| 5 -C5H5Cr(NO)2SR (R = C6H5, C6F5, uC4H9) und [r? 5 -C5H5CrNO]2(ER)2 (E = O, S, Se, Te, R = Alkyl, Aryl); Röntgenstrukturanalysen von [^ 5 -C5H5(NO)Cr(/*-SeC6H5)2Cr(NO)-J7 5 -C5H5] und [^ 5 -C5H5(NO)Cr(iM-Se-n-C4H9)(Jw-OH)Cr(NO)-?? 5 -C5H5] Synthesis and Characterization of Species of Composition ?? 5 -C5H5Cr(NO)2SR (R = C6H5, C6F5, *-C4H9) and [r?5-C5H5CrNO]2(ER)2 (E = 0, S, Se, Te, R = alkyl, aryl); X-ray Structure Analysis of [r?5.C5H5(NO)CrCa-SeC6H5)2Cr(NO)-^.C5H5] and [^-C5H5(NO)Cr(ia-Se-n-C4H9)(ia-OH)Cr(NO)-^.C5H5] The title compounds have been synthesized and characterized by elemental analysis, IR and *H NMR methods and mass spectra. The crystal and molecular structures of the binuclear complexes [^-CsHsfNOJCr^-SeCeHsteCrfNOHS-CgHs] and [/?5-C5H5(NO)Cr(^-Se-n-C4H9)(/u-OH)Cr(NO)-?? 5 -C5H5] have been determined by X-ray structure analysis. The latter is shown to have a four-membered ring consisting of two chromium atoms, one selenium, and one oxygen atom. | | |
Reference
| (Z. Naturforsch. 37b, 13—23 [1982]; eingegangen am 27. August 1981) | | |
Published
| 1982 | | |
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| default:Reihe_B/37/ZNB-1982-37b-0013.pdf | | | Identifier
| ZNB-1982-37b-0013 | | | Volume
| 37 | |
4 | Author
| Thomas Bünger, Udo Engelhardt | Requires cookie* | | Title
| N-Methylsubstituierte Hydrazinderivate der Phosphorsäure aus Phenoxy-phosphoryl-dichlorid und aus Phenoxy-thiophosphoryl-dichlorid N-Methyl Substituted Hydrazine Derivatives of Phosphoric Acid from Phenoxy-phosphoryl-dichloride and from Phenoxy-thiophosphoryl-dichloride  | | | Abstract
| C6H50P(X)C12 (X = O, S) reacts with 1,2-dimethylhydrazine, 1,1-dimethylhydrazine or methylhydrazine, resp., to give the new dihydrazido derivatives la, 2a, 2b, or 3a and 3a-l, resp. Their X H NMR and 31 P NMR data are given. Einführung | | |
Reference
| (Z. Naturforsch. 37b, 24—28 [1982]; eingegangen am 19. August 1981) | | |
Published
| 1982 | | |
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| default:Reihe_B/37/ZNB-1982-37b-0024.pdf | | | Identifier
| ZNB-1982-37b-0024 | | | Volume
| 37 | |
5 | Author
| Heinrich Nöth, Robert Rurländer, Peter Wolfgardt | Requires cookie* | | Title
| 27 AI NMR Spectroscopy  | | | Abstract
| 27 AI NMR Spectra, Aluminium Compounds 27 AI NMR studies of AICI3 solutions in diethyl ether reveal the presence of AICI4 at high concentrations. This ion can also be recognized besides AICI3 • OR2 at low temperature in düute solutions, while at 25 °C a single signal is observed, which represents the average of all species in solution. More extensive dissociation of AICI3 results in tetrahydrofuran. The main species in equilibrium with one another are A1C13-2THF, AlClJ and AlCl2(THF)£. Nearly quantitative dissociation to yield AICI4 and [AlClLs] 2+ occurs in dilute solutions of AICI3 in monoglyme (L reprents one oxygen donor atom); at higher concentration an adduct AlCVL with Al in a tetrahedral environment is also present. This trend towards extensive dissociation is also observed in the solutions of AICI3 in diglyme and triglyme. Relative peak areas are in agreement with the formation of a 1:1 electrolyte [AlCl2L4] + AlCl4 in diglyme, whereas additional dissociation into [A1C1L5] 2+ and A1C1J occurs in triglyme. | | |
Reference
| (Z. Naturforsch. 37b, 29—37 [1982]; received July 22 1981) | | |
Published
| 1982 | | |
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| default:Reihe_B/37/ZNB-1982-37b-0029.pdf | | | Identifier
| ZNB-1982-37b-0029 | | | Volume
| 37 | |
7 | Author
| Carl Habben, Walter Maringgele, Anton Meiler | Requires cookie* | | Title
| Reactions of Multiple Bond Systems with the l,2,4-Trithia-3.5-diborolane Ring  | | |
Reference
| (Z. Naturforsch. 37b, 43—53 [1982]; eingegangen am 9. Juli 1981) | | |
Published
| 1982 | | |
Keywords
| J 4 -1, 3, 2-Dithiaborolenes, A 2 < 5 -1, 4-Thiaboracyclohexadienes, 2-Methyl-4-trimethylsilyl-l, 3, 2-dithiaborolane, NMR Spectra | | |
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| default:Reihe_B/37/ZNB-1982-37b-0043.pdf | | | Identifier
| ZNB-1982-37b-0043 | | | Volume
| 37 | |
8 | Author
| H. Holler, W. Kurtz, D. Babel, Sonderforschungsbereich, (. Kristallstruktur, Chemische Bindung, W. Knop | Requires cookie* | | Title
| Die Kristall-und magnetische Struktur von BaCrF5 Crystal and Magnetic Structure of BaCrF5  | | | Abstract
| A single crystal X-ray structure analysis of orthorhombic BaCrFs (a — 1393.8(1), b = 571,1(1), c = 494,7(1) pm), which crystallizes in the structure type of BaGaF5, space group P2i2i2i, yielded Cr-F distances in the range of 187.3 to 194.9 pm, average 190.2 pm. Using powder neutron diffraction data taken at 2.2 K a G-type antiferromagnetic structure with spin alignment along the c direction of the lattice was worked out. Single crystal susceptibility data were consistent with this model and in addition showed a small net moment, probably due to spin canting, to be present below the Neel temperature of TN = 3.4 K. The orientation of this moment along the b axis is in accordance with the space group symmetry as well, chemical and magnetic cell being the same. From powder susceptibility data an exchange energy of —3.74 K (g = 2.02) was obtained by fitting Fisher's model. The low bridging angle of Cr-F-Cr = 137.4° within the eis corner-sharing chain of octahedra is made responsible for the weak antiferromagnetism in BaCrFs, which is compared to that of other chromium(III) fluorides. | | |
Reference
| (Z. Naturforsch. 37b, 54—60 [1982]; eingegangen am 21. August 1981) | | |
Published
| 1982 | | |
Keywords
| Pentafluorochromate(HI), Crystal Structure, Magnetic Structure, Magnetic Susceptibility | | |
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| default:Reihe_B/37/ZNB-1982-37b-0054.pdf | | | Identifier
| ZNB-1982-37b-0054 | | | Volume
| 37 | |
9 | Author
| Hartmut Maisch | Requires cookie* | | Title
| Die Stabilisierung von P(NH2)Hal2 (Hai = Cl, Br, I) und P(NHMe)2G als Komplexliganden  | | | Abstract
| The Stabilisation of P(NH2)Hal2 (Hal = Cl, Br, I) and P(NHMe)2Cl as Complex Ligands The phosphanes P(NH2)Hal2 and P(NHMe)2Cl are stabilised as ligands in (CO)5MoP(NH2)Hal2 [Hai = Cl (2), Br (3), I (4)] and (CO)5MoP(NHMe)2Cl (10) by reactions of (CO)5MoP(NH2)3 (1) with HHal or of (CO)5MoP(NHMe)3 (8) with HCl, respectively. 4 decomposes at room temperature and reacts with i-BuNH2 to give, (CO)5MOP(NH-<-BU)2NH2 (6). 1 and HI form (CO)5MoPI3. 3 can also be prepared from 2 with HBr, 4 from 2 and 3 with HBr and HI, respectively. The reactions of 2-4 with NR3 produce polymers, whereas the reaction of 3 with pyridine leads to (COjsMoNCsHs. The mixtures (CO)5MoP(NHMe)Br2/(CO)5MoPBr3 and (CO)5MoP(NH-t-Pr)2Cl/ (CO)5MoP(NH-i-Pr)Cl2 are isolated from reactions of 8 with HBr and of 9 with HI, and 9 reacts with HBr to give (CO)sMoPBr3. (CO)sMoP(NHMe)I2 is formed in small amounts by the reaction of 8 with HI, the main product is an insoluble solid, which is probably the impure intermediate [(CO)5MoP(NHMe)(NH2Me)2] 2 +2I-. Reaction of 10 with NEt3 leads to the formation of the dinuclear complex 12 in which the new diazadiphosphetidine [MeNHP-NMe]2 functions as a bridging ligand between two (CO)sMo units. | | |
Reference
| (Z. Naturforsch. 37b, 61—67 [1982]; eingegangen am 1. Oktober 1981) | | |
Published
| 1982 | | |
Keywords
| Ligand Reactions, Hydrogen Halides, Phosphanes | | |
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| default:Reihe_B/37/ZNB-1982-37b-0061.pdf | | | Identifier
| ZNB-1982-37b-0061 | | | Volume
| 37 | |
10 | Author
| Lothar Weber, Dietmar Wewers | Requires cookie* | | Title
| ÜbergangsmetaU-Schwefelylid-Komplexe, XII [1] ?7 5 -Thiacyclohexadienyl-l-oxid als Ligand in neutralen Halogenomolybdän-und Halogenowolframkomplexen Transition Metal Sulfur Ylide Complexes, XII [1] ?y 5 -Thiacyclohexadienyl-l-oxide as a Ligand in Neutral Halide Complexes of Molybdenum and Tungsten  | | | Abstract
| The organometallic anion in tetraethylammonium-tricarbonyl(3,5-diphenylthiacyclo-hexadienyl-1-oxide)molybdate and its tungsten analogue can be halogenated by treatment with iodine, C5H5N • Br2, and I,I-dichloroiodobenzene to yield neutral [7?5.C5H3(C6H5)2SO]M(CO)3X complexes (M = Mo, W; X = Cl, Br, I). Weitere neutrale Komplexe des r/ 5 -Thiacyclohexa-dienyl-l-oxid-Liganden sollten durch Halogenie-rungsreaktionen an 2, 3 und 4 zugänglich sein. Die Ligandenstärke des Heterocyclus sowie die Nucleo-philie von 2, 3 und 4 werden verglichen mit bekann-ten ?7 5 -Liganden wie (T^-CSHS)-und deren Tri-carbonylmetallat-Ionen [(jf-C5H5)M(CO)3]-(M = Cr, Mo, W). Präparative Ergebnisse Die Iodierung von 3 und 4 in Form ihrer Tetra-ethylammoniumsalze gelingt in CH2C12-Lösung durch Umsetzung mit äquivalenten Mengen Iod bei 0 °C (Gl. (2)). Der Verlauf der Reaktion ist IR-spektroskopisch im v(CO)-Bereich leicht zu ver-folgen. Ähnliches gilt für die Bromierung. Jedoch wird hier die Verwendung des bequem ab wägbaren festen Pyridin-Bromaddukts CsHsN-B^ der des freien Halogens vorgezogen (Gl. (3)). Bei der Um-setzung von äquivalenten Mengen an I.I-Dichlor-iodbenzol und 3 bzw. 4 in CH2CI2 werden die entsprechenden Chlorokomplexe erhalten (Gl. (4)). Die Halogenierung des Chromderivates 2 gelang unter analogen Bedingungen nicht. Die so erhaltenen Produkte sind die ersten neutra-len Molybdän-und Wolframkomplexe, die den rf>-Thiacyclohexadienyl-l-oxid-Liganden tragen. Sie stellen ockergelbe bis orangegelbe diamagnetische Feststoffe dar, die kurzzeitig unzersetzt an der Luft gehandhabt werden können. Sie lösen sich gut in CH2CI2 und CHCI3, weniger gut in Aceton, THF, Toluol und Ether und sind in gesättigten Kohlen-wasserstoffen unlöslich. Die Lösungen erleiden bei | | |
Reference
| (Z. Naturforsch. 37b, 68—72 [1982]; eingegangen am 10. September 1981) | | |
Published
| 1982 | | |
Keywords
| 3, 5-Diphenylcyclohexadienyl-l-oxide, Halogenation, Molybdenum and Tungsten Complexes | | |
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| default:Reihe_B/37/ZNB-1982-37b-0068.pdf | | | Identifier
| ZNB-1982-37b-0068 | | | Volume
| 37 | |
11 | Author
| Jochen Eilermann, Martin Lietz | Requires cookie* | | Title
| Chemie polyfunktioneller Liganden, 67 [1]  | | | Abstract
| Die Darstellung von l.l.l-Tris(dichlorarsinomethyl)ethan, Ethan-l.l.l-tris(methylarsonsäure), 1.1.1-Tris (arsinomethyl)ethan und einem neuen Organocyclotriarsan Chemistry of Polyfunctional Ligands, 67 [1] The Preparation of l.l.l-Tris(dichloroarsinomethyl)ethane, Ethane-l.l.l-tris(methylarsonic acid), l.l.l-Tris(arsinomethyl)ethane and of a New Organocyclotriarsane l,l,l-Tris(dichlorarsinomethyl)ethane, CH3C(CH2AsCl2)3 (5) can be obtained in the reaction of CH3C(CH2AsNC6H4CH3)3 (4) with gaseous HCl. The heteroadamantane CH3C(CH2AsO)3 (6) reacts with AsCl3 or PC13 yielding also 5. CH3C(CH2AsO)3, CH3C(CH2AsS)3 and CH3C(CH2AsI 2)3 are oxidized with H202 to give CH3C[CH2As(0)(0H)2]3 (7) and CH3C[CH2As(0)(0H)2]3 • H20 (7 a). CH3C(CH2AsI2)3 and C(CH2AsI2)4 can be reduced with LiAlH4 to give CH3C(CH2AsH2)3 (9) and C(CH2AsH2)4 (12). Oxidation of 9 and 12 leads to the cyclotriarsane compounds CH3C(CH2As)3 (10) and H2AsCH2C(CH2As)3 (13). | | |
Reference
| (Z. Naturforsch. 37b, 73—80 [1982]; eingegangen am 29. Juni/21. September 1981) | | |
Published
| 1982 | | |
Keywords
| Arsenic Compounds, Organocyclotriarsane, Vibrational Spectra, *H NMR Spectra, Mass Spectra | | |
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| default:Reihe_B/37/ZNB-1982-37b-0073.pdf | | | Identifier
| ZNB-1982-37b-0073 | | | Volume
| 37 | |
12 | Author
| V. Zürn, W. Schwarz, W. Rozdzinski, A. Schmidt | Requires cookie* | | Title
| Di-and Trimeric Dimethylaminoisocyanate. Structures and Spectra  | | | Abstract
| N-Heterocyclic Compounds N,N-Dimethyl-N',N'-bis(trimethylsilyl)hydrazine reacts with fluorophosgene to yield 5,5-dimethyl-3-dimethylamino-2,4-dioxo-5-azonia-imidazolidide (1). With phosgene, l-methyl-2-chloroformyl-4-dimethylamino-l,2,4-triazolidine-3,5-dione (5) can be prepared. The thermal decomposition of N,N-dimethyl-N'-carbomethoxi-N'-trimethylsüyl-hydra-zine gives l,3,5-tris(dimethylamino)-l,3,5-hexahydrotriazine-2,4,6-trione (2) and 1,2-dimethyl-4-dimethylamino-l,2,4-triazolidine-3,5-dione (3). 2 can also be prepared by thermal decomposition of N.N-dimethyl-N'-carbomethoxi-N'-fluoroformylhydrazine (4). The crystal and molecular structures of 1 and 2 were determined by X-ray analysis. The iH NMR and vibrational data of 1-5 were communicated. The mass spectra of 1-3 were measured and discussed. | | |
Reference
| (Z. Naturforsch. 37b, 81—90 [1982]; eingegangen am 24. Juli 1981) | | |
Published
| 1982 | | |
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| default:Reihe_B/37/ZNB-1982-37b-0081.pdf | | | Identifier
| ZNB-1982-37b-0081 | | | Volume
| 37 | |
13 | Author
| Gerd Becker, Michael Rößler | Requires cookie* | | Title
| Trimethylsilylverbindungen der Vb  | | | Abstract
| Elemente, HI [1] Tris(trimethylsilyl)-und Tris(trimethylstannyl)bismutan sowie Tetrakis(trimethylsilyl)dibismutan Trimethylsilyl Derivatives of Vb-Elements, III [1] Tris(trimethylsilyl)-and Tris(trimethylstannyl)bismuthine as well as Tetrakis(trimethylsilyl)dibismuthine Tris (trimethylsilyl) bismuthine, Tris(trimethylstanny 1)bismuthine, Lithium Bis(trimethylsilyl)bismuthide * 2 THF, Tetrakis(trimethylsilyl)dibismuthine Chlorotrimethylsilane and sodium/potassium bismuthide, easily prepared from finely powdered bismuth and sodium potassium alloy in 1,2-dimethoxyethane (DME), react to give tris(trimethylsilyl)bismuthine (1) in 48% yield. When compound 1 is treated with chlorotrimethylstannane all trimethylsilyl substituents are successively replaced by stannyl groups, and tris(trimethylstannyl)bismuthine (4) is obtained. As in analogous reactions of other tris(trimethylsilyl) derivatives of Vb-elements with methyl lithium in diethylether/tetrahydrofuran (THF), one trimethylsilyl group of tris (trimethylsilyl)-bismuthine (1) can also be removed, and lithium bis(trimethylsilyl)bismuthide • 2 THF (5) is formed. With 1,2-dibromoethane bismuthide 6 reacts with metal halogen exchange to give green lustrous needles of tetrakis(trimethylsilyl)dibismuthine (6). In contrast to other dibismuthines described in the literature, this compound is thermally rather stable and can be isolated in preparative amounts. Similar to several distibines a colour change from green to red, resp. orange-red occurs on melting or dissolving dibismuthine 6 in organic solvents. | | |
Reference
| (Z. Naturforsch. 37b, 91—96 [1982]; eingegangen am 7. August 1981) | | |
Published
| 1982 | | |
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| default:Reihe_B/37/ZNB-1982-37b-0091.pdf | | | Identifier
| ZNB-1982-37b-0091 | | | Volume
| 37 | |
14 | Author
| Elli Theodoridou, Pantelis Karabinas, Dimitrios Jannakoudakis | Requires cookie* | | Title
| Elektrochemisches Verhalten der Nitrophenole und ihrer Reduktionsprodukte an Graphitelektroden, II Mechanismus und Kinetik Electrochemical Behavior of the Nitrophenols and their Reduction Products at Graphite Electrodes, II Mechanism and Kinetic  | | | Abstract
| The mechanism of the electrochemical reactions of l-nitro-2-naphthol, o-nitrophenol and p-nitrophenol at carbon fibre electrodes is investigated in aqueous solutions with pH= 1-10. The above nitrophenols are reduced to the corresponding amines, which are reoxidized to quinone imines. As the quinone imines are partially hydrolysed to quinones, the kinetic of this hydrolysis reaction is also examined. In the case of l-nitro-2-naphthol the hydrolysis rate constant of 1,2-naphthoquinone imine is estimated as a function of pH by cyclic voltammetry. | | |
Reference
| (Z. Naturforsch. 37b, 97—101 [1982]; eingegangen am 14. September 1981) | | |
Published
| 1982 | | |
Keywords
| Cyclic Voltammetry, Graphite Electrodes, o-Nitrophenol, 1, 2-Naphthoquinoneimine | | |
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| default:Reihe_B/37/ZNB-1982-37b-0097.pdf | | | Identifier
| ZNB-1982-37b-0097 | | | Volume
| 37 | |
16 | Author
| Erich Ziegler, OttoS. Wolfbeis, Iris Trummer, Frau Prof, Dr, MagHelga Et, Wittmann | Requires cookie* | | Title
| Eine Methode zur C-Methylierung cyclischer /3-Dicarbonyl-Verbindungen A Method for the C-Methylation of Cychc /9-Dicarbonyl Compounds  | | | Abstract
| Cyclic /5-dicarbonyl compounds (1, 4, 7, 10) were reacted with either aniline or urea in the presence of trimethoxymethane to give the enamines 2, 5, 8 and 11, resp. The latter were reduced with hydrogen over palladium-charcoal or with the dimethylamine-boron-hydride complex to give the C-methylated /3-dicarbonyl compounds 3, 6, 9 and 12, resp. in moderatly to good overall yields. | | |
Reference
| (Z. Naturforsch. 37b, 105—107 [1982]; eingegangen am 20. Juli 1981) | | |
Published
| 1982 | | |
Keywords
| Enamine Reduction, Catalytic Hydrogenation, Boron Hydride Reduction, C-Methylation | | |
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| default:Reihe_B/37/ZNB-1982-37b-0105.pdf | | | Identifier
| ZNB-1982-37b-0105 | | | Volume
| 37 | |
|