| 1 | Author
| M. Veith | Requires cookie* | | Title
| Cyclische Diazastannylene, II 1 Intermolekulare Lewis-Säure-Base-Addukte bei 1.3.2.4A 2 -Diazasilastannetidinen Cyclic Diazastannylenes, II 1 Intermolecular Lewis-Acid-Base Adducts of 1, 3,2,4A 2 -Diazasilastannetidines  | | | Abstract
| -diazasilastannetidines can be prepared as mono-mers (organyl = <erf-butyl) or dimers (organyl = isopropyl) in nonpolar solvents, depending on the organic nitrogen substituent. The formation of the dimer, which is due to an intermolecular Lewis-acid-base interaction of Sn(II) with nitrogen, can be initiated by solidification. When the tertf-butyl compound is cooled below 0 °C two crystalline modi-fications are found: a monoclinic phase (C 2/c; a= 10.655(5); b = 24.75(1); c = 17.334(9) Ä; ß = 106.9(1)°) and a triclinic phase (P I; a = 10.68(1); b = 13.51(1); c = 12.36(1) A; a = 96.2(1); ß = 102.6(1); y = 118.4(1)°). The crystal structures turn out to be built of dimeric and monomeric units in the first case and presumably only dimeric species in the second case. The isopropyl derivative crystallizes in the space group P 2i/b (a = 10.77(1); b= 12.14(2); c = 11.15(2) A; ß = 120.2(2)°) with only dimeric units being present, as in the liquid. Interrelationships between the three structures are discussed. | | |
Reference
| (Z. Naturforsch. 33b, 1—6 [1978]; eingegangen am 5. September/6. Oktober 1977) | | |
Published
| 1978 | | |
Keywords
| Diazastannylenes, Solid State, X-ray, Crystal Structure, NMR l, 3-Diorganyl-2, 2-dimethyl-I, 3, 2, 4A 2 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0001.pdf | | | Identifier
| ZNB-1978-33b-0001 | | | Volume
| 33 | |
2 | Author
| Cyclic Diazastannylenes, Iii, M. Veith | Requires cookie* | | Title
| Cyclische Diazastannylene, DI 1 Die Kristall-und Molekülstruktur der monoklinen Phase von 1.3-Di-feri-butyl-2.2-dimethyl-1.3.2.4A 2 -diazasilastannetidin The Crystal and Molecular Structure of the Monoclinic Phase of l,3-Di-feri-butyl-2,2-dimethyl-l,3,2,4A 2 -diazasilastannetidine  | | | Abstract
| The crystal and molecular structure of the monoclinic phase of l,3-di-£eri-butyl-2,2-dimethyl-l,3,2,4A 2 -diazasilastannetidine has been determined from three-dimensional X-ray data collected on a two-circle diffractometer at —120 °C (MoKa radiation, 2623 re-flexions, R — 0,050). The crystals are monoclinic, space group C 2/c, with cell dimensions a = 10.655(5), b = 25.75(1), c = 17.33(1) A, ß = 106.8(1)° and Z = 12. Four monomeric (crystal site symmetry 2 (C2)) and four dimeric units (crystal site symmetry I (Cj)) are present in the structure interacting over tin-tin (3.68 A). Remarkable are the very short Sn-N bond (2.09 A) in the monomer and the donation bond Sn-N (2.39 Ä) in the dimer. The coordination of the tin atoms in the different units is discussed in detail. | | |
Reference
| (Z. Naturforsch. 33b, 7—13 [1978]; eingegangen am 5. September/6. Oktober 1977) | | |
Published
| 1978 | | |
Keywords
| Diazastannylenes, X-ray, Molecular Structure, Crystal Structure | | |
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| default:Reihe_B/33/ZNB-1978-33b-0007.pdf | | | Identifier
| ZNB-1978-33b-0007 | | | Volume
| 33 | |
3 | Author
| Cyclic Diazastannylenes, Iv, M. Veith, 0. Reckten, Wald, E. Humpfer | Requires cookie* | | Title
| Cyclische Diazastannylene, IV 1 Zur Oxidation von 1.3-Di-ferf-butyl-2.2-dimethyl-1.3.2.4A 2 -diazasilastannetidin Oxidation of l,3-Di-£erJ-butyl-2,2-dimethyl-1,3,2,4A 2 -diazasilastannetidine  | | | Abstract
| The reactions of l,3-di-<er^-butyl-2,2-dimethyl-l,3,2,4A 2 -diazasilastannetidine (1) with O2 and Sß or SnCU proceed in two steps: In a first redoxtype reaction an intermediate containing tetravalent tin is formed. Some of these intermediates are unstable with respect to the starting material stannylene 1 and undergo a substitution reaction to yield a spiro-tetraazastannane. Under appropriate conditions the intermediate from the sulfur-and SnCLi-reaction can be isolated and turns out to be either dispiro[3,3,3]distanna-disulfa-disila-tetrazane or a diaza-dichlorostannane respectively. Crystal and kinetic data of some products/reactions are reported. | | |
Reference
| (Z. Naturforsch. 33b, 14—19 [1978]; eingegangen am 14. September 1977) | | |
Published
| 1978 | | |
Keywords
| Diazastannylenes, Unsymmetrically Substituted Stannanes, Kinetic Data, NMR, Crystal Data | | |
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| default:Reihe_B/33/ZNB-1978-33b-0014.pdf | | | Identifier
| ZNB-1978-33b-0014 | | | Volume
| 33 | |
4 | Author
| Gert Heller, Bernd Bichowski | Requires cookie* | | Title
| Darstellung von Polyboraten mit sperrigen tertiären Aminen und quaternären Ammoniumbasen in organischen Lösungsmitteln Preparation of Polyborates with Hindered Tertiary Amines and Quaternary Ammonium Bases in Organic Solvents  | | | Abstract
| Polyborates, Ammonium Borates, Isopolyanions, Tris(methoxy)borane, Hydrolysis The preparation of polyborates with bulky cations in organic solvents by the method of "ester hydrolysis" as well as by the method of evaporation of solutions of the base and boric acid reactands under reduced pressure with the very strong bases benzyltrimethyl-ammonium hydroxide and benzyltriethylammonium hydroxide leads to [C6H5CH2N(CH3)3][B506(0H)4] and [C6H5CH2N(C2H5)3][B506(0H)4]. The more bulky, but less basic tri-n-butylamine yields a heptaborate, presumably [(C4H9)3NH][B706(OH)XO]. The less bulky, but more basic triethylamine or tri-n-propylamine yield [(C2H5)3NH][B506(0H)4] or [(C3H7)3NH][B506(0H)4]. The most bulky, but less basic benzylamine or tri-n-octylamine are not capable to function as cations in polyborates. | | |
Reference
| (Z. Naturforsch. 33b, 20—23 [1978]; eingegangen am 3. Oktober 1977) | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0020.pdf | | | Identifier
| ZNB-1978-33b-0020 | | | Volume
| 33 | |
5 | Author
| Franz Gerstner, Johann Weidlein | Requires cookie* | | Title
| N.N' -Dimethylacetamidinderivate des Aluminiums, Galliums und Indiums N,N'-Dimethylacetamidin Derivatives of Aluminium, Gallium and Indium  | | | Abstract
| The interaction of N,N'-dimethylacetamidine with trialkyl derivatives of alumin-ium, gallium and indium yields dialkylmetal compounds of the structural formula R2M(N2Me2CMe) (M = Al, Ga and In). According to the vibrational data the M2N4C2 skeletons of these dimeric products form a centrosymmetric puckered eight-membered ring, probably with C2h symmetry. The IR-and Raman spectra of the amidine HN(Me)C(= NMe)Me are discussed. | | |
Reference
| (Z. Naturforsch. 33b, 24—29 [1978]; eingegangen am 3. Oktober 1977) | | |
Published
| 1978 | | |
Keywords
| Dialkylmetal Acetamidin Derivatives, Preparation, Vibrational Spectra | | |
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| default:Reihe_B/33/ZNB-1978-33b-0024.pdf | | | Identifier
| ZNB-1978-33b-0024 | | | Volume
| 33 | |
6 | Author
| I. M. Issa, E. M. Diefallah, M. R. Mahmoud, A. M. El-, Nady Chem | Requires cookie* | | Title
| Kinetics of the Alkaline Solvolysis of Trichloroacetate Ion in Water-Ethanol Solutions  | | | Abstract
| Alkaline Solvolysis, Trichloroacetate Ion The alkaline solvolysis of trichloroacetic acid in water-ethanol mixtures have been studied in the presence of 0.40-0.80 M sodium hydroxide within the temperature range 35-70 °C. The rate constant increased with progressive addition of the organic solvent. The dielectric constant effect on the reaction rate was investigated. The radius of the activated complex at different temperatures was calculated. The isocomposition and isodielectric energies as well a« the thermodynamic parameters of activation were calculated and their significance in terms of solvent composition has been discussed. It was concluded that the reactant state is extensively higher solvated than the transition state by the highly polar (water) solvent. | | |
Reference
| (Z. Naturforsch. 33b, 30—34 [1978]; received July 15 1977) | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0030.pdf | | | Identifier
| ZNB-1978-33b-0030 | | | Volume
| 33 | |
9 | Author
| Aftabuddin Ahmed, Wolfgang Schwarz, Heinz Hess | Requires cookie* | | Title
| Dibrom Preparation and Crystal Structure  | | | Abstract
| (dimethylamino)alan und Diiod(dimethylamino)alan. Darstellung und Kristallstruktur Dibromo(dimethylamino)alane and Diiodo(dimethylamino)alane. Dibromo(dimethylamino)alane, Diiodo(dimethylamino)alane, Crystal Structure The title compounds were prepared by reaction of dimethylaminoalane with mercury -(II) dibromide and diiodide, respectively, and investigated by X-ray diffraction. Both compounds build structures isotype with that of dichloro(dimethylamino)alane. The molecules exist as dimers with a planar four-membered ring of alternating aluminium and nitrogen atoms. These atoms are four-coordinated. The following bond lengths are found: Al-N 1.94 and 1.95 A, Al-Br 2.26 A, Al-I 2.49 A, N-C 1.50 and 1.55 A. | | |
Reference
| (Z. Naturforsch. 33b, 43—46 [1978]; eingegangen am 21. Oktober 1977) | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0043.pdf | | | Identifier
| ZNB-1978-33b-0043 | | | Volume
| 33 | |
10 | Author
| Ingo-Peter Lorenz, JohnKoshy Thekumparampil | Requires cookie* | | Title
| Koordinationschemie ambivalenter Liganden, VIII 1 Synthese und Reaktivität ionischer und kovalenter Sulfinato-Komplexe von Tetraorganyl-VB-Elementen des Typs R4'E02SR Synthesis and Reactivity of Ionic and Covalent Sulfinato Complexes of Tetraorganyl-VB-Elements of the Type R4'E02SR  | | | Abstract
| The synthesis of the sulfinato derivatives 1-7 of pentavalent YB-elements follows equation (2). These compounds differ significantly in their physical and chemical properties and in their structures. In between the extremes of the purely ionic tetramethylam-monium sulfinates la-c and the typically covalent and pentacoordinated tetraorganyl-sulfinato-O-stiboranes 6-7, there are the hexa-or pentavalent compounds of phosphorus and arsenic 2 and 4 or 3 and 5 with sulfinato-0,0' or sulftnato-0 linkage, which dissociate readily into their ionic components. 1 a-c are suitable for the synthesis of sulfones according to equation (3). All of the methylsulfinato derivatives can be easily transformed (equation (4)) into the corresponding sulfonates by air oxidation. Only the tetraphenylsulfinato-O-stiboranes 7 a-c show S02-elimination forming pentaorganylstiboranes (equation (5)). IR, mass and in some cases NMR spectra are reported. | | |
Reference
| (Z. Naturforsch. 33b, 47—58 [1978]; eingegangen am 22. August/22. November 1977) | | |
Published
| 1978 | | |
Keywords
| Ionic Ammoniumsulfinates, Sulfinato-0 Derivatives, Covalent Tetraorganyl-sulfinato-O-stiboranes, IR, NMR | | |
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| default:Reihe_B/33/ZNB-1978-33b-0047.pdf | | | Identifier
| ZNB-1978-33b-0047 | | | Volume
| 33 | |
11 | Author
| LauriH J Lajunen, Raekko Kivekäs | Requires cookie* | | Title
| Formation of Copper(II) Complexes of l,3-Diamino-2-propanol in Aqueous Solution  | | | Abstract
| Copper(II) Complexes, l,3-Diamino-2-propanol The complex formation between Cu 2+ ions and l,3-diamino-2-propanol has been studied potentiometrically at 25 °C, constant ionic strength equal to 0.1 M NaC104, and pH 5-11. The nature of the complexes has been established by examining the standard deviations and values of the agreement index R of different models. | | |
Reference
| (Z. Naturforsch. 33b, 59—61 [1978]; received October 171977) | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0059.pdf | | | Identifier
| ZNB-1978-33b-0059 | | | Volume
| 33 | |
12 | Author
| Giacomo Martini, M.Francesca Ottaviani | Requires cookie* | | Title
| ESR Study of Copper Complexes Adsorbed on Fully Hydrated X and Y Zeolites  | | | Abstract
| ESR, Cu(II) Complexes, Synthetic Zeolites The ESR spectroscopy is used for the study of the motion of Cu(en)2 2+ and Cu(tmen)(OH)2 in fully hydrated X and Y zeolites. At room temperature steric hindrance in the faujasite cavities and slow motion condition lead to partially anisotropic spectra. In frozen samples, calculation of bonding coefficients indicate small interaction with surface walls. | | |
Reference
| (Z. Naturforsch. 33b, 62—66 [1978]; received October 12 1977) | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0062.pdf | | | Identifier
| ZNB-1978-33b-0062 | | | Volume
| 33 | |
13 | Author
| M.Sakhawat Hussain | Requires cookie* | | Title
| Cyclic Amidines Complexes: Complexes of 5:6:ll:12-Tetrahydro-2,8-dimethylphenhomazine with Copper(II), Nickel(II) and Zinc(H)  | | | Abstract
| Cyclic Amidines Complexes, Copper(II), Nickel(II), Zinc(II) The title compound, PHZ, can be viewed as 1,5-diazacyclooctane (daco) having carbon-3 and carbon-7 fused to benzene rings restricting the vibrational freedom of these carbons and rendering the axial positions in the complexes open for fifth and sixth coordination. Copper(II), nickel(H) and zinc(H) complexes of PHZ have been prepared. Copper(II) formed mono-and bis-complexes, whereas nickel(H) and zinc(II) formed only bis-complexes. The diamagnetic nickel(II) complexes are planar like the corresponding complexes of mesocyclic diamines, daco and dach. The copper(II) complexes differ appreciably from the mesocyclic diamine complexes of copper(II). Zinc (II) formed tetra-hedral complexes with two monodentate PHZ ligands and anions in the first coordination sphere. The structures of the complexes have been assigned by analysis of their spectral, magnetic and conductance data. The thermogravimetric studies of the complexes are also reported and discussed. | | |
Reference
| (Z. Naturforsch. 33b, 67—74 [1978]; received August 23 1977) | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0067.pdf | | | Identifier
| ZNB-1978-33b-0067 | | | Volume
| 33 | |
15 | Author
| IanF. Eckhard, NeilG. Keats, LindsayA. Summers | Requires cookie* | | Title
| Derivatives of 5H-Cyclopenta[2,l-b : 3,4-b']dipyridin-5-one (4,5-Diazafhioren-9-one)  | | | Abstract
| 5H-Cyclopenta[2,I-b: 3,4-b'Jdipyridin-5-one, Diquaternary Salts, Mass Spectra | | |
Reference
| (Z. Naturforsch. 33b, 80—83 [1978]; received August 8 1977) | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0080.pdf | | | Identifier
| ZNB-1978-33b-0080 | | | Volume
| 33 | |
17 | Author
| Bildung Von Pyrimidinthionen, Wolfgang Stadlbauer, Thomas Kappe, Erich Ziegler | Requires cookie* | | Title
| Zur Chemie des Kohlensubsulfids, III 1 Formation of Pyrimidinthiones  | | | Abstract
| Carbon Subsulphide, 2-Aminopyridine, N-Phenylbenzamidine, ß-Aminocrotonate Carbon subsulphide, C3S2, reacts with 2-aminopyridine (la) and N-phenylbenzamidine (lb) to yield the corresponding higher condensed derivatives 4 and 7. Attempts to obtain mesoionic compounds by reaction of N-substituted 2-aminopyridines or N,N'-disubsti-tuted benzamidines were not successful. Efforts to yield a pyridinethione derivative by reaction of C3S2 with /?-aminocrotonate (lc) failed. In this case the sulphur-bridged compound 8 could be isolated. | | |
Reference
| (Z. Naturforsch. 33b, 89—93 [1978]; eingegangen am 27. September 1977) | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0089.pdf | | | Identifier
| ZNB-1978-33b-0089 | | | Volume
| 33 | |
19 | Author
| Klaus Albert, Hans-Peter Schneider, Dieter Koch, Anton Rieker | Requires cookie* | | Title
| Synthese und 13 C-NMR-Spektren ferJ-butylierter Cyclohexenon-Epoxide Synthesis and 13 C NMR Spectra of £erf-Butylated Cyclohexenone Epoxides  | | | Abstract
| Phenol Degradation Products, Epoxidation, Cyclohexenone Epoxides, 13 C PFT NMR 13 C NMR spectra of several cyclohexenone epoxides obtained by oxygenation of 4-R-2,6-di-<er<-butylphenols have been assigned, using substituent induced shifts, off-resonance and C-H single-frequency-decoupling techniques, as well as completely C-H coupled spectra. For the -butyl signals the following sequence rules are relevant: | | |
Reference
| (Z. Naturforsch. 33b, 100—105 [1978]; eingegangen am 10. Oktober 1977) | | |
Published
| 1978 | | |
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| default:Reihe_B/33/ZNB-1978-33b-0100.pdf | | | Identifier
| ZNB-1978-33b-0100 | | | Volume
| 33 | |
20 | Author
| Claudia Bäk, Klaus Praefcke | Requires cookie* | | Title
| Photoreaktionen 2.2'-dihalogensubstituierter Benzoinether und Benzildimethylmonoketale in Lösung 1 Photoreactions of 2,2'-Dihalogen Substituted Benzoin Ether and Benzildimethylmonoketals in Solution  | | | Abstract
| The synthesis of a,a'-dihalogenated benzoin ether 6 and benzildimethylmonoketals 7 are discribed. Their reaction behavior under UV irradiation and electron impact conditions are discussed in comparison with those of arylesters 1 of seleno and thiobenzoic acid. The photoproducts of 6 and 7 are separated and identified with help of column or vaporphase chromatography. Photoinduced a-cleavages of 6 and 7 produce 2-halogenbenzoyl radicals 9 and a-monomethoxybenzyl radicals 10 or a,a-dimethoxybenzyl radicals 15 resp., which undergo four different stabilization reactions under formation of 1) 2-halogenbenzaldehydes 12 from 9 by hydrogenabstraction, 2) 2,2'-dihalogenbenzils 11 and l,2-di(2-chlorophenyl)-1,2-dimethoxyethan (13) via dimerization of 9 or 10 resp., 3) methylesters 16 of 2-halogen-benzoic acids by /^-elimination of methylradicals from 15, and 4) 2-halogenacetophenones 17 via combination of 9 with methylradicals from 15. In addition to these photoproducts 2-phenylbenzoic acidester 18, benzaldehyde (19), and acetophenone (20) are formed by photosubstitution of halogens in benzaldehydes 12 as well as in acetophenones 17 against hydrogen and in benzoic acid-esters 16 against phenyl resp. Independent photoexperi-ments prove 1) the formation of 2-phenylbenzoic acidester 18 by halogen-phenylreplace-ment in 16 and 2) that chlorine is easier than bromine, both in orZ/io-position to a carboxyl function, substituted by phenyl. No photoproducts {e.g. 8 or 14) are formed by substitution of halogen in the 2-halogenbenzoyl part of a-cleavage against neither a-monomethoxybenzyl nor a,a-dimethoxybenzylradicals resp. as expected like the photoinduced formation of selenoxanthones or thioxanthones 2 from selenol-or thiolesters 1. | | |
Reference
| (Z. Naturforsch. 33b, 106—112 [1978]; eingegangen am 5. Oktober 1977) | | |
Published
| 1978 | | |
Keywords
| Carbonyl Compounds, a-Cleavages, Free Radicals, Aromatic Photosubstitutions | | |
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| default:Reihe_B/33/ZNB-1978-33b-0106.pdf | | | Identifier
| ZNB-1978-33b-0106 | | | Volume
| 33 | |
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