Published by De Gruyter

Volume 47 Issue 6

Issue of Zeitschrift für Naturforschung B

Contents
Journal Overview

Open Access June 2, 2014

Das 7,8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ⁵-phosphaspiro[4.4]nonanyl-Kation: Röntgenstrukturanalyse und temperaturabhängige ¹H-NMR-Spektren: The 7, 8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ^).5-phosphaspiro[4.4]nonanyl Cation: X-Ray Crystal Structure Determination and Variable ¹H NMR Spectra

Thomas Kaukorat, Peter G. Jones, Reinhard Schmutzler

Page range: 755-759

More Download PDF

Abstract

The 1 H NMR spectrum of the spirophosphorane 3 at room temperature indicates dynamic behaviour of the cation. The low-temperature 1 H NMR spectra of 3 exhibit two sets of doublets for the protons of the diastereotopic N(CH 3 ) 2 groups. The free enthalpy of activation for the dynamic process was determined (58.6 KJ/mole). In the reaction of 3 with sodium tetraphenylborate the crystalline compound, 4, involving the non-coordinating anion, [B(C 6 H 5 ) 4 ]-, was obtained. The X-ray crystal structure analysis of 4 reveals the presence of a five-membered ring, formally as a result of intramolecular donor-acceptor interaction between the nitrogen atom of the N(CH 3 ) 2 group and phosphorus. The geometry at phosphorus deviates somewhat from ideal trigonal bipyramidal.

Open Access June 2, 2014

Zur Chemie der 4,6-Dioxo-1,3,5,2 λ³-triazaphosphinane. / On the Chemistry of 4,6-Dioxo-1,3,5,2 λ³-triazaphosphinanes.

Teil II. Darstellung von 4,6-Dioxo-1,3,5,2 λ³-triazaphosphinanen / Part II. Preparation of 4,6-Dioxo-1,3,5,2 λ³-triazaphosphinanes

Christian Müller, Thomas G. Meyer, Michael Farkens, Ralf Sonnenburg, Reinhard Schmutzler

Page range: 760-766

More Download PDF

Abstract

In the reaction of phenylisocyanate, 1, with 1,3-dimethylurea, 2, and 1,3-diphenylurea, 4, 1,3-dimethyl-5-phenyl biuret, 3, and 1,3,5-triphenylbiuret, 5, respectively, were obtained. The reaction of 3, 5 and of 1,3,5-trimethylbiuret 6 with a range of P(III) chloro compounds has furnished the new 4,6-dioxo-1,3,5,2 λ 3 -triazaphosphinanes, 7-16. The characterization of 7-16 rests, especially, on their 1 H, 13 C and 31 P NMR, and mass spectra.

Open Access June 2, 2014

Neue Synthesen von Magnesiumhydrid / New Syntheses of Magnesium Hydride

Götz Koerner, Klaus-Dieter Klein, Wilfried Knott

Page range: 767-771

More Download PDF

Abstract

A very easy and safe way for the production of Ni-doped magnesium hydride is reported. Another process, which is not requiring transition metals (e. g. nickel) has also been found as a means to ameliorate the kinetics of hydrogen uptake. MgH 2 itself exerts a catalytic effect on the formation of magnesium hydride from the elements, i. e. by autocatalysis.

Open Access June 2, 2014

Complexes of (CF₃)₃B with Sterically Crowded Amines. Unexpected Side Products from the Trifluoromethylation of Cl₂BN(t-Bu)(Bz). Crystal and Molecular Structures of (CF₃)₃BNH(CH₂)₆, HO(CF₃)₂BCH(Ph)NH(t-Bu)(Bz) and Ph(CF₃)₂BCHN(t-Bu)(Bz)

Andreas Ansorge, David J. Brauer, Hans Bürger, Frank Dörrenbach, Burkhard Krumm, Gottfried Pawelke

Page range: 772-782

More Download PDF

Abstract

Trifluoromethylation of C1 2 BN(CH 2 ) 6 , Cl 2 B(tmp), tmp = 2,2,6,6-tetramethylpiperidino, and Cl 2 BN(t-Bu)(Bz) with three equivalents of CF 3 Br/P(NEt2) 3 yields the amine complexes (CF 3 ) 3 B · NH(CH 2 ) 6 (1), (CF 3 ) 3 B ·NH 2 CMe 2 (CH 2 ) 2 CHCMe 2 (2) and (CF 3 ) 3 B · NH 2 (Bz) (3). The preparation of 3 was accompanied by formation of three unexpected trifluoromethylboron derivatives X(CF 3 ) 2 BCH(Ph)NH(t-Bu)(Bz) (D), X = Br (4), Cl (5), and (Ph)(CF 3 ) 2 BCHN(t-Bu)(Bz) (6), the latter being formed from 4 by HBr elimination and rearrangement. Reaction of 4 with H 2 O, EtOH, HCONMe 2 and Me 3 SnH yielded D, X = OH (7), EtO (8), HCOO (9), and (Ph)(CF 3 ) 2 BCH 2 NH(t-Bu)(Bz) (10), respectively. The structures of 1, 6 and 7 have been determined by X-ray diffraction analysis.

Open Access June 2, 2014

Die Kristallstrukturen der Tetrafluoromanganate(III) AMnF₄ (A = K, Rb, Cs) / The Crystal Structures of the Tetrafluoromanganates(III) AMnF₄ (A = K, Rb, Cs)

Michel Molinier, Werner Massa

Page range: 783-788

More Download PDF

Abstract

The crystal structures of AMnF 4 compounds (A = K, Rb, Cs) were determined by X-ray diffraction on twinned single crystals: The K and Rb compound are isostructural: space group P21/a, Z = 4; KMnF 4 : lattice constants a = 769.9(2), b = 764.4(2), c = 576.9(1) pm, β = 90.54(3)°; R/wR = 0.029/0.025 for 481 reflections; pseudomerohedral (100) twin. RbMnF 4 : lattice constants a = 782.2(5), b = 777.7(3), c = 605.0(2) pm, β = 90.83(4)°; R/wR = 0.0665/0.0513 for 471 reflections. The structure of CsMnF 4 has been refined anew in the space group P4/n (Z = 4) as a merohedral (110) twin (lattice constants a = 794.40(6), c = 633.76(9) pm; R/wR = 0.051/0.044 for 820 reflections). All three structures derive from the T1A1F 4 type and show puckered [MnF 4 ] - layers with an antiferrodistortive order of strongly Jahn-Teller distorted [MnF 6 ] octahedra. The elongated axes (Mn-F for KMnF 4 : 215.8, RbMnF 4 215.2, CsMnF 4 216.8 pm) alternate with shorter ones (188.1,188.3,185.4 pm) within the layer planes. The terminal Mn-F bonds are very short (180.3, 180.6,181.7 pm). The Mn-F-Mn bridging angles are 140.6° and 146.4° for the K, 148.3° and 152.1° for the Rb, and 161.9° for the Cs compound. The magnetostructural relations and the three puckering types are discussed for all the AMnF 4 layered structures.

Open Access June 2, 2014

Kristallstruktur, thermische Zersetzung und Schwingungsspektrum von Ethylendiammonium-pentafluoromanganat(III), enH₂MnF₅ / Crystal Structure, Thermal Decomposition and Vibrational Spectrum of Ethylenediammonium-pentafluoromanganate(III), enH₂MnF₅

Ursula Bentrup, Ludger Schröder, Werner Massa

Page range: 789-794

More Download PDF

Abstract

Single crystals of enH 2 MnF 5 (en = ethylenediamine) have been prepared from aqueous HF solution and the crystal structure was determined by X-ray diffraction: space group Cccm, Z = 16, a = 1710.5(4), b = 1799.2(4), c = 847.8(2) pm, R/wR = 0.040/0.028 for 977 reflections. The structure consists of kinked [MnF 5]2- - chains built by MnF 6 octahedra sharing trans vertices (angles Mn-F-Mn 161.2 and 157.8°). The bridging Mn-F ax bonds are strongly elongated by the Jahn-Teller effect (mean Mn-F ax 215.4, Mn-F 183.8 pm). Each of the enH 2 2+ cations is connected to four anionic chains by hydrogen bonds forming a 3 D network. Thermal decomposition occurs between 200 and 380 °C in two steps giving finally MnF 2 . The IR spectra of enH 2 MnF 5 and its decomposition products are reported.

Open Access June 2, 2014

Silaheterocyclen, XVII / Silaheterocycles, XVII

Synthese und Cycloadditionsreaktionen neuartiger, aminocyclischer Silaethene [1] / Synthesis and Cycloaddition Reactions of Novel Amino Cyclic Silenes [1]

Norbert Auner, Erika Penzenstadler

Page range: 795-804

More Download PDF

Abstract

The silene 2 is formed by reacting 2-chloro-1,3-bis(trimethylsilyl)-2-vinyl-1,3-diaza-2-silacyclopentane (5) with LiBu t in n-pentane in the temperature range from -10 to +10°C. The reaction primarily leads to the corresponding a-lithio adduct 6 by addition of the Li-organyl to the vinyl group of 5; subsequent 1,2-LiCl elimination yields 2 as an intermediate. 2 can be trapped by polar reagents Me 3 SiX (X = OMe, OSO 2 CF 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 (β), with competitive [4+2] and [2+2] addition routes: While with butadienes and norborna-2,5-diene the [2+2] products are formed mainly in a multiple step reaction via zwitterionic intermediates (1,4 dipoles), the ratio of the [4+2]/[2+2] derivatives from 2 and cyclohexa-1,3-diene becomes nearly equivalent. 2 is thus quite comparable in its reactivity to dichloroneopentylsilene, Cl 2 Si = CHCH 2 Bu t .

Open Access June 2, 2014

Silaheterocyclen, XVIII Synthese und Cycloadditionsreaktionen C-silylmodifizierter aminocyclischer Silaethene [1] / Silaheterocycles, XVIII Synthesis and Cycloaddition Reactions of C-Silyl Modified Amino Cyclic Silenes [1]

Norbert Auner, Erika Penzenstadler

Page range: 805-813

More Download PDF

Abstract

The reaction of 2-chloro-1,3-bis(trimethylsilyl)-2-(1′-trimethylsilyl-ethenyl)-1,3-diaza-2-silacyclopentane (5) and LiBu leads to the α-lithio adduct 8 which can be trapped by Me 3 Sitriflate to give 13b, and is a useful silene precursor. Subsequent 1,2-LiCl elimination yields 2 as an intermediate, which does not cyclodimerise giving a 1,3-disilacyclobutane, but can be trapped by Me 3 SiOMe and suitable dienes which add across the Si=C bond. In contrast to silene 1, which favours the [2+2] addition, 2 exclusively forms the Diels-Alder isomers with 2-methyl-1,3-butadiene and 2,3-dimethyl-1,3-butadiene (6 and 7), and the ene products 11 and 12 with norborna-2,5-diene and cyclohexa-1,3-diene, respectively. This quite different cycloaddition behaviour results from the substitution pattern at the Si=C framework, with a changing polarity. 2 thus appears to be a rather electron deficient silene having a polarity more comparable to that of diorganosilenes rather than to 1, which may be compared in its reactivity with Cl 2 Si = CHCH 2 Bu.

Open Access June 2, 2014

Tetraphenylphosphonium-nonachlorodivanadat(III), (PPh₄)₃[V₂Cl₉] · 7 CH₂Cl₂ / Tetraphenylphosphonium Nonachlorodivanadate(III), (PPh₄)3[V₂Cl₉] · 7 CH₂Cl₂

Karin Ruhlandt-Senge, Alfred Dirk Bacher, Gertraude Koellner, Birgit Siewert, Ulrich Müller

Page range: 814-818

More Download PDF

Abstract

Reaction of VC1 4 with (Me 3 Si) 2 S in CH 2 C1 2 yields an insoluble product with the approximate composition VSC1 2 . Its reaction with PPh 4 Cl in CH 2 Cl 2 affords (PPh 4 ) 3 [V 2 Cl 9 ] · 7 CH 2 Cl 2 , whereas PPh 4 [VOCl 4 ] is formed in the presence of oxygen. According to an X-ray crystal structure analysis, (PPh 4 ) 3 [V 2 Cl 9 ] · 7 CH 2 Cl 2 contains [V 2 C1 9 ] 3- ions having two face-sharing coordination octahedra but no significant metal-metal bonding (V-V distance 327.5 pm). Crystal data: a = 1386.4(7), b = 1405.6(7), c = 2710(2) pm, α = 95.800(5), β = 95.370(5), γ = 118.11(3)°, triclinic, Ρ 1̄, Ζ = 2; R = 0.066 for 8779 observed reflexions. PPh 4 [VOCl 4 ] is isotypic with AsPh 4 [VOCl 4 ] and contains tetragonal-pyramidal [VOCl 4 ] - ions; tetragonal, P4/n, Z = 2, a = 1264.5(2), c = 772.0(2) pm; R = 0.050 for 654 observed reflexions.

Open Access June 2, 2014

Natrium-tetraethylammonium-tetrasulfid, Na⁺NEt₄⁺S₄²⁻. Synthese und Kristallstruktur / Sodium Tetraethylammonium Tetrasulfide, Na⁺NEt₄⁺S₄²⁻. Synthesis and Crystal Structure

Irina Sens, Alfred Dirk Bacher, Ulrich Müller

Page range: 819-822

More Download PDF

Abstract

NaNEt 4 S 4 was obtained from an equimolar solution of Na 2 S 4 and NEt 4 Cl 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, β = 105.8(3)°, space group P2 1 /n, Ζ = 4. In the structure, chains consisting of Na + and S 4 2− ions run in the a direction, every Na + being coordinated by four terminal S atoms of S 4 2− ions (two terminal, one chelating). The chains are separated by the NEt 4 + ions.

Open Access June 2, 2014

Molekülstrukturen von (o-Brombenzyl)diphenylphosphan und 1,3-Bis(diphenylphosphinomethyl)benzol / Molecular Structures of (o-Bromobenzyl)diphenylphosphine and 1,3-Bis(diphenylphosphinomethyl)benzene

Gerhard Müller, Joachim Lachmann, Jürgen Riede

Page range: 823-828

More Download PDF

Abstract

(o-Bromobenzyl)diphenylphosphine, 1, and 1,3-Bis(diphenylphosphinomethyl)benzene, 2, have conformations in the solid state with the phosphino groups being displaced noticeably from the plane of the central aromatic rings. The molecular structures allow conclusions about the chelating complexation capability of the ligands (o-diphenylphosphinomethyl)phenyl(-1) and 2,6-bis(diphenylphosphinomethyl)phenyl(-1) derived from 1 and 2 by metallation.

Open Access June 2, 2014

Synthesis, Spectroscopic and X-Ray Structural Characterization of [Cd(linpen)]²⁺, a Model for Metal Complexes of the Chelating Polymer Polyethyleneimine (linpen = Linear Pentaethylenehexamine)

Henry Strasdeit

Page range: 829-836

More Download PDF

Abstract

The isolation of 3,6,9,12-tetraazatetradecane-1,14-diamine (linear isomer of pentaethylenehexamine, linpen) from a technical polyamine mixture is described. In methanol, linpen acts as a hexadentate ligand towards cadmium(II). The solid compounds [Cd(linpen)](BPh 4 ) 2 (1), [Cd(linpen)](BPh 4 ) 2 •2 DMSO (2) and [Cd(linpen)](BF 4 ) 2 (3) have been isolated and characterized by elemental analysis, spectroscopy and X-ray powder diffraction. The 113 Cd NMR resonance of 1 is at 351 ppm (0.30 M in DMSO-d 6 , standard: 0.10 M Cd(ClO 4 ) 2 in D 2 O). 2 and 3 have been structurally characterized by single-crystal X-ray diffraction. 2: C 2/c; a = 19.337(1)Å, b = 17.937(1)Å, c = 18.584(1)Å, β = 111.54(1)°; Z = 4, R = 0.034, R w = 0.033.3: P2 1 /n; a = 8.607(1)Å, b = 14.851(2)Å, c = 15.703(2)Å, ß = 91.21(2)°; Z = 4,R = 0.083, R w = 0.072. Both compounds contain discrete [Cd(linpen)] 2+ complexes. The hexamine wraps around the metal ion in a helical manner. This results in a strong distortion of the coordination polyhedron. The mean Cd-N bond lengths are 2.38Å and 2.37Å for 2 and 3, respectively. Models for MN 6 centers in metal-polyethyleneimine (PEI) complexes are derived from the structure of [Cd(linpen)] 2+ . For example, loops at the MN 6 site in molecules of linear PEI are proposed.

Open Access June 2, 2014

Oxoporphyrins – The Molecular Structure of 5,15-Dioxo-2,3,7,8,12,13,17,18-octaethyl-porphodimethene-thallium(III) Chloride

Mathias O. Senge, Kevin M. Smith

Page range: 837-841

More Download PDF

Abstract

The crystal structure of the title compound was determined in order to obtain structural information on a tetrapyrrole bearing meso-oxo-functions. C 36 H 42 N 4 O2T1C1 · CH 3 OH, P1̄, a = 10.358(2), b = 12.344(3), c = 15.490(3) Å, a = 84.36(2)°, β = 78.53(2)°, γ = 82.26(2)°, V = 1918.2(7) Å 3 , Z = 2, 130 K, R = 0.04 for 6749 reflections with I > 4σ(Ι). The structure consists of the penta-coordinated thallium ligated by the four nitrogens of the porphodimethene ligand and a chloride in the axial position. The central macrocycle shows some degree of ruffling with the carbonyl groups pointing slightly above and below the mean plane of the molecule.

Open Access June 2, 2014

Zur Chemie der Proto-und allo-Proto-lichesterinsäure / Contribution to the Chemistry of Proto- and allo-Proto-lichesterinic Acids

Siegfried Huneck, Reiji Takeda

Page range: 842-854

More Download PDF

Abstract

The isolation and spectroscopic characterization of (-)-allo-proto-lichesterinic acid from Cetraria komarovii is described. Proto-lichesterinic and allo-proto-lichesterinic acids are transformed into numerous nitrogen-containing derivatives and the isomerization of the dihydro acids is investigated.

Open Access June 2, 2014

Tetrafluorcyclodi- und Hexafluorcyclotrisilazane / Tetrafluorocyclodi- and Hexafluorocyclotrisilazanes

Brigitte Tecklenburg, Uwe Klingebiel, Mathias Noltemeyer, Dieter Schmidt-Bäse

Page range: 855-860

More Download PDF

Abstract

Bis(silylamino)difluorosilanes (1,2) are prepared in the reaction of lithiated di-tert-butylmethyl- and tert-butyl-dimethylsilylamine with tetrafluorosilane. The dilithium derivative of 1 reacts with SiF 4 to give the tetrafluoro-substituted four-membered (Si-N) ring system [(CMe 3 ) 2 MeSiN-SiF2] 2 (3). Two four-membered rings [(RN-SiF 2 ) 2 (4), (RN-SiFNRSiF 3 ) 2 (5), R=CMe 3 SiMe2] are obtained in the reaction of dilithiated 2 with SiF 4 . The dilithiated silylamines and SiF 4 also react with formation of 3 and 4. However, besides 4 the six-membered ring (CMe 3 SiMe 2 N-SiF 2 ) 3 (6) is obtained. Crystal structures of 3,5, and 6 were determined. A transannular Si ··· Si ring distance of 237,5 pm is found in 3.

Open Access June 2, 2014

Synthesis and Structural Elucidation of the Acetylation Reaction’s Product(s) of the 2(1H)-Quinoxalinones Derived from L-Ascorbic Acid. X-Ray Molecular Structure of 3-(N-acetyl-2-naphthylhydrazono)-2,3-dihydro-2-acetoxyfuro[2,3-b]quinoxaline [1]

Adel Amer, Douglas M. Ho

Page range: 861-868

More Download PDF

Abstract

Acetylation reaction’s product(s) of 3-[L-threo-2,3,4-trihydroxy-1-(2-naphthylhydrazono)-butyl]quinoxalin-2(1H)-one (2b) were found to be dependent on the reaction condition. While the tri-O-acetyl (3b) was isolated in high yield from 2b under the action of acetic anhydride/pyridine mixture, compounds 4b and 5b as well as trace of 3b were obtained when 2b was heated in acetic anhydride. On the other hand, 3-[1-(2-naphthylhydrazono)-glyoxal-1-yl]quinoxalin-2(1H)-one (7) underwent ring closure and afforded the condensed tricyclic compound 8 under the action of acetic anhydride/pyridine mixture.

Open Access June 2, 2014

Polymeric [N-Lithio-benzimidazole(DMSO)₂]∞ The Crystal Structure and ab initio Calculations

Christoph Lambert, Paul von Ragué Schleyer, M. Gary Newton, Peter Otto, Peter Schreiner

Page range: 869-876

More Download PDF

Abstract

That lithiated aromatic amines with more than one nitrogen atom can favor polymeric aggregates in the solid state is demonstrated by the single crystal X-ray diffraction structure of [N-lithio-benzimidazole(DMSO) 2 ] ∞ 4; ab initio calculations on model compounds and simple electrostatic models indicate that the preference of the polymeric structure over dimeric alternatives is due to resonance stabilization and to Coulomb attraction between alternating benzimidazole anions and lithium cations.

Open Access June 2, 2014

Conformational Analyses of Alkylated β-Cyclodextrins by NMR Spectroscopy

Wolfram Meier-Augenstein, Barend V. Burger, Hendrik S. C. Spies, Wina J. G. Burger

Page range: 877-886

More Download PDF

Abstract

β-Cyclodextrin was derivatized with 1-bromoalkanes of different chain lengths. The yield as well as the purity of the resulting cyclodextrin derivatives were improved by using solvent mixtures instead of pure solvents. The heptakis(2,6-di-O-alkyl)- and heptakis(2,3,6-tri-O-alkyl)-β-cyclodextrins were studied by means of NMR spectroscopy employing one-dimensional as well as two-dimensional NMR techniques. Analysis of the NMR data showed that only in completely derivatized β-cyclodextrins the cyclodextrin torus undergoes a conformational change. Best separation factors were found for the cyclodextrin derivative with the highest internal mobility as determined from the corresponding NT 1 -values, the validity of which was confirmed by NOE determinations. Therefore, 13 C relaxation times could be used as a measure of the efficiency and usefulness of a given cyclodextrin derivative as an enantioselective stationary phase.

Open Access June 2, 2014

2-(4-Toluenesulphonyl)-3-aryloxaziridines as Oxidizing Reagents for P(III) Compounds

Manuela Klein, Ivar Ugi

Page range: 887-890

More Download PDF

Abstract

The preparation of four 2-(4-toluenesulphonyl)-3-aryloxaziridines by oxidation of the corresponding imines by peracids is described. The relative oxidation rates of trimethyl phosphite by these oxaziridines are determined.

Open Access June 2, 2014

Synthesis and NMR Studies of Some Steroidal Isoxazoles

Sergio Giacopello, Mónica E. Deluca, Alicia M. Seldes

Page range: 891-897

More Download PDF

Abstract

A short synthesis of 17α-pregna-2,4-dien-[2,3-d]isoxazol-17β-ol (1) is described using mild reaction conditions and with a high overall yield. The equilibrium between keto-enolic forms has been studied by 1 H NMR methods. Complete assignments of all the resonances in the 1 H and 13 C NMR spectra of Danazol have been made using a variety of one and two-dimensional correlation methods. 13 C NMR spectra of all the intermediate and related model compounds were also assigned.

Open Access June 2, 2014

Notizen: 4,5-Ethylenedithio-1-selenole-3-thiole-2-one as Starting Material for the Preparation of New Tetrachalcogenafulvalenes

D. J. Lagouvardos, G. C. Papavassiliou

Page range: 898-900

More Download PDF

Abstract

Starting from 3-chloro-2-oxo-1,4-dithiane the title compound was prepared and characterized analytically and spectroscopically. It was used then for the preparation of some new tetrachalcogenafulvalenes (π-donor molecules).

Open Access June 2, 2014

Notizen: Ga_0,5V₂Se₄, eine neue gemischtvalente Verbindung mit Spinellstruktur / Ga_0,5V₂Se₄, a New Mixed Valence Compound with Spinel Structure

H. Haeuseler, W. Cordes

Page range: 901-902

More Download PDF

Abstract

The mixed valence compound Ga 0,5 V 2 Se 4 has been prepared and characterized by X-ray powder methods and infrared spectroscopy. The compound crystallizes in a spinel structure with 1:1 ordering on the tetrahedral sites. The lattice parameter of the cubic cell is a = 1013.8 pm.

Open Access June 2, 2014

Notizen: Einfache Synthese funktioneller Mono- und Di(t-butyl)borverbindungen / Facile Synthesis of Functional Mono- and Di(t-butyl)boron Compounds

Gerhard Müller, Joachim Lachmann

Page range: 903-903

More Download PDF

Abstract

The functional mono- and di(t-butyl)boron compounds t BuB(OMe) 2 and t Bu 2 Bu 2 BOMe are easily prepared in good yield by a one-pot synthesis from excess B(OMe) 3 and t-butyllithium in ether at -60 °C.

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)

> Information on submission process

Volume 47 Issue 6

Issue of Zeitschrift für Naturforschung B

Abstract

Zur Chemie der 4,6-Dioxo-1,3,5,2 λ3-triazaphosphinane. / On the Chemistry of 4,6-Dioxo-1,3,5,2 λ3-triazaphosphinanes.

Teil II. Darstellung von 4,6-Dioxo-1,3,5,2 λ3-triazaphosphinanen / Part II. Preparation of 4,6-Dioxo-1,3,5,2 λ3-triazaphosphinanes

Abstract

Neue Synthesen von Magnesiumhydrid / New Syntheses of Magnesium Hydride

Abstract

Complexes of (CF3)3B with Sterically Crowded Amines. Unexpected Side Products from the Trifluoromethylation of Cl2BN(t-Bu)(Bz). Crystal and Molecular Structures of (CF3)3BNH(CH2)6, HO(CF3)2BCH(Ph)NH(t-Bu)(Bz) and Ph(CF3)2BCHN(t-Bu)(Bz)

Abstract

Die Kristallstrukturen der Tetrafluoromanganate(III) AMnF4 (A = K, Rb, Cs) / The Crystal Structures of the Tetrafluoromanganates(III) AMnF4 (A = K, Rb, Cs)

Abstract

Kristallstruktur, thermische Zersetzung und Schwingungsspektrum von Ethylendiammonium-pentafluoromanganat(III), enH2MnF5 / Crystal Structure, Thermal Decomposition and Vibrational Spectrum of Ethylenediammonium-pentafluoromanganate(III), enH2MnF5

Abstract

Silaheterocyclen, XVII / Silaheterocycles, XVII

Synthese und Cycloadditionsreaktionen neuartiger, aminocyclischer Silaethene [1] / Synthesis and Cycloaddition Reactions of Novel Amino Cyclic Silenes [1]

Abstract

Silaheterocyclen, XVIII Synthese und Cycloadditionsreaktionen C-silylmodifizierter aminocyclischer Silaethene [1] / Silaheterocycles, XVIII Synthesis and Cycloaddition Reactions of C-Silyl Modified Amino Cyclic Silenes [1]

Abstract

Tetraphenylphosphonium-nonachlorodivanadat(III), (PPh4)3[V2Cl9] · 7 CH2Cl2 / Tetraphenylphosphonium Nonachlorodivanadate(III), (PPh4)3[V2Cl9] · 7 CH2Cl2

Abstract

Natrium-tetraethylammonium-tetrasulfid, Na+NEt4+S42−. Synthese und Kristallstruktur / Sodium Tetraethylammonium Tetrasulfide, Na+NEt4+S42−. Synthesis and Crystal Structure

Abstract

Molekülstrukturen von (o-Brombenzyl)diphenylphosphan und 1,3-Bis(diphenylphosphinomethyl)benzol / Molecular Structures of (o-Bromobenzyl)diphenylphosphine and 1,3-Bis(diphenylphosphinomethyl)benzene

Abstract

Synthesis, Spectroscopic and X-Ray Structural Characterization of [Cd(linpen)]2+, a Model for Metal Complexes of the Chelating Polymer Polyethyleneimine (linpen = Linear Pentaethylenehexamine)

Abstract

Oxoporphyrins – The Molecular Structure of 5,15-Dioxo-2,3,7,8,12,13,17,18-octaethyl-porphodimethene-thallium(III) Chloride

Abstract

Zur Chemie der Proto-und allo-Proto-lichesterinsäure / Contribution to the Chemistry of Proto- and allo-Proto-lichesterinic Acids

Abstract

Tetrafluorcyclodi- und Hexafluorcyclotrisilazane / Tetrafluorocyclodi- and Hexafluorocyclotrisilazanes

Abstract

Synthesis and Structural Elucidation of the Acetylation Reaction’s Product(s) of the 2(1H)-Quinoxalinones Derived from L-Ascorbic Acid. X-Ray Molecular Structure of 3-(N-acetyl-2-naphthylhydrazono)-2,3-dihydro-2-acetoxyfuro[2,3-b]quinoxaline [1]

Abstract

Polymeric [N-Lithio-benzimidazole(DMSO)2]∞ The Crystal Structure and ab initio Calculations

Abstract

Conformational Analyses of Alkylated β-Cyclodextrins by NMR Spectroscopy

Abstract

2-(4-Toluenesulphonyl)-3-aryloxaziridines as Oxidizing Reagents for P(III) Compounds

Abstract

Synthesis and NMR Studies of Some Steroidal Isoxazoles

Abstract

Notizen: 4,5-Ethylenedithio-1-selenole-3-thiole-2-one as Starting Material for the Preparation of New Tetrachalcogenafulvalenes

Abstract

Notizen: Ga0,5V2Se4, eine neue gemischtvalente Verbindung mit Spinellstruktur / Ga0,5V2Se4, a New Mixed Valence Compound with Spinel Structure

Abstract

Notizen: Einfache Synthese funktioneller Mono- und Di(t-butyl)borverbindungen / Facile Synthesis of Functional Mono- and Di(t-butyl)boron Compounds

Abstract

Zur Chemie der 4,6-Dioxo-1,3,5,2 λ³-triazaphosphinane. / On the Chemistry of 4,6-Dioxo-1,3,5,2 λ³-triazaphosphinanes.

Teil II. Darstellung von 4,6-Dioxo-1,3,5,2 λ³-triazaphosphinanen / Part II. Preparation of 4,6-Dioxo-1,3,5,2 λ³-triazaphosphinanes

Complexes of (CF₃)₃B with Sterically Crowded Amines. Unexpected Side Products from the Trifluoromethylation of Cl₂BN(t-Bu)(Bz). Crystal and Molecular Structures of (CF₃)₃BNH(CH₂)₆, HO(CF₃)₂BCH(Ph)NH(t-Bu)(Bz) and Ph(CF₃)₂BCHN(t-Bu)(Bz)

Die Kristallstrukturen der Tetrafluoromanganate(III) AMnF₄ (A = K, Rb, Cs) / The Crystal Structures of the Tetrafluoromanganates(III) AMnF₄ (A = K, Rb, Cs)

Kristallstruktur, thermische Zersetzung und Schwingungsspektrum von Ethylendiammonium-pentafluoromanganat(III), enH₂MnF₅ / Crystal Structure, Thermal Decomposition and Vibrational Spectrum of Ethylenediammonium-pentafluoromanganate(III), enH₂MnF₅

Tetraphenylphosphonium-nonachlorodivanadat(III), (PPh₄)₃[V₂Cl₉] · 7 CH₂Cl₂ / Tetraphenylphosphonium Nonachlorodivanadate(III), (PPh₄)3[V₂Cl₉] · 7 CH₂Cl₂

Natrium-tetraethylammonium-tetrasulfid, Na⁺NEt₄⁺S₄²⁻. Synthese und Kristallstruktur / Sodium Tetraethylammonium Tetrasulfide, Na⁺NEt₄⁺S₄²⁻. Synthesis and Crystal Structure

Synthesis, Spectroscopic and X-Ray Structural Characterization of [Cd(linpen)]²⁺, a Model for Metal Complexes of the Chelating Polymer Polyethyleneimine (linpen = Linear Pentaethylenehexamine)

Polymeric [N-Lithio-benzimidazole(DMSO)₂]∞ The Crystal Structure and ab initio Calculations

Notizen: Ga_0,5V₂Se₄, eine neue gemischtvalente Verbindung mit Spinellstruktur / Ga_0,5V₂Se₄, a New Mixed Valence Compound with Spinel Structure