bluuebunny/crossref_metadata_2025 huggingface dataset:
Notizen: Bis(trimethylsilylhydrazido)-thiophosphorsäurephenylester – ein neues Zwischenprodukt für die Synthese anorganischer Heterocyclen / Bis(trimethylsilylhydrazido)-thiophosphoric Acid Phenylester - A New Intermediate for the Synthesis of Inorganic Heterocycles
Authors: Steger Lothar , Engelhardt Udo
Published: March 2015

The title compound,

C6H5O-(S)P[NH-NH-Si(CH3)3]2 (1), m. p. 37-39°C, is prepared by silylation of the parent dihydrazide with (CH3)3SiCl in the presence of an excess of base. 1 is purified by vacuum destillation and characterized by 1 H NMR, IR, Ra, mass spectra and analysis. Phosphorus hydrazine heterocycles, such as cis- and trans-C6H5O-(S)P(NH-NH)2P(X)-OC6H5 (X = S, O) and others can be prepared from 1 and C6H5O-(X)PCl2 or other element dihalogene compounds.
Notizen: Contributions to the Chemistry of Mo and W, XVII.
Authors: Schröder F. A.
Published: March 2015

The results of a bond order/bond distance relationship have been applied upon the known structure of Mo-O and Mo-S double bridge compounds. Mo-Ot bonds neighboring to Mo-S bridges are always about 0.03 Å longer than expected, indicating a π-bonding contribution in these bridges in contrary to the Mo-O double bridges.
Notizen: Selektive katalytische Hydrierung von 1.3-Cyclohexadien zu Cyclohexen mit dem Katalysator-System NiCl2 plus NaBH4 in Dimethylformamid / Selective Catalytic Hydrogenation of 1,3-Cyclohexadiene to Cyclohexene with the Catalyst System NiCl2 plus NaBH4 in Dimethylformamide
Authors: Strohmeier Walter , Steigerwald Hannelore
Published: March 2015

With a catalyst, prepared by reaction of NiCl2 with NaBH4 in dimethylformamide, 1,3-cyclohexadiene is selectively hydrogenated to cyclohexene without formation of cyclohexane.
Notizen: Dialkylindiummono- und Alkylindiumdihalogenide R2InX und RInX2 (mit R = CH3, C2H5 und X = Cl, Br, J), IV Alkylierungsreaktionen mit Dialkylindiumchloriden / Dialkyl Indium Mono- and Alkyl Indium Dihalides R2InX and RInX2 (with R = CH3,C2H5 and X = Cl, Br, J), IV Alkylation Reactions with Dialkyl Indium Chlorides
Authors: Widler H. J. , Hausen H.-D. , Weidlein J.
Published: March 2015

Dimethyl indium chloride alkylates SbCl5, (CH3)3SbCl2 and (CH3)3AsCl2 forming ionic tetramethylstibonium and tetramethylarsonium derivatives such as [(CH3)4Sb]+ [SbCl6]-, [(CH3)4Sb]+ [CH3InCl3]- and [(CH3)4As]+ [CH3InCl3]-. The vibrational spectra are discussed.
Notizen: 13C NMR Spectra of Alkyl Substituted Pyrylium Salts
Authors: Balaban A. T. , Wray V.
Published: March 2015

The 13C chemical shifts of several alkylsubstituted pyrylium salts are presented. Charge densities in the isoelectronic series benzene, pyridine, pyridinium cation and pyrylium cation, calculated from INDO M. O. theory, are shown to correlate well with the ring carbon 13C chemical shifts. The effect of alkyl substitution on ring carbon 13C chemical shifts in the pyrylium salts are shown to correlate with those of the alkyl benzenes.
High Pressure Reactions in the Systems Zn3As2—As and Cd3As2—As
Authors: Clark J. B. , Range Klaus-Jürgen
Published: March 2015

ZnAs2 and CdAs2 decompose at high pressure and temperature. The determined decomposition boundaries are presented. From synthesis experiments in the systems Cd3As2—As and Zn3As2—As, the decomposition products were found to be mixtures of CdAs + As and ZnAs + As. The high pressure phases CdAs and ZnAs are orthorhombic, space group D15
2h — Pbca, with αo = 5.993 A, bo = 7.819 A, co = 8.010 Å and αo = 5.679 A, bo = 7.277 A, co = 7.559 Å, respectively. Further phases are recovered from the high temperature region at high pressure.
Assignment of cis-trans Geometry in Diastereomeric 2-Benzyl-4-methyl-1,3,2-dioxaphosphorinans and their 2-Oxo- and 2-Seleno-Derivatives
Authors: Stec W. J. , Lesiak K. , Mielczarek D. , Stec B.
Published: March 2015

MICHAELIS-ARBUSOV reaction of diastereoisomeric 2-methoxy-4-methyl-1,3,2-dioxaphosphorinans with benzyl halides is non-stereospecific. Cis- and trans-2-benzyl-2-oxo-4-methyl-1,3,2-dioxaphosphorinans were separated and analysed by means of IR, 31P and 13C NMR spectroscopy. 2-Benzyl-2-seleno-4-methyl-1,3,2-dioxaphosphorinans were synthesized and stereospecifically converted to 2-oxo-analogues. Stereochemistries are assigned to the geometrical isomers of all new compounds described in this paper. Application of direct spin-spin coupling constant values for structural elucidation is emphasized.
Reaktionen von Metallcarbonylen mit Diazirin / Reactions of Metal Carbonyls with Diazirine
Authors: Beck Wolfgang , Danzer Wolfgang
Published: March 2015

Pentamethylendiazirine (N͡=N) has been found in metal carbonyl compounds as a monodentate two electron ligand (π-CH3C5Η4Mn(CO)2 N͡=N, (OC)5W N͡=N) or as a bidentate four electron ligand ((OC4M (N͡=N)2M(CO)4 (M = Mo, W), (OC)4Fe N͡=N Fe(CO)4). The reaction of Fe2(CO9 with diazirine affords the isocyanate and/or methylenamino-bridged complexes (OC)3Fe(NCO) (N=C< )Fe(CO)3 and (OC)3Fe (N=C< )2Fe(CO)3.
Untersuchungen an Stickstoff-Jod-Verbindungen, XV Neue Addukte des Stickstofftrijodids mit tertiären N-Basen-Chinuclidiniumpentajodid (Chin H)J3 · J2, ein neues Polyjodid / Studies on Nitrogen-Iodine Compounds, XV New Adducts of Nitrogen Triiodide with Tertiary N-Bases-Chinuclidiniumpentaiodide (Chin H)I3 · I2, a New Polyiodide
Authors: Jander Jochen , Pritzkow Hans , Trommsdorff Klaus-Uwe
Published: March 2015

New adducts of nitrogen triiodide with several tertiary N-bases have been prepared. Their analyses, general properties, IR-spectra and structures are reported briefly. Experiments to crystallize a compound with a ratio N : I : chinuclidin = 1 : 4 : 1 resulted in the preparation of cristallized chinuclidiniumpentaiodide (chin H)I3 • I2, the X-ray structure analysis of which is reported.
13C-NMR-Spektroskopie an polycyclischen Aromaten, II. Die 13C-NMR-Spektren von 1- und 2-Fluornaphthalin. Überprüfung der Signalzuordnung und Untersuchung der Substituenteneffekte auf die chemischen Verschiebungen / 13C NMR Spectroscopy of Polycyclic Aromatics, II. The 13C NMR Spectra of 1- and 2-Fluoronaphthalene. Reexamination of Signal Assignments and Investigation of Substituent Effects on Chemical Shifts
Authors: Ernst Ludger
Published: March 2015

During a reinvestigation of the 13C NMR spectra of 1-fluoronaphthalene (1) and of 2-fluoronaphthalene (2) at 20 and 25.16 MHz, uncertainties that existed in the literature about signal assignments for 1 could be cleared. In the spectral analyses for 2 given so far, five out of ten signals were incorrectly assigned. The corrected assignment is supported by extensive 13C{1H} double resonance experiments, by recording of proton-coupled 13C and 13C{19F} spectra and by off-resonance 13C{1H} noise-decoupling. The results show a strong + M-effect of the fluorine substituents on 13C chemical shifts similar to the effects of OH and OCH3 groups. 1H NMR spectra of 1 and 2 could be partially assigned by decoupling of the 19F resonances and by iterative analysis.
Die photoinduzierte Carbonylierung von Di(π-cyclopentadienyl)-dimethyl-titan und Di(π-indenyl)-dimethyl-titan / The Photo-induced Carbonylation of Di(π-cyclopentadienyl)-dimethyl-titanium and Di(π-indenyl)-dimethyl-titanium
Authors: Alt Helmut G. , Rausch Marvin D.
Published: March 2015

The photo-induced carbonylation of (C5H5)2(CH3)2Ti and (C9H7)2(CH3)2Ti in pentane solution results in a cleavage of the methyl-metal bonds, and the formation of the corresponding carbonyl titanium complexes.
Notizen: Selektive Hydrierung von 1.3- und 1.5-Cyclooctadien mit dem Katalysatorsystem NiCl2+ NaBH4 in Dimethylformamid / Selective Hydrogenation of 1,3- and 1,5-Cyclooctadiene with Catalyst-System NiCl2 + NaBH4 in Dimethylformamide
Authors: Strohmeier Walter , Steigerwald Hannelore
Published: March 2015

With the catalyst-system NiCl2 · 6 H2O and NaBH4 dissolved in dimethylformamide 1.3- and 1.5-cyclooctadiene are selectively hydrogenated to cyclooctene under mild conditions.
Notizen: Umsetzung von Δ 4-Steroidketonen mit dem Dihalogencarbenreagens der Phasentransfer-Katalyse / Conversion of Δ 4-Steroidketones with the Dihalocarbene Reagent of Phase Transfer Catalysis
Authors: Dehmlow Eckehard V. , Ezimora Gordian C.
Published: March 2015

Chloroform/concentrated aqueous NaOH/catalyst transform testosterone acetate (1) into a mixture of the α- and β-stereoisomers of dichlorocyclopropyl derivatives (2) and tetrachlorospiropentane derivates (3). 2 are the precursors of 3. Formation of analog chloro as well as bromo derivatives of cholestenone was demonstrated.
The Electronic Structure of Organometallic Complexes Involving f-Electrons, II Magnetic Susceptibility and Crystal Field Splitting of Uranium(IV)-tetracyclopentadienide
Authors: Amberger H.-D. , Fischer R. D. , Kanellakopulos B.
Published: March 2015

Some significant features of the low-energy part of the crystal field (=CF) splitting pattern of the organometallic 5f2-system (η5-C5H5)4U(IV) can be deduced from the temperature dependence of the magnetic susceptibility which has been measured on polycrystalline samples between 1.1 and 298 K. The results of model calculations performed independently on the basis of three different semi-empirical approaches are compatible with the deductions from the experiments and allow estimates of the sign and order of magnitude of quantities like the CF-splitting parameters B4
0 and B6
0 viz. the (averaged) angular overlap parameters eσ and eπ„ and of the valence state ionisation potential of the 5f-electrons. Anticipating a rather weakly perturbed tetrahedral CF, the observed magnetic properties may be satisfactorily simulated if the six lowest-lying first-order CF-states and one common scaling factor are accounted for
1H- und C-NMR-Spektren von Methoxy-substituierten Äthylenen / 1H and 13C NMR Spectra of Methoxy-substituted Ethylenes
Authors: Herberhold M. , Wiedersatz G. O. , Kreiter C. G.
Published: March 2015

The charge distribution in the methoxy -substituted olefins of the series ethylene, methyl vinyl ether, 1,1-dimethoxyethylene, cis- and trans-dimethoxyethylene, tetramethoxyethylene, is discussed on the basis of the 1H and 13C NMR spectra
Bleidioxidverbundelektroden für die Elektrosynthese, I Abscheidung von β-Bleidioxid auf Titan / Leaddioxide Electrodes for Electrosynthesis, I Deposition of β-Leaddioxide on Titanium
Authors: Wabner Dietrich W. , Fritz Heinz P. , Missol Detlef , Huss Rainer , Hindelang Fritz
Published: March 2015

Noble metal electrodes do not stand the tests for anodic electro syntheses in technical applications. Mainly due to the high oxygen overvoltage lead dioxide can act as substitute. A novel process for the preparation of lead dioxide coated titanium anodes is described. The important procedure is a treatment of the clean titanium surface with a Ti(IV)-containing solution. By scanning electron microscopy it is established that three dimensional nucleation takes place. Lead dioxide anodes prepared following this process until now have livetimes of better than 3400 hours
Umsetzung von P[P(O)(OC2H5)2]3 mit Aminen. Darstellung von [(C2H5O)2(O)P-P-P(O)(OC2H5)2] [H2NR2] / Reaction of P[P(O)(OC2H5)2]3 with Amines. Preparation of [(C2H5O)2(O)P-Ρ-P(O)(OC2H5)2][H2NR2]
Authors: Weber Dieter , Heckmann Gernot , Fluck Ekkehard
Published: March 2015

By the reaction of tris(diethylphosphoryl)phosphine with amines compounds of type 1 are obtained, the structure of which is discussed by NMR and X-ray photoelectron spectra. Some chemical and physical properties are described
Vergleich der Amino- und Hydroxy-Nachbargruppe bei Dehydrierungen.
Authors: Möhrle H. , Kamper Chr. , Feil R.
Published: March 2015

The mercuric EDTA dehydrogenation of the isomeric 1,2- and 2,1-(phenyl-pyrrolidino)-ethanols yields with two electron removal the corresponding oxazolidines. The analogous 1,2- and 2,1-(amino-phenyl)pyrrolidines by double dehydrogenation produce the amidines resp. by subsequent hydrolysis the lactams. An explanation for the different course of the reaction is given
Chemical Constitution and Activity of Bipyridylium Herbicides, X1 3-Substituted-6,7-dihydrodipyrido[1,2-a: 2′,1′-c]-pyrazinediium Dibromides and Related Compounds
Authors: Pirzada Nasim H. , Pojer Peter M. , Summers Lindsay A.
Published: March 2015

The synthesis of 3-substituted-6,7-dihydrodipyrido-[1,2-α:2′,1′-c]-pyrazinediium dibromides is described. The 3-alkoxy and 3-carbomethoxy derivatives can be regarded as reversible one electron transfer systems. The most active compound is the 3-methoxy derivative which is a very effective post-emergent herbicide at 1-2 kg/hectare
Isolation of Flaviolin from the Potato Culture Solution of Phoma wasabiae Yokogi
Authors: Soga Osamu
Published: March 2015

Flaviolin was found in the blackish potato culture solution of Phoma wasabiae
Sulfonylierungs- und Aminierungsreaktionen von Sulfonsäureaziden.
Authors: Kreher Richard , Jäger Gerhard
Published: March 2015

The reaction of aromatic and aliphatic sulfonic azides with benzene under the influence of aluminiumchloride has been examined. The intermolecular substitution reactions - sulfonylation, amination and alkylation - are dependent from the structural effect of the corresponding substituent
Reaktionen von 1-Phenyl-3-alkoxycarbonyl-triazenen mit Lewis-Säuren in Benzol. / Reactions of 1-Phenyl-3-alkoxycarbonyl-triazenes with Lewis Acids in Benzene
Authors: Kreher Richard , Goth Kurt
Published: March 2015

1-Phenyl-3-alkoxycarbonyl-triazenes react with aluminiumchloride in benzene by elimination of nitrogen, especially to alkylbenzenes and diphenyl; anilin is formed with practical constant yield, independently of the alkyl group. On the basis of these experimental results during the reaction of alkoxycarbonyl azides with benzene under the influence of Lewis acids triazenes are not formed as intermediates
Notizen: Die Phase Mg2,5Ni11.5P7 / The Phase Mg2,5Ni11,5P7
Authors: Mewis Albrecht
Published: March 2015

By investigations in the system Mg-Ni-P we found the phase Mg2,5Ni11.5P7, which crystallizes in a hexagonal lattice
Bindungsverhältnisse in Berlinerblau-Analoga des Typs Fe[MB(CN)6] / Chemical Bonding in Prussian Blue Analogs of the Type Fe[MB(CN)e]
Authors: Inoub H. , Fluck E. , Yanagisawa S.
Published: March 2015

All three compounds of the type Fe[MB(CN)6] (MB = Co, Rh and Ir) crystallize in the face-centered cubic system: space group Fm3m (Oh5), Z = 4. The lattice constants increase in the order Fe[Co(CN)6] (10.16 ± 0.01 A) < Fe[Rh(CN)6] (10.42 ± 0.01 A) < Fe[Ir(CN)6] (10.43 ± 0.01 A). The infrared spectra showed four absorption bands which are assigned to the normal vibrations: VCN-, VMB_C', υMB-CN and υFe-N• The observation of Fe-N stretching bands substantiates the existence of chemical bonding between iron and nitrogen atoms of the cyanide ligands. The intensive absorption bands around 26,5 kK are assignable to the charge transfer between Fe(III) and [MB(CN)6]3- groups, while the absorption bands in the UV region are assigned to the ligand field transitions of the [MB(CN)6]3~ moiety. The Mössbauer spectra gave a single absorption line with a relatively small isomer shift, which is explained in terms of the formation of σ-bonding between Fe-N.
Elektrochemische Synthesen, V. Die anodische α-Hydroxylierung von Isobutyraldehyd / Electrochemical Syntheses, V. The Anodic α-Hydroxylation of Isobutyraldehyde
Authors: Becker Bernhard F. , Fritz Heinz P.
Published: March 2015

The electrolysis of isobutyraldehyde in the presence of water in alkaline methanol leads to α-hydroxy-isobutyraldehyde-dimethylacetal (1). The reaction probably occurs via the oxidation of the base conjugate to isobutyraldehyde to the carbenium ion and the subsequent nucleophilic addition of hydroxyl ion present in the electrolyte.
Diborylverbindungen als Liganden in Metallkomplexen, III Synthese und Struktur von Bis(2.5-dimethyl-3.4-diäthyl-1.2.5-thiadiborolen)-nickel(0) / Diboryl Compounds as Ligands in Metal Complexes, III Synthesis and Structure of Bis(2,5-dimethyl-3,4-diethyl-1,2,5-thiadiborolene)-nickel(0)
Authors: Siebert Walter , Full Roland , Krueger Carl , Tsay Yi-Hung
Published: March 2015

2,5-Dimethyl-3,4-diethyl-1,2,5-thiadiborolene (1) and Ni(CO)4 yield yellow 1 • Ni(CO)2, which is converted to the corresponding bis( 1,2,5-thiadiborolene)-nickel(0), the first thermostable thioborane nickel complex. Spectroscopic data indicate a pentahapto sandwich compound with the electron-donating groups in approximately tetrahedral arrangement. This is confirmed by X-ray structural analysis. The title compound crystallizes in the space group p21/c with α = 19.594(2), b = 11.8593(4), c = 9.3736(3) Å, β = 102.848(6)° and four molecules per unit cell.
Notizen: Nitroxylradikal-Metallkomplexe / Nitroxyl Radical Metal Complexes
Authors: Weissgerber Rudolf , Schwarzhans Karl E.
Published: March 2015

A series of complexes formed between metal ions and the stable free radicals 3-carboxy-2,2,5,5-tetramethylpyrroline-1-oxyl, 3-carboxy-2,2,5,5-tetramethylpyrrolidine-1-oxyl, 4-amino-2,2,6,6-tetramethylpiperidine-1-oxyl and glyoxal-bis(2,2,6,6-tetramethyl-4-iminopiperidine-1-oxyl) has been prepared. The magnetic moments and the EPR spectra of the complexes and the free ligands have been investigated. Some of the complexes show a temperature dependent interaction between the radicalic groups of the ligands.
Markierte Verbindungen, XXII1 1.2.3.3-Tetrachlor-(1.3-14C)-1-propen mit unsymmetrischer 14C-Verteilung / On Labelled Compounds, XXII l,2,3,3-Tetrachloro-(1,3-14C)-1-propene with Unsymmetrical Distribution of 14C
Authors: Boberg Friedrich , Voss Rainer
Published: March 2015

Starting with (14C)chloroform 1,2,3,3-tetrachloro-(1,3-14C)-1-propene (7 z) with unsymmetrical distribution of 14C is synthesized according reaction scheme 1. 7 z is isomerized with AlCl3 to 1,2,3,3-tetrachloro-(1,3-14C)-1-propene (7 t) with symmetrical distribution of 14C. From 7 z and 7 t the dichloro-(14C)acetanilides (13 z) and (13 t) are formed via the dichloro-(14C) acetic acids. The distribution of 14C on C-1 (75%) and C-3 (25%) from 7 z follows from comparison of the activities of 13 z, 13 t with 7 z.
Notizen: Binding and Kinetics of 1-Methylimidazol on Fe(III)-Protoporphyrin(IX)dimethylester and Fe(III)-Tetraphenylporphyrin in Chloroform
Authors: Goldammer Eberhard V. , Zorn Herbert
Published: March 2015

Nuclear magnetic line widths data have been used to determine the rate of solvent exchange between the coordination sphere of Fe(III)-protoporphyrin(IX)dimethylester or Fe(III)-tetraphenylporphyrin and the bulk phase of 1-methylimidazol/chloroform. At temperatures below 322 K both porphyrins are in the low-spin state and separate PMR absorption caused by the methyl protons of two 1-methylimidazol molecules complexed in fifth and sixth position of ferri-porphyrins is detected. At T ≳ 320 K an accelerated exchange of these ligands was observed and the underlying kinetic parameters have been extracted. It was found that this exchange takes place when the paramagnetic species is in its low-spin state. For 240 K ≲ T ≲ 290 K dynamic line broadening of bulk phase 1-methylimidazol indicates occurrence of chemical exchange attributed to 1-methylimidazol interacting with ferri-porphyrin in addition to the strongly bound axial ligands.
Notizen: Die Kristallstruktur des Mauritins-A / The Crystal Structure of Mauritine-A
Authors: Kibfel A. , Will G. , Tschesche R. , Wilhelm H.
Published: March 2015

The constitution and conformation of the known cyclopeptide alkaloid mauritine-A were determined by X-ray diffraction methods. All amino acids belong to the L-series, 3-hydroxy proline has trans-configuration. As indicated by the UV-spectrum, the 14-membered ring system is considerably strained.
Darstellung und Charakterisierung von Halogeniden und Pseudohalogeniden des Typs π-C7-Μ(CO)2Χ (M = Mo, W; X = Br-, Cl-, NCO-, NCS-, N3
-).
Authors: Hoch Gerhard , Panter Rainer , L. Manfred
Published: March 2015

Halides and pseudohalides of formula π-C7H7M(CO)2X were synthesized by reaction of [π-C7H7M(CO)3][BF4] and π-C7H7M(CO)2Br, with NaX or KX (M = Mo, X = OCN-, SON-, N3-; M = W, X = Cl-, Br-, OCN-, N3-). In the OCN- and SCN- complexes the ligands are coordinated by the nitrogen atoms. The reaction of [π-C7H7W(CO)3][BF4] with KOCN yielded (besides π-C7H7W(CO)2NCO) a compound which proved to be the mono-tricarbonyl-tungsten derivative of bicycloheptatrienyl (C7H7)2W(CO)3. This compound could also be isolated from [π-C7H7W(CO)3][BF4] and Na[NCNH]. Ring contraction occurred when [π-C7H7W(CO)3][BF4] was treated with Na2[NCN].
Die Röntgenstrukturanalyse von (CO)9Co3CΟΒΒr2Ν(C5)3. X-ray Structure Analysis of (CO)9Co3COBBr2N(C2H5)3
Authors: Bätzel Volker
Published: March 2015

Using three dimensional X-ray data collected on a four circle diffractometer, the structure of (CO)9Co3COBBr2N(C2H5)3 was solved by Patterson and Fourier methods. Least squares refinement with a block-diagonal matrix leads to a reliability index of R = 10.7%. Crystal data: α = 13.277(6) Å, b = 10.17(1) Å, c = 9.22(2) Å; α = 91.12(6)°, β = 87.61(4)°, γ = 98.79(2)°; space group P1̅; Z = 2; V = 1229,7 Å3; Dx = 1.97 gcm-3.
The Axial Preference of Fluorine Atom in 2-Fluoro-4-methyl-1,3,2-dioxaphosphorinanyl Ring System
Authors: Okruszek A. , Stec W. J.
Published: March 2015

The axial preference of fluorine substituent at phosphorus involved in 4-methyl-1,3,2-dioxaphosphorinanyl ring system was established.

Cis-trans geometry in this family of compounds was assigned by chemical correlation and by means of 1H, 13C, 19F and 31P NMR.
Zur Chemie des Tellurophens.
Authors: Müller Eugen , Luppold Ernst , Winter Werner
Published: March 2015

Electrophilic substitution of 2,5-diphenyltellurophene (1) affords 2,5-diphenyl-3,4-chloromethyl-tellurophene (2). The reaction of 2 with nucleophilic reagents leads to the tetrasubstituted derivates (3-6). Oxidation of 5 with seleniumdioxide affords 2,5-diphenyltellurophene-3,4-dicarbaldehyde (7).
Notizen: Electron-radiolysis of Diphenylpicrylhydrazyl in Tetranitromethane. Evidence for a Free Radical Nitration Process
Authors: Filby W. G. , Kalus W. H.
Published: March 2015

Isolation, Diphenylpicrylhydrazyl

Products and yields for the electron radiolytical decomposition of DPPH in tetranitro methane have been determined. Reaction occurs via attack of NO2 radicals, the dinitro adduct being the main product at the lowest doses investigated.
Die Kristallstruktur zweier Modifikationen des Bis(1.2-benzochinondioximato)-platinjodids.
Authors: Pritzkow H.
Published: March 2015

Bis(1,2-benzoquinonedioximato)-platinum iodide crystallizes in two modifications. Both consist of centrosymmetric Pt(BCD)2I2 molecules, which are held together by intermolecular hydrogen bonds.
Raman- und IR-Spektren von festen Alkali-Polysulfiden.
Authors: Hermann Eysel Hans , Wieghardt Gertraud , Kleinschmager H. , Weddigen G.
Published: March 2015

The Raman, IR and FIR spectra of polycrystalline samples of the polysulfides Na2S4, K2S5, Na2S5 have been measured. A unique assignment of the internal vibrations of the tetrasulfide ion could be achieved.
Elektronenübertragungsreaktionen, I Produktanalysen der Einelektronen-Oxidation von Olefinen mit Ferriin oder Bleidioxid in wäßriger und methanolischer Lösung/ Electron Transfer Reactions, I Product Analyses of One-Electron Oxidations of Olefins by Ferriin or Lead Dioxide in Aqueous and Methanolic Solutions
Authors: Frühauf Hans-Werner , Koerner Von Gustorf Ernst A.
Published: March 2015

The oxidation of the substituted ethylenes, 2,3-dimethylbutene-2 (1), 2-methylbutene-2 (8), and α-methylstyrene (18), by ferriin or lead dioxide in water and/or methanol has been studied. Product analyses of the reactions, which lead to kinetically controlled product distributions, showed that lead dioxide, just as ferriin, reacts as a one-electron-oxidant. The product distributions, which arise from further reactions of the primary intermediates, i. e. the radical cations formed via one-electron transfer, were found to depend on substituents, acidity and solvent. The results are consistent with three separate reaction paths of the radical cation, each of which leads to specific products. The radical cation can either deprotonate, be nucleophilicly attacked by solvent, or lead to dimeric products. The first two possibilities only are observed in the oxidation of 1 and 8, while only the latter two are found in the oxidation of 18.
Darstellung und Oxidation von Mangan(II)-Komplexen mit L-Cystein und Dipeptiden als Liganden.
Authors: Guntner Hans , Schwarzhans Karle.
Published: March 2015

Complexes formed between manganese(II) and the ligands Gly-Tyr, Gly-Phe, Ala-Ala, Tyr, cysteine and cystine have been prepared. The IR, EPR spectra and the magnetic moments of the compounds have been collected. Oxidation of the dipeptide complexes in solution leads to manganese(III) species.
A Reinvestigation of the Reaction of Salicylideneaniline with Potassium Cyanide
Authors: Harhash Abdel Hamid , El-Bannani Afaf Abdel Aziz
Published: March 2015

Treatment of salicylidene-anils with potassium cyanide in acetic acid affords 1:1 adducts shown to be the hydrocyano derivatives. When the reaction is conducted in alcohol, salicylidene derivatives of 2-amino-3-arylaminobenzofurans or α-arylamino-o-hydroxyphenylacetamides are formed depending on the molar ratio of the reactants. The formation of the products and the previously reported structures are discussed.
Notizen: Darstellung und Kristallstruktur des Sr2Si / Preparation and Crystal Structure of Sr2Si
Authors: Widera Axel , Eisenmann Brigitte , Schäfer Herbert
Published: March 2015

Single crystals of Sr2Si have been prepared. From a complete X-ray structure determination follows the anti-PbCl2 structure type.
Characterization of Tetrakis(isonitrile)platinum(II)-tetrachloroplatinates(II), [Pt(CNR)4] [Pta4]
Authors: Keller H. J. , Lorentz R.
Published: March 2015

Coordination compounds of unusual color and stoichiometry PtCl2(CNR)2 are identified by experimental evidence as ionic tetrakis(isonitrile)platinum(II)tetrachloroplatinates(II). The synthesis of several new complexes [Pt(CNR)4][PtCl4] with varying R and of “mixed” compounds [Pt(CNR)2(CNR')2][PtCl4] is described. The influence of the isonitrile ligands in these complexes is discussed especially concerning the resulting solid state properties.
Notizen: Zur Reaktion von En-diolen mit Halogendisilanen.
Authors: Hengge E. , Brandstätter E.
Published: March 2015

Alkalistilbenolate does not react, as expected, with dichlorotetramethyldisilane (1) to a six-membered heterocyclic, but the SiSi linkage is nucleophilic attacked by the oxygen and a five-membered heterocycle with only one Si-atom is formed. On the other hand, 1,2-dihydroxybenzene reacts with 1 to the new six-membered heterocycle in good yield.
Darstellung, Struktur und Eigenschaften von N-Alkyliminoalanen / Preparation, Structure and Properties of N-Alkyliminoalanes
Authors: Nöth H. , Wolfgardt P.
Published: March 2015

The N-alkyliminoalanes [tert-C4H9NAIH]4, [tert-C4H9NAID]4, [iso-C3H7NAIH]6, [C2H5NAlH]8 and [CH3NAIH]n have been prepared and intermediates such as Al3H3(N tert-C4H9)2(N tert-NHC4H9)2 and Al8H10(NC2H5)6(NHC2H5)2 isolated. Cage structures and opened cages respectively are suggested on the basis of physical data.

Halogenation of these iminoalanes by HgX2 proceeds in a complicated manner, the products depending on the mole ratio used, the size of the alkylgroup and cage. HX formation during the halogenation is indicated by the formation of [Cl2AlNHR]2. Regioselectivity was observed for partial chlorination of [C2H5NAlH]8. Pyrolysis of [RNHAIHCl]2 yields [tert-C4H9NAlCl]4 and [iso-C3H7NAlCl]4.
Synthese, Basenaddition und Fragmentierung der 1.3.2-Dioxaborolan-4-one / Synthesis, Addition of Bases, and Fragmentation of 1,3,2-Dioxaborolane-4-ones
Authors: Paetzold Peter , Bohm Peter , Richter Anette , Scholl Ernst
Published: March 2015

2,5,5-Triorgano-1,3,2-dioxaborolane-4-ones RB(—O—CO—CXY—O—) (2-6) can be prepared from α-hydroxycarboxylic acids XYC(OH)—COOH and dihalogenoorganoboranes RBHal2. They are much weaker Lewis acids than the 2-organo-1,3,2-dioxaborolane-4,5-diones RB(—O—CO—CO—O—) (1). The compounds 1 give 1:1 adducts with the bases DINO, MANO, PyO, and PSy, respectively; the crystal structure determination of 1f · DINO reveals a simple BO-coordination between the components. On electron impact, the chief fragmentation path is the elimination of CO2 from compounds 1-6. The thermal degradation of 2-6 seems to be rather complicated in the liquid phase but is unique in the gaseous phase forming the compounds (RBO)3, CO, and XYC=O.
Komplexone, XLVII Die Thermodynamik der Komplexbildung von einigen ein- und zweiwertigen Metallionen mit Aethylendiamintetraacetat- und Uramildiacetat-Ion / Complexone, XLVII Thermodynamics of Complex Formation of Some Univalent and Bivalent Metal Ions with Ethylenediaminetetraacetate and Uramildiacetate Anions
Authors: Anderegg G.
Published: March 2015

The enthalpies of complex formation of EDTA and uramildiacetate (UDA) with univalent cations (H+, Li+, Na+, K+, Ag+ and Tl+) have been obtained by direct calorimetric measurements at ionic strength 0.1 (or 1) and 20°C. For comparison data for the formation of 1:1 UDA complexes with Mg2+, Ca2+, Ba2+ and Sr2+ have also been obtained. From these values and the stability constants the thermodynamic functions ΔG and ΔS are calculated. The results are compared with those of similar systems.
Synthesis of Low Melting Liquid Crystalline N-(4-n-Alkylbenzilidene)-4′ -n-alkylanilines
Authors: Osman Maged A.
Published: March 2015

The synthesis of a number of dialkylbenzilidene anilines is described. Mesomorphic phases are found at or below room temperature. An efficient method for the preparation of the 4-n-alkylanilines and their benzilidene derivatives is described.
Untersuchung der cis-trans-Isomerie des WITTIGschen Kohlenwasserstoffs / Investigation of the cis-trans-Isomerism of the WITTIG Hydrocarbon
Authors: Sartorius Rolf , Schmidt Reinhard , Kelm Hartwig , Brauer Hans-Dieter
Published: March 2015

The cis-trans-isomerism of the WITTIG hydrocarbon was investigated in solid state and solution by means of fluorescence spectroscopy. The fluorescence behavior of both isomers in 2-methyltetrahydrofurane was determined as a function of concentration, temperature, and wavelength of exciting radiation. Furthermore, irradiation experiments were undertaken with light of various wavelengths.

The results obtained are in agreement with the assumption that the WITTIG hydrocarbon behaves with regard to the cis-trans-isomerism like a 1,3-butadien derivative, i.e. a thermal but no photochemical cis-trans-isomerisation can be detected. The enthalpy difference between the two isomers was estimated to ΔΗ = 250 ± 50 cal/mole. It could be shown that the fluorescence of the cis-isomer is quenched by the trans-isomer. This quenching occurs probably according to the resonance energy transfer mechanism.
Reactions of tert-Butylperoxy Esters. XV. Decomposition of Dialkyl tert-Butylperoxy Phosphates
Authors: Sosnovsky G. , Zaret E. H.
Published: March 2015

The thermal decomposition of dialkyl tert-butylperoxy phosphates, in the presence and absence of solvents, yields the corresponding dialkyl phosphate, acetone, methanol, 2,2-dimethoxypropane, and methyl isopropenyl ether as the primary products. Prolonged heating of the product mixture produces trialkyl phosphates, (RO)3P(O), which arise from the thermal decomposition of dialkyl phosphates. Data are presented to support a mechanism involving the heterolytic cleavage of the peroxide linkage.
Radiation Chemistry of Carbohydrates, Vlll. γ-Radiolysis of Cellobiose in N2O-saturated Aqueous Solution. Part II. Quantitative Measurements. Mechanisms of the Radical-induced Scission of the Glycosidic Linkage
Authors: Von Sonntag Clemens , Dizdaroglu Miral , Schulte-Frohlinde Dietrich
Published: March 2015

The γ-radiolysis of cellobiose (10-2 M) in N2O saturated aqueous solution has been investigated and the G-values of the following 21 products containing six or less C-atoms have been measured (G-values in parentheses): glucose (2.1), gluconic acid (0.70), 4-ketoglucose (0.07), 5-keto-glucose (0.05), 4-deoxy-glucose (0.27), 5-deoxy-gluconic acid (0.18), 2-deoxy-gluconic acid (0.13), 3-deoxy-4-keto-glucose (0.23), 2-deoxy-5-keto-glucose (0.34), 4-deoxy-5-keto-glucose (0.14), 6-deoxy-5-keto-glucose (0.02), arabinose (0.07), ribose (0.015), 2-deoxy-ribose (0.17), 3-deoxy-pentulose (0.01), erythrose (0.015), threose (0.015), 2-deoxy-tetrose (0.01), butanone-(2)-diol(1.4) (0.01), dihydroxyacetone (0.01), carbon monoxide ( > 0.02).

The formation of the major part (98%) of the measured products could be explained on the base of the following assumption: The first step of reaction sequence is abstraction of H atoms from C-Η bonds of the cellobiose by OH radicals. Radicals at C-1′, C-5′ and C-4 and their successors undergo in a second step four types of reactions: hydrolysis, rearrangement and H2O and CO elimination. In a third step the transformed radicals give rise to products by disproportionation reaction. Only two products out of 16 predicted under the above assumption are not observed. G-values for the attack at C-1′, C-5′ and C-4 are 1.4, 0.6 and 0.3 respectively.
Mechanismen der elektronenstoßinduzierten Methanoleliminierung aus ortho- und para-substituierten Benzoesäuremethylestern / Mechanisms of Electron Impact Induced Elimination of Methanol from ortho- and para-Substituted Benzoic Acid Methyl Ester
Authors: Herrmann Rupert , Schwarz Helmut
Published: March 2015

Using deuterium labelled compounds the mechanisms of methyl as well as methanol elimination from the title compounds have been established. It can be shown that in the case of 4-methoxy-methyl benzoic acid methyl ester the unusual methanol elimination from the [M-methyl]+ ion probably proceeds via the formation of a π-complex and a ring expansion reaction. In addition to this novel fragmentation some ortho-effects and other fragmentation reactions useful for an analytical identification of the ortho/para-isomers by means of mass spectrometry are discussed.
Notizen: Darstellung sulfamoyl-substituierter Silazane.
Authors: Appel Rolf , Montenarh Mathias
Published: March 2015

Diorganyldichlorosilanes (2 a, b) react with the disilylated sulfamides (1 a, b) to give the cyclodisilazanes (3a-c), however with the monosilylated sulfamide (4) the silazanes of type 5 are formed. Reaction of 1 a with bis-(dimethylchlorosilyl) sulfurdiimide (6) affords the cyclic compound (7).
Notizen: Synthesis of Trimethylphosphazenyl- and Triphenylphosphazenyl-fluorocyclotriphosphaza-trienes by a Silylation Method
Authors: Du Plessis Jan A. K. , Rose Hans , Shaw Robert A.
Published: March 2015

The synthesis of trimethylphosphazenyland triphenylphosphazenyl-fluorocyclotri-phosphazatrienes, N3P3F6-n(NPR3)n, by a silylation method using Me3SiNPR3 (R = Me or Ph) is reported. More phosphazenyl groups can be introduced if R = Me than if R = Ph. Isomers have been isolated, as have been mixed phosphazenyl derivatives,

N3P3Fe6-n-m(NPR3)n(NPR3′)m

(R = Ph, R′ = Me). Substituted fluorophosphazenes,

N3P3F6-nXn (X = Ph, NMe2, or OPh) also undergo similar reactions.
Notizen: Elektrochemische Synthesen, IX. Elektrochemisch initiierte Oligomerisierung von tert-Butylisonitril.
Authors: Bockmair G. , Fritz H. P. , Köhler F. H.
Published: March 2015

The electrochemical (catalytical) oxidation of tent-butylisocyanide yields the dimer, trimer and higher oligomers.
Notizen: Photolyse und Thermolyse von 2-(α-Diazo-benzyl)-pyridin-1-oxid / Photolysis and Thermolysis of 2- (α-Diazo-benzyl) -pyridine-1-oxide
Authors: Güsten Hans , Ullman Edwin F.
Published: March 2015

Direct and sensitized photolysis of 2-(a- diazo-benzyl)-pyridine-1-oxide (2) as well as its thermolysis in deoxygenated solvents resulted 2-benzoylpyridine (3) in nearly quantitative yield. As a geometrical consequence of the intramolecular abstraction of oxygen from the N→O group by the triplet carbene (1) the formation of an oxazetine intermediate (4) is discussed.
Notizen: Protonierung und Alkylierung von Olefin-cyano-dicarbonyl-ferraten(0).
Authors: Behrens Helmut , Moll Matthias , Würstl Peter
Published: March 2015

The anionic complexes [olenFe(CO)2CN]- (olen = butadiene, 1,3-cyclohexadiene, cyclooctatetraene), formed by the reaction of olenFe(CO)3 with NaN[Si(CH3)3]2, have been protonated to the isocyanic acid derivates olenFe(CO)2CNH, and alkylated with [Et3O]BF4 to give the isonitrile complexes olenFe(CO)2CNEt.
Derivatives of cis-NPCl2 (NSOCl)2 and (NPCl2)2NSOCl, IV
Isothiocyanato Derivatives of cis-NPCl2(NSOF)2
Authors: Klei E. , Grampel J. C. van de
Published: March 2015

The compounds NPClNCS(NSOF)2 and NP(NCS)2(NSOF)2 are prepared by reaction of cis-NPCl2(NSOF)2 with KSCN. The mono(isothiocyanato) derivative obtained is a colourless liquid, consisting of two isomers in a ratio of 1:3.8; the bis(isothiocyanato) compound is a white crystalline solid.
Zur Umsetzung von Trichloracetimidsäuremethylester mit Antimon(V)-chlorid.
Authors: Rössler Manfred , Schmidt Armin
Published: March 2015

Trichloroacetimidicacidmethylester reacts with antimony(V) chloride to yield the 1-trichloromethyl-1-methoxi-methylenimonium-hexachloroantimonate(V) (1). 1 eliminates methylchloride and gives the 1:1-adduct (3) of trichloroacetamide and antimony(V) chloride. The vibrational spectra of 1 and 3 are communicated.
Antipodentrennung eines unsymmetrisch substituierten Triarylphosphins.
Authors: Luckenbach Reiner
Published: March 2015

The separation of an unsymmetrically substituted triarylphosphine, phenyl-m-carboxyphenyl-p-biphenylyl-phosphine (1), into its enantiomers is reported.
Notizen: 13C-NMR an paramagnetischen Phenylmetallocenen1: Analogie zum Benzylradikal.
Authors: Köhler Frank H. , Matsubayashi G.
Published: March 2015

The 13C NMR spectra of seven phenylated paramagnetic metallocenes have been recorded. From the spectra the 13C hyperfine coupling constants A(13C) have been extracted and compared with corresponding A(1H). It is found that the phenyl A′s in nickelocenes and cobaltocenes behave as in benzyl radical being reduced by a factor of 27. This offers a new route to informations about spin density distribution in substituted methyl radicals.
Notizen: Kristall- und Molekülstruktur von 4-Jod-2′.4′.6′-trimethylbiphenyl.
Authors: Häfelinger Günter , Strähle Joachim
Published: March 2015

The space group of 4-iodo-2′,4′,6′-trimethylbiphenyl was determined by means of an automatic single crystal diffractometer as P 21/c with 4 molecules in the unit cell and the molecular structure was refined to a R-value of 3.3%. The angle of twist between the two best planes of the phenylrings is 84 ± 1°.
Die Struktur von Ph-P[C5H5(CO)2MnFe2(CO)6]. Ein Komplex mit einem verbrückenden μ3-Ph-P-Liganden.
Authors: Huttner G. , Frank A. , Mohr G.
Published: March 2015

The title compound, which may be prepared from C5H5(CO)2Mn—P(Ph)Cl2 and Fe2(CO)9 crystallizes in the monoclinic space group C 2/c with a = 1579(2), b = 1592(2), c = 1790(3) pm, β = 97.2(1)°, Z = 8. The structure was solved by direct methods. Full matrix refinement led to R1= 0.066. The compound contains a threemembered metallocycle with two iron and one manganes atoms. Each iron atom bears three terminal carbonyl groups; the two CO-ligands of the C5H5Mn(CO)2 fragment form unsymmetrical bridges with the two iron atoms. The metal triangel is capped by a Ph—P group with a triply bridging phosphorus atom.
Darstellung und Trennung der Isomeren des Natrium-bis(L-aspartato)chromat(III).
Authors: Grouhi-Witte Gisela , Weiss Erwin
Published: March 2015

Sodium bis(L-aspartato)chromate(III), a complex with L-aspartic acid as tridentate ligand, has been prepared by reaction of chromium(III)chloride, L-aspartic acid and sodium hydroxid. Infrared, electronic absorption and circular dichroism spectra of three isolated isomers have been measured.
Substituentenaustausch bei tetrameren N-Alkylimino-alanen / Exchange of Substituents in Tetrameric N-Alkylimino-alanes
Authors: Nöth H. , Wolfgardt P.
Published: March 2015

The exchange of H versus D between [HAlNC(CH3)3]4 and [DAlNC(CH3)3]4 leads to an equilibrium mixture of H4-nDn [AlNC(CH3)3]4 with statistical distribution of H and D. This is, as expected, not the case for the H/Cl-distribution achieved between [HAlNC(CH3)3]4 and [ClAlNCH(CH3)2]4. Although a series H6-nCln[AlNCH(CH3)2]6 can be detected besides H4-nCln[AlNCH(CH3)2]4 and H4-nCln[AlNC(CH3)3]4 the absence of alkyl group exchange proves that the redistribution of Al-substituents occurs without transfer of XAlNR units by an exopolyhedral exchange mechanism involving pentacoordinate aluminium.
Radiation Chemistry of Carbohydrates, IX γ-Radiolysis of N-Acetyl-glucosamine in Aqueous Solution
Authors: Bradbury Allan G. W. , Sonntag Clemens von
Published: March 2015

The γ-radiolysis of N-acetyl-glucosamine in deoxygenated (N2O saturated) and oxygenated (N2O/O2 saturated) solutions has been investigated. Eleven products have been characterised and their G-values estimated.

Deoxygenated conditions: The principal products identified are 1-acetamido-1,3-dideoxy-2-pentulose (4), 1-acetamido-1-deoxy-2-pentulose (5), 2-acetamido-2,3-dideoxyhexos-4-ulose (6), 2-acetamido-2-deoxy-hexodialdose (7), 2-acetamido-2-deoxy-hexos-5-ulose (8) and 2-acetamido-2-deoxy-gluconic acid (9). Products 1 to 3 contain 3-5 carbon atoms (acetamido group eliminated). Their yields are low.

Oxygenated conditions: G values of 5, 7, 8 and 9 are increased, whereas compounds containing a deoxy-keto group (4 and 6) are absent. C-C-bond scission is more important in the presence of oxygen. 2-Acetamido-2-deoxy-tetrodialdose (10) has been identified and a number of products with 5 carbon atoms in the chain retaining the acetamido group (11) have been recognised.

Mechanisms for the formation of products are proposed.
Notizen: (i-C37HNH3
+)8(Cl-)4[SbCl6]3-[SbCl6]- eine neue mixed valence-Verbindung.
Authors: Birke G. , Latscha H. P. , Pritzkow H.
Published: March 2015

The reaction between isopropylamine and isopropylammonium hexachloroantimonate(V) yields a red product of the composition C12H40Cl8N4Sb. The X-ray structure analysis showed that this is a mixed valence compound of SbCl6
3- and SbCl6
- octahedra.
Notizen: Zur Kenntnis und Struktur des Tetrathioperrhenat-Ions in (C5H6)4P[ReS4].
Authors: Diemann Ekkehard , Müller Achim
Published: March 2015

Tetraphenylphosphonium tetrathiorhenate(VII) is shown to be isostructural with tetraphenylarsonium tetrachloroferrate(III) and by means of radial distribution analysis the average metal ligand distance was estimated as d(ReS) = 2.155(30) Å.
Notizen: Synthesis and Crystal Structure of the Hydrogen Bonded Complex of Tri-paratoluidylphosphazenyl Oxide with Ethyl Alcohol
Authors: Cameron T. Stanley , Magee M. Gerard , Mclean Samuel
Published: March 2015

The title compound was synthesised and its structure determined by X-ray crystallography. The structure contains a hydrogen bond between the OH group of the alcohol and the phosphoryl oxygen atom. The P–N bond lengths are significantly different and the differences can be attributed to varying ρπ—dπ interactions along the bonds.
Notizen: Thienoquinolines, II. A New and Convenient Synthesis of Thieno(2,3-b)quinoline
Authors: Shanmugam P. , Kanakarajan K. , Soundararajan N.
Published: March 2015

A new and convenient synthesis of thieno-(2,3-b)quinoline starting from methyl-3-vinylquinolin-2(1H)-one-4-carboxylate is described.
Darstellung, Eigenschaften und Struktur von Bis(biscyclopentadienyltitan(III))-bis(dodekahydronido-dekaborato)zinkat, [(η-C5H5)2Ti · OC4H8 · OC3H6]2[Zn(Β10Η12)2] · OC4H8.
Authors: Allmann Rudolf , Bätzel Volker , Pfeil Reinhard , Schmid Günter
Published: March 2015

Reaction between (η-C5H5)2TiCl and Zn(B10H12) in tetrahydrofurane leads to a green, paramagnetic [(η-C5H5)2Ti · OC4H8 · OC3H6]2[Zn(B10H12)2] · OC4H8 whose structure was solved by statistical and Fourier methods.
Neue ternäre Telluride und Selenide der Alkalimetalle mit Elementen der 3. Hauptgruppe.
Authors: Weis Jürgen , Schäfer Herbert , Schön Günter
Published: March 2015

The new ternary compounds NaAlSe2, NaAlTe2, NaGaTe2 and KAlTe2 crystallize in the TlITlIIISe2-structure type. The analogous Tl-compounds build up the same structure but show a variable composition within the limits (NaxTl1-x)TlSe2 (0 < x < 0.47) and (KxTl1-x)TlSe2 (0 < x < 0.56). The compounds KAlSe2, KGaSe2, KInSe2 and KGaTe2 crystallize in a new structure type.
E. Radiation Chemistry of Diphenylpicrylhydrazyl (DPPH), IV. The Mass Spectra of Some Aromatic Hydrazines. Comparison of Radiolytic and Photolytic Fragmentations
Authors: Filby W. G. , Kalus W. H.
Published: March 2015

The mass spectra of some aryl hydrazines under electron impact are reported. In every case studied fragmentation occurs via fission of the weak hydrazyl N—N bond and hydrogen migration. Metastable ion data is presented in support of a proposed mechanism and some comparisons made between electron and radiation induced processes.
Preparation of N,N,N′,N′-Bis(ethylene)-phosphorodiamidates of Steroids, Diacetone-D-glucose, and α-Tocopherol
Authors: Sosnovsky G. , Konieczny M.
Published: March 2015

The phosphorodichloridates (1) of cholesterol, β-sitosterol, testosterone, diacetone-D-glucose, and tocopherol were prepared from phosphorus oxychloride in the presence of triethylamine. Tocopheryl phosphorodichloridate was too unstable to be isolated. Reaction of 1 with ethyleneimine in the presence of triethylamine gave the corresponding Ν,Ν,Ν′,N′-bis(ethylene)-phosphorodiamidates (2).
Notizen: Zur Existenz des CrO3J--Ions.
Authors: Königer-Ahlborn E. , Müller A.
Published: March 2015

The preparation, infrared and electronic spectra of the salts [(C6H5)4A]CrO3J (A = As, P) are reported and discussed.
Fluorreiche Oxofluorovanadate(V): Die Kristallstruktur von [enH2][VOF5]. / Fluorine-Rich Oxofluorovanadates(V): Crystal Structure of [enH2][VOF5]
Authors: Rieskamp Helmut , Mattes Rainer
Published: March 2015

The crystal structure of triclinic [enH2][VOF5], prepared in aqueous solution, has been determined from X-ray diffractometer data (R = 0.076 for 527 reflections). The structure contains monomeric [VOF5]2--ions. The bond distances are 1.54(1) Å (terminal oxygen), 1.80(1) (average for the cis-fluorine atoms) and 2.10(1) Å for the fluorine atom in transposition to the terminal oxygen atom. This fluorine atom is involved in strong hydrogen bonds originating from the [NH3CH2CH2NH3]
2+ cation with cisoid conformation. Earlier results about the existence of K2VOF5 could not be confirmed
Crystallographic Data for the High-Pressure Phases CsClO4 IV and CsBF4 IV
Authors: Richter P. W. , Whalley E. , Pistorius C. W. F. T.
Published: March 2015

The high-pressure phases CsClO4 IV and CsBF4 IV have been quenched to atmospheric pressure at 100°K. The powder patterns can be indexed on the basis of tetragonal cells with a0 = 12.965, 12.728 Å, c0 = 5.230, 5.126 Å, respectively, containing eight formula weights. The cell volumes are in excellent agreement with the values expected from direct measurements of the III (barite)/IV transition volume changes. Arguments are advanced to show that these high-pressure phases, slightly more densely packed than the scheelite structure, probably contain the large cations in eightfold sites, the smaller ones in tetrahedral sites, and have cation-cation coordination numbers of approximately eight
Zur Kenntnis der interatomaren Abstände des statistisch orientierten CrO3F--Ions in Kaliumfluorochromat(VI). / Interatomic Distances of the Statistically Oriented CrO3F- Ion in Potassium Fluorochromate(VI)
Authors: Diemann E.
Published: March 2015

Since the O/F sites in KCrO3F are statistically occupied by both ligands only average metal ligand distances can be obtained by the usual single crystal structure determination. Fourier transformation of the reduced intensity distribution of the crystalline powder, however, yields the radial distribution function in which all interatomic vectors are put into a one-dimensional common scale with the same origin. From an analysis of this function the distances d(CrO) = 1.615(20) and d(CrF) = 1.78(3) Å were obtained. By the same technique also KCrO3Cl and Na3CrO4 were investigated resulting in d(CrO) = 1.617(20) and d(CrCl) = 2.183(35) for the former and d(CrO) = 1.70(2) Å for the latter compound