Published by De Gruyter

Volume 38 Issue 3

Issue of Zeitschrift für Naturforschung B

Contents
Journal Overview

Open Access June 2, 2014

Atran-analoge Verbindungen des Typs / Atrane Analogous Compounds of Type

Joseph Grobe, Nikolaos Voulgarakis

Page range: 269-279

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Abstract

Heterocyclic ring compounds of type I (compounds 9 and 10) have been prepared by condensation reactions of α,ω-difunctional derivatives XMe 2 SiCH 2 M'Me 2 X (X = Cl, NMe 2 ; M' - Si, Sn) with N-methyldiethanolamine using the "Dilution Principle". The starting compounds XMe 2 SiCH 2 M'Me 2 X are obtained by reacting XMe 2 SiCH 2 MgCl with ClM'Me 2 X (Scheme, Abb. 1). The existence of transanular N→Si or N→M' interactions depends on the N-M distance and the acidity of the acceptor atoms. In order to clarify the weight of these factors acyclic analoga of compounds 9 and 10 have been prepared.

Open Access June 2, 2014

Alternativ-Liganden, XIV [1]. Neue Chelatliganden des Typs (2-Me₂E′C₆H₄)Si(EMe₂)Me₂ (E, E′ = N, P, As; Me = CH₃) / Alternative Ligands, XIV [1]. Novel Chelating Ligands of the Type (2-Me₂E′C₆H₄)Si(EMe₂)Me₂ (E, E′ = N, P, As; Me = CH₃)

Paraskevas Aslanidis, Joseph Grobe

Page range: 280-288

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Abstract

Chelating ligands of the type (2-Me 2 NC 6 H 4 )Si(EMe 2 )Me 2 (E = N, P, As) are prepared by ortho-lithiation of N,N-dimethylaniline followed by reaction with ClSi(NMe 2 )Me 2 to yield (2-Me 2 NC 6 H 4 )Si(NMe 2 )Me 2 . Cleavage of the SiN-bond with MePCl 2 affords (2-Me 2 NC 6 H 4 )Si(Cl)Me 2 , which on substitution with LiEMe 2 (E = P, As) gives the corresponding ligands. Synthesis of (2-Me 2 E'C 6 H 4 )Si(EMe 2 )Me 2 with E' = P or As is accomplished by producing 2-ClC 6 H 4 MgBr followed by reaction with either Me 2 E'Cl or ClSi(NMe 2 )Me 2 to yield (2-ClC 6 H 4 )E'Me 2 and (2-ClC 6 H 4 )Si(NMe 2 )Me 2 , respectively. The second donor group is introduced by Cl/Li exchange and reaction of the resulting lithium compounds with either ClSi(NMe 2 )Me 2 or Me 2 E'Cl. (2-Me 2 PC 6 H 4 )Si(NMe 2 )Me 2 and (2-Me 2 AsC 6 H 4 )Si(NMe 2 )Me 2 then are used to prepare the additional four ligands with E, E' = P, As via (2-Me 2 E'C 6 H 4 )Si(Cl)Me 2 by substitution with LiEMe 2 .

Open Access June 2, 2014

Alternativ-Liganden, XV [1]. Neue Liganden des Typs (4-XC₆H₄)SiMe(EMe₂)CH₂CH₂E′Me₂ (E, E′ = N, P, As; X = Cl, F; Me = CH₃) / Alternative Ligands, XV [1]. Novel Ligands of the Type (4-XC₆H₄)SiMe(EMe₂)CH₂CH₂E′Me₂ (E, E′ = N, P, As; X = Cl, F; Me = CH₃)

Paraskevas Aslanidis, Joseph Grobe

Page range: 289-298

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Abstract

Starting from Cl 2 Si(Me)CH = CH 2 (1) the title compounds are obtained by two different routes: a) Ligands with E = N and E' = N, P, As are prepared by aminolysis of 1 yielding Cl(Me 2 N)Si(Me)CH = CH 2 (2) followed by SiCl-substitution with (4-ClC 6 H 4 )MgCl (3). Photochemical or base catalyzed addition of HE'Me 2 (E' = N, P, As) to the vinyl group of (4-ClC 6 H 4 )SiMe(NMe 2 )CH = CH 2 (4) produces the corresponding ligands 5 to 7 (Abb. 2). Cleavage of the SiN bond in 7 leads to (4-ClC 6 H 4 )SiMe(Cl)CH 2 CH 2 NMe 2 (8) which on substitution with LiEMe 2 (E = P, As) gives the ligands 9 and 10. b) Ligands with E, E' = P, As are obtained by first introducing the aryl substituent to yield (4-ClC 6 H 4 )SiMe(Cl)CH = CH 2 (11) which by photochemical addition of HE'Me 2 (E' = P, As) gives the semi-ligands 12 and 13. Replacement of SiCl by SiEMe 2 (E = P, As) with LiEMe 2 affords compounds 14 to 17 (Abb. 3). - Some representative ligands with p-fluorophenyl groups (19, 20, 24, 25) are prepared by similar procedures (Abb. 4). New compounds are characterized by spectroscopic methods (IR, NMR, MS).

Open Access June 2, 2014

Darstellung and Kristallstruktur von [(C₆H₅)₄As]₂M(NO₃)₅ (M = Ho, Er, Tm, Yb) / Preparation and Crystal Structure of [(C₆H₅)₄As]₂M(NO₃)₅ (M = Ho, Er, Tm, Yb)

W. Urland, E. Warkentin

Page range: 299-302

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Abstract

The compounds [(C 6 H 5 ) 4 As] 2 M(NO 3 ) 5 (M = Ho, Er, Tm, Yb) were prepared and investigated by X-ray diffraction. It has been found that they are isotypic with [(C 6 H 5 ) 4 As] 2 Eu(NO 3 ) 5 . The structure was refined by single crystal data for [(C 6 H 5 ) 4 As] 2 Er(NO 3 ) 5 .

Open Access June 2, 2014

Triphenylstannyltris(trimethylphosphan)cobalt - Molekülstruktur und Eigenschaften / Triphenylstannyltris(trimethylphosphane)cobalt -Molecular Structure and Properties

Hans-Friedrich Klein, Klaus Ellrich, Dietmar Neugebauer, Olli Orama, Karl Krüger

Page range: 303-310

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Abstract

Potassium cobaltates K+CoLsL' -(L = Me 3 P, L' = N 2 , olefin) react with SnCl(C 6 H 5 ) 3 or GeBr(CeH 5 ) 3 to give tetracoordinate complexes containing Co-Sn and Co-Ge bonds. Crystal and molecular structures of two single crystals were determined. They show tetrahedral molecules Co[Sn(C 6 H 5 ) 3 ][P(CH 3 ) 3 ] 3 in different packing order. Both tetra-coordinate compounds take up small ligands thereby completing their 18-electron valence shells in compounds Co[E(C 6 H 5 ) 3 ]L 3 L' (L = (CH 3 ) 3 P; E = Ge, L' = CO; E = Sn, L' = CO, C 2 H 4 ). A sparingly soluble paramagnetic adduct Co[Sn(C 6 H 5 ) 3 ]L 4 is believed to contain a tin-bonded phosphane.

Open Access June 2, 2014

Die quaternären Systeme ZnAl₂S₄-ZnGa₂S₄, ZnAl₂S₄-CdAl₂S₄ und ZnAl₂S₄-ZnAl₂Se₄. Röntgenographische und schwingungsspektroskopisehe Untersuchungen / Investigation of the Quaternary Systems ZnAl₂S₄-ZnGa₂S₄, ZnAl₂S₄-CdAl₂S₄ and ZnAl₂S₄-ZnAl₂Se₄ by X-Ray Diffraction and Vibrational Spectroscopy

H. Haeuseler, A. Cansiz

Page range: 311-316

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Abstract

The quasi-binary systems Zn 1-x Cd x Al 2 S 4 , ZnAl 2(1-x) Ga 2x S 4 and ZnAl 2 S 4(1-x) Se 4x have been investigated by X-ray diffraction and vibrational spectroscopy. In the spinel ZnAI 2 S 4 up to 20% of Zn can be replaced by Cd. In the two other systems, ZnAl 2 S 4 has no detectable homogeneity range. The thiogallate phases have much broader ranges of homogeneity. The compositions of the compounds at the phase boundary of the thiogallate phase are Zn 0.4 Cd 0.6 Al 2 S 4 , ZnGa 0.4 Al 1.6 S 4 , and ZnAl 2 S 2.8 Se 1.2 . At approximately 950 °C ZnAl 2 Se 4 undergoes a reversible phase transition to a wurtzite-type structure. This phase transition is also observed for the solid solutions ZnAl 2 S 4(1-x) Se 4x ; with 1.0 > x > 0.3. The FIR spectra are discussed.

Open Access June 2, 2014

Über die Staudinger-Reaktion mit Tantaltetrachloridazid. Die Kristallstruktur von Tantal(V)-(triphenylphosphinimino)tetrachlorid, Ta[NP(C₆H₅)₃]Cl₄ / On the Staudinger Reaction with Tantalum Tetrachloride Azide. The Crystal Structure of Tantalum(V)(triphenyl-phosphinimino)tetrachloride, Ta[NP(C₆H₅)₃]Cl₄

Hans Bezler, Joachim Strähle

Page range: 317-320

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Abstract

[TaCl 4 N 3 ] 2 reacts easily with PPh 3 yielding TaCl 4 (NPPh 3 ) , TaCl 4 (NPPh 3 )(NHPPh 3 ) and TaCl 5 . The latter are supposed to be products of the reaction of primarily formed TaCl 4 (NPPh 3 ) 2 -TaCl 4 + with the solvent ClCH 2 -CH 2 Cl. TaCl 4 (NPPh 3 ) crystallizes in the monoclinic system with the space group P2 1 /c. The crystal structure shows centrosymmetric dimers, in which the Ta atoms are linked together by asymmetric Cl bridges. The phosphinimino ligand is coordinated trans to the Cl bridge and causes a strong trans effect. A linear P = N = Ta group with double bonds of P = N = 159.3 and Ta = N = 180,1 pm is observed.

Open Access June 2, 2014

[1]Metallocenophane: ¹H-NMR-Untersuchungen / [1]Metallocenophanes: ¹H NMR Investigations

Hartmut Köpf, Nikolaos Klouras

Page range: 321-325

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Abstract

The synthesis of a series of [1]metallocenophanes has been achieved. The structure and conformation of these compounds are discussed in the light of their 1 H NMR spectra.

Open Access June 2, 2014

Schwefel-Stickstoff-Verbindungen, XII [1]. ¹⁹F-NMR-und ¹³C-NMR-spektroskopische Untersuchung einiger aromatisch substituierter Schwefeldiimide / Sulfur-Nitrogen Compounds, XII [1]. ¹⁹F NMR and ¹³C NMR Spectroscopic Investigation of Some Aromatic Substituted Sulfurdiimides

Gilbert Brands, Alfred Golloch

Page range: 326-331

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Abstract

19 F NMR and 13 C NMR spectra of the sulfur(IV)diimines R 1 -NSN-R 2 (R 1/2 = C 6 H 5 , C 6 F 5 , C 6 H 5 S, C 6 F 5 S) and the corresponding N-sulfinylamines R 1/2 -NSO are discussed. Chemical shifts are correlated to the electron withdrawing properties of the substituents.

Open Access June 2, 2014

Bor- und Arsen-methoxotetrafluorotellurate(VI) / Boron and Arsenic Methoxotetrafluorotellurates(VI)

Walter Tötsch, Heinrich Aichinger, Fritz Sladky

Page range: 332-334

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Abstract

The interaction of cis-and trans-HOTeF 4 OCH 3 with BCl 3 yields B(cis-and trans-OTeF 4 OCH 3 ) 3 . The ability of these compounds to transfer the CH 3 OTeF 4 O entities has been demonstrated in reactions with AsF 3 , with the formation of As (cis-and trans-OTeF 4 OCH 3 ) 3 respectively. All compounds have been characterized by NMR spectroscopy ( 125 Te, 19 F, 11 B, 1 H).

Open Access June 2, 2014

Molekülstrukturen, Schwingungsspektren und Konformation der Thiooxalsäurederivate CH₃S-CO-CONH₂, CH₃S-CS-CONH₂, C₂H₅O-CO-CSNH₂ und K[OSC-CONH₂] / Molecular Structure, Vibrational Spectra and Conformation of the Thiooxalic Acid Derivatives CH₃S-CO-CONH₂, CH₃S-CS-CONH₂, C₂H₅O-CO-CSNH₂ and K[OSC-CONH₂]

Rainer Mattes, Franz Waldmann

Page range: 335-340

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Abstract

The crystal structures of CH 3 S-CO-CONH 2 (1), CH 3 S-CS-CONH 2 (2), C 2 H 5 O-CO-CSNH 2 (3) and K[OSC-CONH 2 ] (4) have been determined by single crystal X-ray diffraction. The molecules 1, 2 and 3 are nearly planar and form centrosymmetric dimers by N H···O or N-H···S hydrogen bonds with the amidic oxygen or sulfur atom as acceptor atoms. The anion of 4 is not quite planar. The torsional angle around the C-C bond is 18.4°. The conformations of the title compounds are E, Z' (1 and 2), Z, Z' (3) and Z (4). According to the vibrational spectra, which are discussed briefly, 1 and 3 retain their conformation also in solution.

Open Access June 2, 2014

Darstellung und Kristallstruktur des 2:3-Adduktes von Antimontrichlorid und 4-Phenylpyridin, 2 SbCl₃ · 3 (C₁₁H₉N) / Preparation and Crystal Structure of the 2:3 Adduct of Antimony Trichloride and 4-Phenylpyridine, SbCl₃ · 3 (C₁₁H₉N)

Annegret Lipka

Page range: 341-346

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Abstract

A congruently melting phase of molar ratio 2:3 was identified in the system SbCl 3 /4-phenylpyridine. The structure consists of two different types of complex units: One SbCl 3 molecule is bonded to one 4-phenylpyridine ligand only, whereas the other one forms a complex with two 4-phenylpyridine ligands. The SbCl 3 unit in the 1:1 species is pyramidally shaped, whereas the SbCl 3 unit in the 1:2 species displays a T-shaped geometry. The mean angle between the phenyl and pyridyl planes is 33.3°; mean bond lengths are 〈Sb-Cl〉 = 247.6 pm and 〈Sb-N〉 = 241.7 pm.

Open Access June 2, 2014

Zur Darstellung und Struktur des 1.3-Dichloro-5-N.N-dimethylamino-1.3-dithia-2.4.6-triazins / Synthesis and Structure of 1,3-Dichloro-5-N,N-dimethylamino-1,3-dithia-2,4,6-triazine

Herbert W. Roesky, Pierre Schäfer, Mathias Noltemeyer, George M. Sheldrick

Page range: 347-349

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Abstract

The six membered ring of composition (CH 3 ) 2 NCN 3 S 2 Cl 2 3 a was prepared from N,N-dimethylguanidinhydrochloride and trithiadiazindichloride. 3 a was characterized on the basis of mass, 1 H, 13 C NMR spectra and X-ray structure analysis. Crystals of 3 a are monoclinic, space group P2 1 /c, with a = 660.3(6), b = 834.5(7), c = 1774.7(15) pm, β = 112.83(6)° and Z = 4. The C 2 N unit lies approximately in the plane of the [-CNSNSN-] ring, with both Cl atoms on the same side of the ring.

Open Access June 2, 2014

Deprotonated Complexes of Bis(o-aminobenzenesulfonyl)ethylenediamine with Mn(II), Co(II), Ni(II) and Cu(II)

S. P. Perlepes, Th. F. Zafiropoulos, A. G. Galinos, J. M. Tsangaris

Page range: 350-356

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Abstract

The new complexes K 2 [ML 2 ] (M = ═Mn, Cu), K 2 [ML 2 (H 2 O) 2 ] (M = Co, Ni), K 2 [Cu 2 L 2 (OH) 2 ] and K 2 [Cu 2 L 2 (OH) 2 (H 2 O) 4 ], where LH 2 = Bis(o-aminobenzenesulfonyl)ethylenediamine, have been prepared. Properties, X-ray powder patterns, molar conductance measurements, magnetic moments and spectral (IR, diffuse reflectance, visible in solution) data are discussed in terms of possible structural types and the nature of the bonding. Distorted octahedral geometries are proposed for the Mn(II), Co(II), Ni(II) and dimeric Cu(II) chelates in the solid state, while K 2 [CuL 2 ] appears to have a distorted tetrahedral structure. The Mn(II) complex exhibits evidence of a polymeric configuration. The L 2 - anion acts as a bidentate N 2 or tetradentate N 4 ligand.

Open Access June 2, 2014

Metallomethane, VI [1]. Kristallstruktur von Tetrakis(chloroquecksilber)methan-Dimethylsulfoxid C(HgCl)₄ · (CH₃)₂SO / Metallomethanes, VI [1]. Crystal Structure of Tetrakis(chloromercuri)methane-Dimethylsulfoxide C(HgCl)₄ · (CH₃)₂SO

Dietrich K. Breitinger, Günter Petrikowski, Günter Liehr, Raymond Sendelbeck

Page range: 357-364

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Abstract

The tetrakis (halomercuri) methane dimethylsulfoxide solvates C(HgX) 4 · DMSO (X = Cl and Br) have been prepared. - The crystal structure of the chloro compound C(HgCl) 4 · DMSO has been determined (R = 0.0611 and Rw = 0.0562). The compound crystallizes in space-group P2 1 /n with a = 1854(1) pm, b = 727.3(5) pm, c = 1049.1(6) pm, β = 94.82(3)°, Z = 4; d c = 4.873 g·cm -3 , d 0 = 4.51 g-cm -3 . - The C(HgCl) 4 molecules have C-Hg bond lengths in the range 201.4(26) to 209.9(27) pm (average 207.0 pm), and Hg-Cl bonds between 231.4(9) and 234.2(9) pm (average 233.2 pm). The bond angles Hg-C-Hg vary from 107.3(3) to 111.7(4)° (average 109.5°), and the angles C-Hg-Cl are found within the limits 172.2(24) and 178.3(25)° (mean 174.3°). DMSO molecules (S-O bond 148.6(23)pm) are coordinated via oxygen to two Hg atoms of one C(HgCl) 4 molecule and to one Hg atom of a neighbouring C(HgCl) 4 molecule forming two bifurcated bridges in a dimer [C(HgCl) 4 · DMSO] 2 ; two strong Cl→···Hg and two weak S→···Hg interactions also contribute to this pair formation. The dimeric units are arranged to layers in the planes (100) and (200), such that each C(HgCl) 4 molecule has six C(HgCl) 4 and two DMSO molecules as neighbours; with two C(HgCl) 4 molecules from each adjacent layer, each C(HgCl) 4 molecule achieves a total coordination number of ten. Depending on the van der Waals radius assumed for mercury a packing coefficient 0.640 ≤ k ≤ 0.691 is obtained. - Cryoscopy and vibrational spectrometry suggest monomeric, unperturbed tetrahedral C(HgX) 4 molecules in DMSO solutions.

Open Access June 2, 2014

Diphenylphosphino -α -aminosäureester als Liganden in Palladium(II)-und Platin(II)-Komplexen [1] / Diphenylphosphino-α-Amino Acid Esters as Ligands in Palladium(II) and Platinum(II) Complexes [1]

Herbert Trampisch, Wolfgang Beck

Page range: 365-369

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Abstract

cis-Dichlorobis(chlorodiphenylphosphine)palladium-and platinum(II) react with N-alkyl-α-amino acid esters to give the complexes MCl 2 [Ph 2 PN(R)C(H)(R')CO 2 Me] 2 (M = Pd, Pt; R = CH 2 Ph, i-C 3 H 7 ; R' = CH 3 , CH 2 Ph). With lysine ester dimeric, bis(chelate) complexes (M = Pd, Pt; R = CH 3 , C 2 H 5 ) have been isolated. The reaction of cis-MCl 2 (PPh 2 Cl) 2 with cysteine and serine methylester affords the complexes MCl 2 [Ph 2 P(X)CH 2 C(H)(NH 2 )CO 2 CH 3 ] 2 (M = Pd, Pt; X = O, S).

Open Access June 2, 2014

Reaktionen von S-Methylthiireniumsalzen mit nucleophilen Übergangsmetall-Komplexen [1] / Reactions of S-Methylthiirenium Salts with Nucleophilic Transition Metal Complexes [1]

Franz Götzfried, Wolfgang Beck

Page range: 370-372

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Abstract

Abstract 1 -Methyl-2,3-di-t-butyl-thiirenium-tetrafluoroborate (1) reacts with K + [π-C 5 H 5 (CO) 3 Mo] and (PPh 3 ) 4 Pt to give [(π-C 5 H 5 )(CO) 2 MoSCH 3 ] 2 and [(Ph 3 P) 3 PtSCH 3 ] + BF 4 - , respectively. With 1 and (Ph 3 P) 4 Pd the phosphonium salt [Ph 3 PSCH 3 ] + BF 4 -has been isolated.

Open Access June 2, 2014

Zur Struktur von (Pyrazolinonyl)-(hydroxypyrazolylium)methanperchloraten NMR-, IR-spektroskopische Studien und Kristallstruktur / The Structure of (Pyrazohnonyl)-(hydroxypyrazolyhum)methaneperchlorates NMR, IR Spectroscopic Studies and Crystal Structure

Christian Burschka, Eyup Akgün, Ulf Pindur

Page range: 373-377

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Abstract

The structures of 1a-1d were investigated by spectroscopic methods and in the case of la in addition by X-ray diffraction, 1a, vicarious for the compounds 1, is stabilized in solution and in the crystal by an intramolecular hydrogen bond in an eight-membered ring. The IR and NMR spectra show that 1 exhibit a symmetrical structure. In the case of 1 a the molecular structure is affected by unsymmetrical packing and electrostatic effects in the crystal and is therefore approximated best between the forms I and II.

Open Access June 2, 2014

Lösliche Phthalocyaninatometalloxane, Dotierung und Leitfähigkeit / Soluble Phthalocyaninatometaloxanes, Doping and Conductivity

Josef Metz, Georg Pawlowski, Michael Hanack

Page range: 378-382

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Abstract

The polymeric μ-oxo-(tetraalkylphthalocyaninato)-metal IV B derivatives 1 a-d were synthesized by thermal condensation of the monomeric dihydroxo(tetraalkylphthalo-cyaninato)-metal IV B compounds 5 a-d. The high solubility of the metaloxanes 1 a-d enables a homogeneous reaction with the dopant. The electrical conductivities of the undoped and doped compounds are reported.

Open Access June 2, 2014

Derivate des Benzo[1.3]dioxols, 47 [1]. Darstellung und Reaktionen des 4.8-Dimethoxy-bis[1.3]dioxolo[4.5]benzo- [1.2-d; 1′ .2′ -f] [1.3]dioxepins / Derivatives of 1,3-Benzodioxoles, 47 [1]. Preparation and Reactions of 4,8-Dimethoxy-bis[1,3]dioxolo[4,5]benzo- [1,2-d; 1',2'-f][1,3]dioxepine

Franz Dallacker, Wim Coerver

Page range: 383-391

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Abstract

In 1957 some dibenzo[d,f][1,3]dioxepines were isolated from Cercospora kikuchii. We describe the preparation of 4,8-dimethoxy-bis[1,3]dioxolo[4,5]benzo[1,2-d; 1',2'-f][1,3]-dioxepine (3). It shows a high S E -reactivity. Bromination yields the monobromo-and dibromocompounds 3 a and 3 b. Treatment of 3 with copper(II) nitrate leads to the dinitrocompound 3c. With the same reagent 3a gives 3d. Reduction of 3d with hydrogen and Palladium as catalyst yields the mono-amine 3e under bromine loss. Under the same reduction conditions in acetic anhydride 3d and 3c yields 3f respectively 3g. The carboxylic acid 3i and the aldehyd 3h are prepared by bromine-lithium exchange from 3 a. In the same manner the dibromocompound 3 b is a suitable starting material to obtain the dicarboxylic acid 3k and the dialdehyd 3j. 3j undergoes easily a thiazolium catalysed oin-condensation, yielding the phenanthrenequinone 3l. The cyclic anhydride 3 m can be prepared by heating 3 k in acetic anhydride.

Open Access June 2, 2014

Derivate des 1.3-BenzdioxoIs, 48 [1]. Darstellung und Reaktionen von substituierten 1.3-Benzdioxol-4.7-cliinonen / Derivatives of 1,3-Benzdioxoles, 48 [1]. Preparation and Reactions of 1,3-Benzdioxole-4,7-quinones

Franz Dallacker, Bodo Holtmann, Wim Coerver

Page range: 392-397

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Abstract

We describe the preparation of a substituted 1,3-benzdioxole-4,7-quinonecomplex (2) by reaction of 4-hydroxy-1,3-benzdioxole (1) with potassiumnitrosodisulfonate. The quinones 4a-d can be obtained by treatment of the 4-hydroxy-7-methoxy-1,3-benzdioxoles 3 a-d with ammoniumcerium(IV)nitrate. Reaction of 2 with several cyclophiles gives the addition compounds resp. the dehydrogenation-products 6b-d in partly high yields.

Open Access June 2, 2014

Ylide von Heterocyclen, V [1]. I-, N-und S-Ylide des 2-Pyrons und 2-Pyridons / Ylides of Heterocycles, V [1]. I-, N-and S-Ylides of 2-Pvrones and 2-Pyridones

Thomas Kappe, Gertraud Korbuly, Erik Pongratz

Page range: 398-403

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Abstract

The reaction of the pyrone 1 a or the pyridones 1 b, c with iodosobenzene leads to the iodonium-ylides 2 which undergo thermal rearrangement to the 4-phenyloxy-3-iodo compounds 3. Reductive deiodination of 3 gives the 4-phenyloxy compounds 4. By acid catalyzed treatment with nucleophiles (such as pyridine, nicotinamide, isoquinoline and thiophane) the iodonium-ylides 2 can be converted into the corresponding N- and S-ylides 5. Reaction of 2 with concentrated HCl or HBr gives the 3-halogeno substituted compounds 6.

Open Access June 2, 2014

NOTIZEN. Darstellung und Struktur von Ba₆Sn₂P₆ / Preparation and Crystal Structure of Ba₆Sn₂P₆

Brigitte Eisenmann, Hanna Jordan, Herbert Schäfer

Page range: 404-406

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Abstract

The new compound Ba 6 Sn 2 P 6 crystallizes in the monoclinic system, space group P2 1 /c with lattice constants a = 883.7 ± 0.5 pm b = 1268.8 ± 0.8 pm c= 862.3 ± 0.5 pm β = 114.42 ± 0.10°. The compound is isotypic to K 6 Sn 2 Te 6 and contains the Sn 2 P 6 12- -anions which are isosteric with the Sn 2 Te 6 6- -units.

Open Access June 2, 2014

Direkte Lithiierung von BicycIo[3,2,1]octa-2.6-dien / Direct Lithiation of Bicyclo[3,2,1]octa-2,6-diene

Frank H. Köhler, Norbert Hertkorn

Page range: 407-408

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Abstract

Bicyclo[3,2,1]octa-2,6-diene (1) has been lithiated directly with t-butyllithium/TMEDA at low temperature. After quenching with tri-methyltin chloride essentially two stannyl derivatives of 1 were obtained. The stannyl group did not bind to the allylic carbon of 1 as expected but to C-6 and C-7. This has been shown by means of elemental analysis, mass spectroscopy as well as 1 H, 13 C and 119 Sn NMR spectroscopy.

About this journal

Objective
Zeitschrift fuer Naturforschung B (ZNB) publishes novel research in all areas of inorganic chemistry, organic chemistry, and analytical chemistry. In particular, the journal focuses on solid state chemistry, coordination chemistry, main group element chemistry, synthetic organic chemistry, natural product chemistry and, to a lesser extent, on analytical chemistry. For more than 65 years Zeitschrift fuer Naturforschung B has been open to contributions from all fields of experimental and theoretical chemistry. Zeitschrift fuer Naturforschung B publishes 12 issues per volume/year. Sometimes double issues occur.

Topics

Solid state chemistry
Coordination chemistry
Main group element chemistry
Organic chemistry
Natural product chemistry

Article formats
Original (full) papers, research notes and preliminary communications, reports on specific research topics of current interest (reviews)

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Volume 38 Issue 3

Issue of Zeitschrift für Naturforschung B

Atran-analoge Verbindungen des Typs / Atrane Analogous Compounds of Type

Abstract

Alternativ-Liganden, XIV [1]. Neue Chelatliganden des Typs (2-Me2E′C6H4)Si(EMe2)Me2 (E, E′ = N, P, As; Me = CH3) / Alternative Ligands, XIV [1]. Novel Chelating Ligands of the Type (2-Me2E′C6H4)Si(EMe2)Me2 (E, E′ = N, P, As; Me = CH3)

Abstract

Alternativ-Liganden, XV [1]. Neue Liganden des Typs (4-XC6H4)SiMe(EMe2)CH2CH2E′Me2 (E, E′ = N, P, As; X = Cl, F; Me = CH3) / Alternative Ligands, XV [1]. Novel Ligands of the Type (4-XC6H4)SiMe(EMe2)CH2CH2E′Me2 (E, E′ = N, P, As; X = Cl, F; Me = CH3)

Abstract

Darstellung and Kristallstruktur von [(C6H5)4As]2M(NO3)5 (M = Ho, Er, Tm, Yb) / Preparation and Crystal Structure of [(C6H5)4As]2M(NO3)5 (M = Ho, Er, Tm, Yb)

Abstract

Triphenylstannyltris(trimethylphosphan)cobalt - Molekülstruktur und Eigenschaften / Triphenylstannyltris(trimethylphosphane)cobalt -Molecular Structure and Properties

Abstract

Die quaternären Systeme ZnAl2S4-ZnGa2S4, ZnAl2S4-CdAl2S4 und ZnAl2S4-ZnAl2Se4. Röntgenographische und schwingungsspektroskopisehe Untersuchungen / Investigation of the Quaternary Systems ZnAl2S4-ZnGa2S4, ZnAl2S4-CdAl2S4 and ZnAl2S4-ZnAl2Se4 by X-Ray Diffraction and Vibrational Spectroscopy

Abstract

Abstract

[1]Metallocenophane: 1H-NMR-Untersuchungen / [1]Metallocenophanes: 1H NMR Investigations

Abstract

Schwefel-Stickstoff-Verbindungen, XII [1]. 19F-NMR-und 13C-NMR-spektroskopische Untersuchung einiger aromatisch substituierter Schwefeldiimide / Sulfur-Nitrogen Compounds, XII [1]. 19F NMR and 13C NMR Spectroscopic Investigation of Some Aromatic Substituted Sulfurdiimides

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Bor- und Arsen-methoxotetrafluorotellurate(VI) / Boron and Arsenic Methoxotetrafluorotellurates(VI)

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Abstract

Darstellung und Kristallstruktur des 2:3-Adduktes von Antimontrichlorid und 4-Phenylpyridin, 2 SbCl3 · 3 (C11H9N) / Preparation and Crystal Structure of the 2:3 Adduct of Antimony Trichloride and 4-Phenylpyridine, SbCl3 · 3 (C11H9N)

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Zur Darstellung und Struktur des 1.3-Dichloro-5-N.N-dimethylamino-1.3-dithia-2.4.6-triazins / Synthesis and Structure of 1,3-Dichloro-5-N,N-dimethylamino-1,3-dithia-2,4,6-triazine

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Deprotonated Complexes of Bis(o-aminobenzenesulfonyl)ethylenediamine with Mn(II), Co(II), Ni(II) and Cu(II)

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Metallomethane, VI [1]. Kristallstruktur von Tetrakis(chloroquecksilber)methan-Dimethylsulfoxid C(HgCl)4 · (CH3)2SO / Metallomethanes, VI [1]. Crystal Structure of Tetrakis(chloromercuri)methane-Dimethylsulfoxide C(HgCl)4 · (CH3)2SO

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Diphenylphosphino -α -aminosäureester als Liganden in Palladium(II)-und Platin(II)-Komplexen [1] / Diphenylphosphino-α-Amino Acid Esters as Ligands in Palladium(II) and Platinum(II) Complexes [1]

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Reaktionen von S-Methylthiireniumsalzen mit nucleophilen Übergangsmetall-Komplexen [1] / Reactions of S-Methylthiirenium Salts with Nucleophilic Transition Metal Complexes [1]

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Zur Struktur von (Pyrazolinonyl)-(hydroxypyrazolylium)methanperchloraten NMR-, IR-spektroskopische Studien und Kristallstruktur / The Structure of (Pyrazohnonyl)-(hydroxypyrazolyhum)methaneperchlorates NMR, IR Spectroscopic Studies and Crystal Structure

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Lösliche Phthalocyaninatometalloxane, Dotierung und Leitfähigkeit / Soluble Phthalocyaninatometaloxanes, Doping and Conductivity

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Derivate des Benzo[1.3]dioxols, 47 [1]. Darstellung und Reaktionen des 4.8-Dimethoxy-bis[1.3]dioxolo[4.5]benzo- [1.2-d; 1′ .2′ -f] [1.3]dioxepins / Derivatives of 1,3-Benzodioxoles, 47 [1]. Preparation and Reactions of 4,8-Dimethoxy-bis[1,3]dioxolo[4,5]benzo- [1,2-d; 1',2'-f][1,3]dioxepine

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Derivate des 1.3-BenzdioxoIs, 48 [1]. Darstellung und Reaktionen von substituierten 1.3-Benzdioxol-4.7-cliinonen / Derivatives of 1,3-Benzdioxoles, 48 [1]. Preparation and Reactions of 1,3-Benzdioxole-4,7-quinones

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Ylide von Heterocyclen, V [1]. I-, N-und S-Ylide des 2-Pyrons und 2-Pyridons / Ylides of Heterocycles, V [1]. I-, N-and S-Ylides of 2-Pvrones and 2-Pyridones

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NOTIZEN. Darstellung und Struktur von Ba6Sn2P6 / Preparation and Crystal Structure of Ba6Sn2P6

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Direkte Lithiierung von BicycIo[3,2,1]octa-2.6-dien / Direct Lithiation of Bicyclo[3,2,1]octa-2,6-diene

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Alternativ-Liganden, XIV [1]. Neue Chelatliganden des Typs (2-Me₂E′C₆H₄)Si(EMe₂)Me₂ (E, E′ = N, P, As; Me = CH₃) / Alternative Ligands, XIV [1]. Novel Chelating Ligands of the Type (2-Me₂E′C₆H₄)Si(EMe₂)Me₂ (E, E′ = N, P, As; Me = CH₃)

Alternativ-Liganden, XV [1]. Neue Liganden des Typs (4-XC₆H₄)SiMe(EMe₂)CH₂CH₂E′Me₂ (E, E′ = N, P, As; X = Cl, F; Me = CH₃) / Alternative Ligands, XV [1]. Novel Ligands of the Type (4-XC₆H₄)SiMe(EMe₂)CH₂CH₂E′Me₂ (E, E′ = N, P, As; X = Cl, F; Me = CH₃)

Darstellung and Kristallstruktur von [(C₆H₅)₄As]₂M(NO₃)₅ (M = Ho, Er, Tm, Yb) / Preparation and Crystal Structure of [(C₆H₅)₄As]₂M(NO₃)₅ (M = Ho, Er, Tm, Yb)

[1]Metallocenophane: ¹H-NMR-Untersuchungen / [1]Metallocenophanes: ¹H NMR Investigations

Schwefel-Stickstoff-Verbindungen, XII [1]. ¹⁹F-NMR-und ¹³C-NMR-spektroskopische Untersuchung einiger aromatisch substituierter Schwefeldiimide / Sulfur-Nitrogen Compounds, XII [1]. ¹⁹F NMR and ¹³C NMR Spectroscopic Investigation of Some Aromatic Substituted Sulfurdiimides

Darstellung und Kristallstruktur des 2:3-Adduktes von Antimontrichlorid und 4-Phenylpyridin, 2 SbCl₃ · 3 (C₁₁H₉N) / Preparation and Crystal Structure of the 2:3 Adduct of Antimony Trichloride and 4-Phenylpyridine, SbCl₃ · 3 (C₁₁H₉N)

Metallomethane, VI [1]. Kristallstruktur von Tetrakis(chloroquecksilber)methan-Dimethylsulfoxid C(HgCl)₄ · (CH₃)₂SO / Metallomethanes, VI [1]. Crystal Structure of Tetrakis(chloromercuri)methane-Dimethylsulfoxide C(HgCl)₄ · (CH₃)₂SO

NOTIZEN. Darstellung und Struktur von Ba₆Sn₂P₆ / Preparation and Crystal Structure of Ba₆Sn₂P₆