bluuebunny/crossref_metadata_2025 huggingface dataset:
Das Tricarbonyl-eisen-cycloheptatrienid-Anion [C7H7Fe(CO)3]–: η3-Allylanion- oder η4-Butadienkomplex? / The Triearbonyl Iron Cyeloheptatrienide Anion: η3-Allyl Anion or η4-Butadiene Complex?
Authors: Hofmann Peter
Published: February 2015

Molecular orbital calculations for [C7H7Fe(CO)3]-predict a η3 -allyl anion Fe(CO)3 complex with un-coordinated diene part of the C7H7 ligand to be more stable than the alter-native η4 -butadiene Fe(CO)3 form, the cyclopolyenyl ligand being nonplanar in either case. The tiny energy difference between both coordination modes accounts for the observed high fluxionality of the anion.
Die Strukturen der Phasen Na9Sn4 und Na15Sn4 / The Structures of the Phases Na9Sn4 and Na15Sn4
Authors: Midler Wiking , Volk Klaus
Published: February 2015

The crystal structures of Na9Sn4 and Na15Sn4 have been determined. Na9Sn4 crystallizes orthorhombic, a=542 ±1, b = 939 ±2, c = 2962 ± 6 pm, isotypic with LigGe4. Na15Sn4 crystallizes cubic, a = 1314 ± 2 pm, isotypic with Na15Pb4 (Cu15Si4-type). The structural relationship of Na9Sn4 to the variants of the W-Structure type is shown.
Die Alkoholyse von 3.5-Difluor-1.1.3.5-tetraoxo-2-alkyl-1λ6.3λ6.5λ6.2.4.6- trithiatriazin / The Alcoholysis Reaction of 3,5-Difluoro-l,l,3,5-tetraoxo-2-alkyl-1λ6,3λ6,5λ6,2,4,6-trithiatriazin
Authors: Wagner Diec-Lang , Wagner Hartmut , Glemser Oskar
Published: February 2015

(NSOF)2(CH3NSO2) 2a reacts with methanol to give sulfuric acid, aminosulfuric acid and SO2(NHCH3)2 as final products. The primary reaction was studied by 1H and 19F NMR spectroscopy. A 1:1 adduct 2a · CH3OH (=3) and a monosubstituted product which has the formula (NSOF)(NSOOCH3)(CH3NSO2)4 were detected to be intermediates.

As 2 a is chiral, the reaction with racemic butanol-2 proceeds via diastereomeric inter-mediates which were identified by their 19F NMR spectrum.

The reaction pattern of 2a is explained.
Eigenschaften von Molekülen in angeregten Zuständen / Properties of Molecules in Excited States
Authors: Fabian Walter
Published: February 2015

Using bisisochinolin derivatives and related compounds it is shown that information about the fluorescent state can be obtained by comparison of experimental fluorescence data and calculated energies of the Si-state assuming various geometries.
Die Kristallstruktur yon RbGeCl3 / The Crystal Structure of RbGeCl3
Authors: Messer Dieter
Published: February 2015

RbGeCl3 is prepared from RbCl and Ge(II) in 6 N HCl or by reaction of RbCl with HGeCl3. The compound crystallizes monoclinic, space group P21/m, with a = 798.8, b = 694.1, c = 580.0 pm, β = 106.34° and Z = 2. The crystal structure has been determined by SHELX and refined till R = 0.067. RbGeCl3 is built up by Rb+ and pyramidal GeCl3−-units. The coordination of Ge and the anionic framework is discussed.
Molekulare Reaktionen in kalten Methan-Wasser-Plasmen und die Wirkung von UV-Bestrahlung / Molecular Reactions in Cold Methane-Water Plasma and the Effect of UV Irradiation
Authors: Simionescu Cr. , Dumitriu S. , Bulacovschi V. , Popa V. I. , Simionescu B.
Published: February 2015

After passage of methane-water mixtures through the state of a cold plasma, numerous products were identified, especially aldehydes, ketones, alcohols and acids. Their concentration was dependent on the methane/water ratio. Irradiation with UV light during or after the process gave transformations of the above compounds to more complex combinations. For the formation of ketones, aldehydes, alcohols and acids a detailed mechanism is proposed.
Synthesis and Mesomorphic Properties of Diphenyl- and Biphenylyl-pyrimidines
Authors: Boiler Arthur , Cereghetti Marco , Scherrer Hanspeter
Published: February 2015

The synthesis and mesomorphic properties of four classes of cyano-substituted diphenyl -and biphenylyl-pyrimidines are reported. The new compounds are colourless, chemically and photochemically stable and have wide mesomorphic ranges. The synthesis of one member of each homologous series is described in detail.
The Nature of Zolon Red
Authors: Qureshi A. M. , Patel A. N.
Published: February 2015

Zolon red is an acid dye obtained in the enol form as the stable condensation product of glutaconic aldehyde with two molecules of 1-phenyl-3-methylpyrazol-5-one. Silver(l) replaces the hydroxylhydrogen of the dye to give deep blue precipitate of silver-zolon red compound.
Ringschlußversuche mit Phenylborsäure / Attempts for Synthesis of Inorganic Rings with Phenylboric Acid
Authors: Wannagat Ulrich , Eisele Gerd
Published: February 2015

The inorganic ring systems BNCO2Si2 (B) and BCO3Si4 (E) were prepared for the first time via equations (1) and (5), system BCO3Si2 (C) enlarged by preparation of compound C 1 via eq. (4). Synthesis of a system BCO2Si2 (D) failed as well as preparation of five and seven membered building units VI and VIII. For bis(trimethylsiloxy)phenylborane (IX) detailed and additional information about preparation, properties and structure analysis is given. Compound VTI, C5H15NOSi, was obtained for the first time via eq. (7) and described in its properties.
Die Kristallstruktur des dimeren Dimethylantimontrichlorids und des Tetramethylantimon-hexachloroantimonats [(CH3)2SbCl3]2 und [(CH3)4Sb] + [SbCl6]- / Crystal Structure of the Dimeric Dimethylantimony Trichloride and Tetramethylantimony Hexachloroantimonate [(CH3)2SbCl3]2 and [(CH3)4Sb]+[SbCl6]-
Authors: Schwarz Wolfgang , Guder Hans-Jürgen
Published: February 2015

Dimethylstibonium trichloride (CH3)2SbCl3 exists in two isomeric forms. In the dimeric "covalent" one, [(CH3)2SbCl3]2, two formula units are bridged by chlorine, building a fourmembered ring. It crystallizes in the orthorhombic space group Pnma with lattice constants a = 1212.9, b = 1910 and c = 610.2 pm. The mean value of bond length from antimony to the terminal chlorine atoms is 235.5 pm, to the bridging chlorine atoms 280.0 pm and the averaged Sb-C distance is 213.3 pm.

The second form [(CH3)4Sb]+[SbCl6]- is an ionic one and crystallizes in the triclinic space group P1̅ with lattice constants a = 715.6, b = 744.2, c = 1415.2 pm, a = 90.01, β = 93.39 and γ = 106.4°. The mean values of bond lengths are Sb-C 211.5 pm and Sb-Cl 238.2 pm. The tetrahedrical as well as the octahedrical coordination polyhedra are only slightly distorted.
Synthesis of Chiral and Non-chiral Phosphites Containing the Hexafluoroisopropoxy Group
Authors: Dakternieks Dainis , Röschenthaler Gerd-Volker , Schmutzler Reinhard
Published: February 2015

A series of new phosphorus (III) compounds containing the hexafluoroisopropoxide group has been synthesised by reacting halophosphines with lithium hexafluoroisopropoxide. The phosphites ButPX[OCH(CF3)2] (where X = F, Cl), ButMeP[OCH(CF3)2] and C6H5PF[OCH(CF3)2] each contain a chiral center at phosphorus.
14N-NMR-Untersuchungen an Aminophosphinen / 14N NMR Studies on Aminophosphines
Authors: Barlos K. , Nöth H. , Wrackmeyer B.
Published: February 2015

14N chemical shifts of a series of cyclic and noncyclic aminophosphines are reported. The nuclear shielding of nitrogen decreases with increasing number of halogen substituents at phosphorus as well as with increasing number of phosphinyl groups attached to nitrogen. In addition to the influence of electronegativity PN(π)-interactions may account for the observed shielding. Steric effects are discussed.
Substitution und Ringkopplung am Cyclotrisilazan-System / Substitution and Ring Coupling at the Cyclotrisilazane System
Authors: Enterling Detlev , Klingebiel Uwe , Melier Anton
Published: February 2015

Fluorosilanes, chlorodiorganylboranes and chlorotrimethylstannane react with lithiated cyclotrisilazanes under LiF elimination and substitution. Mixed substituted compounds are obtained by the reaction of lithio-fluorosilyl-cyclotrisilazanes with other fluorosilanes. Ring coupling is achieved by the reaction of lithio-hexamethylcyclotrisilazane with 2-chloro-1,3,4,5,6-pentamethylborazine. The reaction of a fluoro(methylamino)silylsubstituted cyclotrisilazane with butyllithium leads to a system consisting of two hexamethyleyclotrisilazanes connected through a diazadisilacyclobutane ring.
Die Reaktion eines gemischten Doppelylids mit Ethylenoxid / Reaction of a Mixed Double Ylide with Ethylene Oxide
Authors: Schmidbaur Hubert , Holl Peter
Published: February 2015

Dimethyl-trimethylphosphinimino-methylene-phosphorane, (CH3)3P=N-P(CH3)2 = CH2 was found to react with ethylene oxide to form a 1:1 adduct, that was identified as 2,2-dimethyl-2-trimethylphosphinimino -1,2λ5 -oxaphospholane. According to its 1H, 13C, 31P NMR spectra it is assigned a rigid trigonal bipyramidal structure with nitrogen and oxygen atoms in axial positions.
Alkylsulfonylhydroxylamine CH3(CH2)nSO2NH0H (n = 1, 2, 3) / Alkylsulfonyl Hydroxylamines CH3(CH2)nSO2NH0H ( » = 1. 2. 3)
Authors: Hermann Ulrich , Yaktapour Morteza , Bliefert Claus
Published: February 2015

Some properties of alkylsulfonyl hydroxylamines CH3(CH2)nSO2NH0H (n = 1. 2. 3), prepared by reaction of the sulfonyl chlorides and hydroxylamine, are reported.
Fluorescence and Proton Nuclear Magnetic Resonance Studies of Thallous Ions - Crown Ether Complexes in Organic Solvents
Authors: Platzner T. , Thomas J. K.
Published: February 2015

The complexing of thallous ions (T1+), with the crown ether dibenzo 18 crown-6 poly-ether (DB) has been studied by NMR, fluorescence, and pulse radiolysis techniques. NMR data show a strong interaction of the T1+ ions with the aromatic moieties. This is also illustrated by a static quenching of the aromatic fluorescence by Tl+ . The rates of reactions of T1+ with hydrated electrons eaq- and pyrene excited singlet states are decreases on complexing the ion by the crown ether.
Über die Farbe von „NiO" / The Different Colours of „NiO”
Authors: Propach V. , Reinen D.
Published: February 2015

Depending on the method of preparation ,,NiO”-single crystals of different colours can be synthesized. It is shown by ligand field spectroscopy that the ligand field and interelectronic repulsion parameters are the same for the green, yellow and brown crystals. There is definite spectroscopic evidence, that the colour of stochiometric NiO is green
Präparative organische Chemie unter Verwendung einfach herzustellender Katalysatoren / A Simple Method for Preparation of Catalysts for Preparative Organic Chemistry
Authors: Bölsing Friedrich , Hakim Assadollah
Published: February 2015

There are numerous simple chemical reactions in which reaction products arise, which compared with the materials at the outset, possess a considerably greater surface area. A significant example is the reaction of aluminium alcoholates with water. Reactions of this kind can, to a certain extent, be used as auxiliary reactions, in order to distribute other materials homogenously. In the chosen example, a material dissolved beforehand in the alcoholate, e.g. a solution of a metal salt, would be transferred in the course of the distributing reaction into the newly-developing structure of the reaction product. In this publication the application of some catalysts thus prepared to some classical organic chemical reactions is described by way of example
Zur Reaktivität von C—N-Doppelbindungssystemen, XIV [1] Über das 3.4-Dihydroisochinolin / The Reactivity of the C=N-Double Bound System, XIV [1] Reactions with 3,4-Dihydroisoquinoline
Authors: Ziegler Erich , Leitner Wolfgang , Sterk Heinz
Published: February 2015

3,4-Dihydroisoquinoline reacts with ethyl cyanoacetate in acetic acid/ acetic anhydride to yield the olefine 2. Cyanoacetic acid, ω-cyanoacetophenone and ω-nitroacetophenone act in the same way. Other CH-acidic compounds give addition reactions with 3,4-dihydroisoquinoline yielding 1,2,3,4-tetrahydroisoquinoline derivatives (9-22)
Ternäre Verbindungen in den Dreistoffsystemen Calcium-Kupfer-Phosphor (Arsen) / Ternary Compounds in the Systems Calcium - Copper - Phosphorus (Arsenic)
Authors: Mewis Albrecht , Blumstengel Peter
Published: February 2015

By investigations in the systems Ca-Cu-P(As) we found two ternary phases of the formulas CaCuP and CaCuAs, which crystallize in a hexagonal lattice. We suppose a modified Ni2lntype structure. Some details about a Calcium Copper Phosphide with a ThCr2Si2-type structure are given
Darstellung und Assoziation einiger Phosphiniminoborane / Preparation and Association of Some Phosphiniminoboranes
Authors: Maringgele W. , Meiler A. , Nöth H. , Schroen R.
Published: February 2015

N -Trimethylsily 1 -triphenylphosphinimine re - acts with halogenoboranes R2BX (R = organyl, F, Cl, Br; X = F, Cl, Br) to yield triphenylphosphiniminodihalogenoboranes and triphenylphosphiniminodiorganylboranes, respectively. In solution, the dihalogeno compounds are associated, probably dimeric, while the diorganyl derivatives are monomeric. Mass spectroscopic data of the compounds show them to be monomeric in the vapor phase
Entsteht bei der thermischen Zersetzung yon Natriumtrichloracetat Phosgen ? / Is Phosgene Formed in the Thermal Decomposition of Sodium Trichloroacetate ?
Authors: Dehmlow Eckehard V. , Franke Karl Heinz
Published: February 2015

Decomposition of sodium trichloroacetate in an autoclave yields mainly trichloroacetyl chloride (80%) at 180-200 °C. Carbon tetrachloride, chloroform, and perchloroacetic anhydride are minor products. Only traces of phosgene are formed. These arise from decomposition of perchloroacetic anhydride at temperatures above 200-220 °C (equation (5)). Phosgene is not formed in normal phase transfer catalytic reactions
Synthesis and Crystal Structure of μ-Oxo-bis(phosphenyl-ortho-toluidide)
Authors: Cameron T. Stanley , Cordes Ruth E. , Jackman Florence A.
Published: February 2015

The title compound was synthesised in an attempt to prepare phosphenyl-tri-ortho-toluidine, X-ray crystallographic studies show that it contains a P-O-P bridge with extensively hydrogen bonding between

groups. The P-N bond lengths are different and this can be attributed to some combination of hydrogen bonding and varying p II-d ZII interactions along the bond.
Elektrochemische Intercalation und elektrische Leitfähigkeit von Graphitfasern / Electrochemical Intercalation and Electrical Conductivity of Graphite Fibers
Authors: Besenhard J. . , Fritz H. P. , Möhwald H. , Nicki J. J.
Published: February 2015

Lamellar compounds of graphite fibers have been prepared by electrochemical intercalation. The dependence of the electrical resistance on the intercalate concentration was determined by a quasi simultaneous method. A factor 30 decrease of the relative fiber resistance was obtained with fluorosulfuric acid.
Molekül-und Kristallstruktur des 5.5' -Diethoxycarbonyl-3.3' -diethyl-4.4' -dimethyl-pyrromethen-hydrobromids / Crystal and Molecular Structure of 5,5'-Diethoxycarbonyl-3,3'-diethyl-4,4'-dimethyl-pyirromethene Hydrobromide
Authors: Struckmeier G. , Engel J. , Thewalt U.
Published: February 2015

The crystal and molecular structure of the title compound has been determined by X-ray diffraction. The compound possesses an (almost) planar Z configuration. The ions form ion pairs in the solid state: each bromide anion is connected via two hydrogen bonds with a cation. The crystal data are: space group P21/n with Z = 4; cell dimensions a = 14.097(2), b = 11.591(2), c = 14.133(3) Å, β = 106,22(2)°.
Spectra and Decay Kinetics of Diadamantyl-Dioxetane Chemiluminescence
Authors: Neidl Cornelia , Stauff Joachim
Published: February 2015

The thermal decomposition of 1,2-diadamantyldioxetane was studied by kinetic and spectroscopic methods. Spectra of the chemiluminescence emitted during the thermally induced decomposition of 1,2-diadamantyldioxetane, tetramethyldioxetane and trimethyldioxetane were obtained and the influence of quenchers and radical-scavengers, and the presence of "heavy atoms" in the surrounding of the emitting species was investigated. The kinetics of the decay mechanism was followed by measuring the time dependence of the chemiluminescence. The influence of radical-scavengers, quenchers and "external heavy atoms" on the kinetics was assessed. Experimental results were discussed in terms of a biradical decay mechanism.
Utilization of the Sterically Hindered Base, 4-Hydroxy-2,2,6,6-tetramethylpiperidine, as a Hydrogen Halide Acceptor
Authors: Sosnovsky George , Konieczny Maria
Published: February 2015

The synthetic utility of the sterically hindered base, 4-hydroxy-2,2,6,6-tetramethylpiperidine (1) as a hydrogen halide acceptor was studied.

It was shown that base 1 can be effectively used in the quaternization reaction of primary aliphatic and aromatic amines to give the corresponding trimethylammonium iodides 2 in 88-98% yield. Base 1 was used also as the dehydrobrominating agent of alkyl and cycloalkyl bromides to give the corresponding unsaturated compounds in 82-95% yield.
Investigation of Inductive Effects on the Transphosphorylation Reaction of Spin-Labeled Phosphoryl Imidazolides, Part II
Authors: Sosnovsky George , Konieczny Maria
Published: February 2015

The effect of electron-releasing and electron-withdrawing groups in the benzene ring of imidazolide 4 (R1 = CH3, Cl, NO2) was studied. The

transphosphorylation reaction of imidazolide 4 was not affected by the methyl and chloro substituents, and was accelerated by the nitro substituent. Furthermore, the released imidazole caused the elimination of the p-nitrophenoxy moiety from the product in the presence of the nucleophile.
Organoborierung von Alkinylstannanen, VIII [1] Zur Reaktion von Alkinyltrimethylstannanen mit 1-Boracyclopentanen und Methylbis(tert-butyl)boran / Organoboration of Alkynylstannanes, VIII [1] The Reaction of Alkynyltrimethylstannanes with 1-Boracyclopentanes and Methy Ibis (tert-butyl) borane
Authors: Schmidt Axel , Wrackmeyer Bernd
Published: February 2015

1-Organyl-1-boracyclopentanes react with alkynyltrimethylstannanes to give 1-bora-cyclohexylid(2)enes as the only products. The analogous reaction with methylbis (tert-butyl)borane leads to a nonstatistical distribution of organoboration products. Structure and stereochemistry of the new compounds are discussed on the basis of methanolysis reactions and 1H, 11B and 13C NMR data.
Ag8GeTe6, ein Vertreter der Argyroditfamilie / Ag8GeTe6, a Representative of the Argyrodite Family
Authors: Unterrichter Johanna von , Range Klaus-Jürgen
Published: February 2015

A single crystal of Ag8GeTe6 was found to be rhombohedral, pseudocubic, space group R3m, with a = 817.6 pm, a = 60° and Z= 1. The anion lattice consists of three-dimen­sionally connected Frank-Kasper polyhedra with C. N. 12 and 16. The structure comprises isolated GeTe4-tetrahedra and silver ions, statistically distributed over a number of sites with distorted tetrahedral, trigonal and linear co-ordination. Structural data for some other compounds of the argyrodite family are given.
The Molecular Structure of Allenes and Ketenes, XII [1] Four-Bond Proton-Proton Spin-Spin Couplings in Allenes
Authors: Runge Wolfgang
Published: February 2015

Four-bond proton-proton coupling constants in allenes are reported. The substituent effects on the coupling constants are discussed on the basis of the dual-substituent parameter approach. Furthermore, the coupling constants are related to quantum-chemical indices (electron densities, overlap populations) obtained from semiempirical CNDO/S and ab initio STO-3G calculations.

The magnitudes of the coupling constants depend upon the polar natures of the substituents as well as upon their charge-transfer abilities (resonance effects) to a com-parable amount.

In general, the coupling constants in 1,3-disubstituted allenes are nonadditive in ligand -specific parameters.
Strontiumphosphat-chromat( VI), Sr3(PO4)2·SrCrO4, eine dimorphe Hochtemperaturverbindung / Strontiumphosphate-chromate(VI), Sr3(PO4)2·SrCrO4, a Dimorphie High-Temperature Compound
Authors: Hartl K. , Braungart R.
Published: February 2015

Equimolar mixtures of Sr3(PO4)2 and SrCrO4 form two high-temperature compounds with different ranges of thermal stability. A rhombo-hedral defect-bariumphosphate structure with hexagonal axes ao - 1091 pm and c0 = 3978 pm is stable at 800-1100 °C. At higher temperatures (1200-1400 °C) it changes reversibly to a cubic Eulytite-type structure with ao = 1031 pm. At room temperature both modifications are meta-stable. The thermal stability of the rhombo-hedral form is raised by minute concentrations of gaseous chromium oxides or by partially ex-changing phosphate by chromate(V). With more than 6 mole% of Sr substituted by Ba, the cubic modification only can be obtained.
Kristallstruktur von Sr0,5Ba0,5Si2 bei hohen Drücken / Crystal Structure of Sr0,5Ba0,5Si2 at High Pressures
Authors: Evers Jürgen , Oehlinger Gilbert , Weiss Armin
Published: February 2015

A cubic polymorph (SrSi2 type of structure) is obtained if orthorhombic (BaSi2 type of structure) Sro.5Bao.5Si2 is treated in a belt type apparatus (40 kbar, 1000 °C): P4332 (or P4i32), Z = 4, a = 662.2 pm, xSi = 0.419.
Abbau von Induktionsperioden und Steigerung der Aktivität homogener Hydrierungskatalysatoren mit Iridium als Zentralatom / Reduction of Induction Periods and Increase of Activity of Homogenous Iridium Hydrogenation Catalysts
Authors: Hitzel Erich
Published: February 2015

With complexes of iridium as catalysts, induction periods are typical for homogeneous hydrogenation of olefins in bulk. The induction period decreases, as a rule with increasing activity, at higher temperatures and may be suppressed with dibenzoylperoxide, azobisisobutyrodinitrile, tetrachloro-1,4-benzoquinone or by preactivation. Triethylamin and SnCl2 · 2H2O are unsuitable additives. The operation “preactivation” leads additionally to great substrate/catalyst-turnover numbers.
Reaction of Trivalent Organophosphorus Compounds with Selenium
Authors: Konieczny Maria , Sosnovsky George
Published: February 2015

Selenium derivatives of pentavalent organophosphorus compounds 9, 10, 11 (Ṙ = 2,2,6,6- tetramethyl-1-oxyl-4-piperidyl), 12 and 13 were prepared in 79-99%

yields via the reaction of the corresponding trivalent phosphorus compounds 14, 15, 16, 17, 18 with black

selenium in benzene at room temperature in 20 hours.
Ein Beitrag zur Synthese und Reaktivität von Nitrosyl-Komplexen. Direkte Darstellung von Thiocyanatonitrosyl- Komplexen und von [Mo(NO)(CN)5]3- / A Contribution on the Synthesis and Reactivity of Nitrosyl Complexes. Direct Preparation of Thiocyanatonitrosvl Complexes and of [Mo(NO)(CN)5]3-
Authors: Sarkar S. , Midler A.
Published: February 2015

Some new aspects of the synthesis and reactivity of nitrosyl complexes are given. The complexes [Cr(NO)(NCS5]3-, [Mo(NO)(NCS)4]2- [3a], [Os(NO)(NCS)5]2- and [Mo(NO)(CN)5]3- have been isolated as tetraphenylphosphonium salts.
Unusual Grignard Reaction of α-Arylcinnamonitriles [1]
Authors: Prashad Mahavir , Seth M. , Bhaduri A. P.
Published: February 2015

Reaction of α-arylcinnamonitriles with excess of alkylmagnesium halide yielded predominantly the erythro isomer of α,β-dialkyl-α,β-diarylpropionitriles. PMR spectra of the diastereoisomers have been described.
Ein neues Verfahren zur Bestimmung kleinster Mengen H2O mittels Ph3P und CCl4 /A New Way to Determine Smallest Amounts of H2O by Means of Ph3P and CCl4
Authors: Appel Rolf , Michel Werner , Morbach Wolfgang
Published: February 2015

A new and easier method of water determination in numerous organic solvents is founded on the measurement of the electrical conductivity in the system Ph3P/CCl4/H2O, that is characterised by a typical maximum minimum pattern.

The time interval up to the registration of the well-defined minimum is proportional to the amount of water which can be determined down to concentrations of 10-3 %.
High Power Density Lead Acid Cell Operating at 70 °C
Authors: Fritz Heinz P. , Besenhard Jürgen O. , Paxinos Antonios S.
Published: February 2015

The results presented show the feasibility of a high power density lead acid cell with tubular negatives and positives, operating at 70 °C. Although lead negatives are supposed to deteriorate fast at temperatures above 50 °C, tubular negatives at 70 °C exceed the cycle life of pasted negatives operating at conventional conditions. The high rate discharge capacity of negatives and positives is increasing considerably with temperature. It is concluded that the “temperature gain” of the negative electrode is due to increased mobility of soluble Pb2+ species through the passivating PbSO4 layer and to improved diffusion of H2SO4 in the pore structure.
Kristall- und Molekülstruktur eines „linearen“ Festkörpers mit drei verschiedenen Metallsträngen: [Pt(dapn)2] [Pt(dapn)2Br2] [(Cu3Br5)2] (dapn = 1.2-Diaminopropan)/Crystal and Molecular Structure of a Linear Chain Solid with Three Different Metal Chains: [Pt(dapn)2][Pt(dapn)2Br2][(Cu3Br5)2] (dapn = 1,2-diaminopropane)
Authors: Keller H. J. , Martin R. , Traeger U.
Published: February 2015

The compound {[Pt(dapn)2][Pt(dapn)2Br2]}(Cu3Br5)2, which was prepared by oxidation of Pt(dapn)2Br2 with CuBr2, crystallizes in the orthorhombic space group Bmmb (D2h
17), a = 5.617(4) Å, b = 16.206(6) Å, c = 22.00(1) Å, Z = 2. The experimentally determined density is 3.22 g · cm-3 (calculated 3.40). The structure has been determined by Patterson and Fourier methods from single crystal diffractometer data and refined by least squares to R = 0.085 for 485 independent reflections. Crystals of the title compound contain halide-bridged copper and platinum chains.
Metallkomplexe mit anionischen Liganden von Elementen der 4. Hauptgruppe, XI Homogene Trichlorstannidometallat(O)-Komplexe der 6. und 8. Nebengruppe/Metal Complexes with Anionic Ligands of Elements of the Main Group IV, XI Homogenous Trichlorostannido Metalate(O) Complexes of the Transition Groups VI and VIII
Authors: Krück Thomas , Thielmann Werner , Sauer Christian
Published: February 2015

Various homogeneous metalate(O) complexes are synthesized with [SnCl3] -as a ligand. Complexes of the type [M(SnCl3)6]6- are prepared from [M(CO)3(SnCl3)3]3-(M = Cr, Mo, W) in nitromethane. [Fe(SnCl3)5]5- is formed by UV irradiation of [Fe(CO)4SnCl3]- in aceto-nitrile. [M(SnCl3)4]4-(M = Ni, Pd, Pt) anions are synthesized by thermal substitution reactions with Ni(CO)4, Pd(PF3)4, and Pt(PF3)4. All metalate(O) ions are isolated as salts with the [N(C2H5)4]+ cation and characterized by IR spectra and 119mSn-Mössbauer spectra as well as by analysis.
Einige Gold(I)-Komplexe von Phosphor-yliden und ihre Wirkung in der Gold-Therapie am Modell der Adjuvans-Arthritis /Some Gold(I) Complexes of Phosphorus Ylides and their Effect in Gold Therapy with the Adjuvans Arthritis Model
Authors: Schmidbaur Hubert , Mandl Johann R. , Wohlleben Anette , Fügner Armin
Published: February 2015

A series of ionic phosphorus ylide complexes of gold(I) halides has been prepared and characterized through analytical and spectroscopic data. The compounds are of the type [R3PAu-CH2PR3]⊕Cl⊖, R = C2H5, and [(R3PCH2)2Au]⊕X⊖ where R = CH3, C2H5, n-C4H9, C6H5, and X = Cl, Br (1-6). Along with a cyclic complex [(C2H5)2P(CH2)2Au]2 (7) these materials have been tested in a pharmacological study for a possible use in an oral arthritis therapy.

Compounds 1 and 5-7 showed no or only neglegible effects on Adjuvans-arthritis induced in rats, while 3 and 4 were very toxic. Complex 2 was comparable to standard chrysotherapeutic agent3 in a preliminary study, but a more detailed investigation including LD50 tests for mice showed too narrow a gap between its toxical and therapeutically useful doses.
Di-μ-methoxi-bis[dicarbonyl(tri-tert-butylphosphin)ruthenium(I)](Ru-Ru)/Di-μ-methoxi-bis[dicarbonyl(tri-tert-butylphosphine)ruthenium(I)](Ru-Ru)
Authors: Schumann Herbert , Opitz Joachim
Published: February 2015

{(Ru(μ-OCH3)(CO)2[P(t-C4H9)3]}2 is prepared by the reaction of Ru3(CO)12 with P(t-C4H9)3 in methanol or by refluxing Ru(CO)3[P(t-C4H9)3]2 in methanol. The IR, Raman, and NMR spectra are reported and discussed.
Zweikernkomplexe mit heterometallischer Palladium-Platin-Bindung/Binuclear Complexes Containing a Heterometallic Palladium-Platinum Bond
Authors: Werner Helmut , Kühn Alfred
Published: February 2015

The reaction of C5H5Pt(2-RC3H4) (R = H, CH3) with PdL2 (L = P(i-C3H7)3, P(c-C6H11)3) in the molar ratio of 1:1 produces the binuclear complexes (μ-C5H5)(μ-2-RC3H4)PdPtL2 in which the metal atoms have the formal oxidation state + 1. Based on the 1H, 13C and 31P NMR spectra it is assumed that the structures of the new complexes are analogous to those of the corresponding Pd2 and Pt2 compounds but that they contain a heterometallic palladium-to-platinum bond. The synthesis and the spectra of the bis(allyl) complex (μ-2-CH3C3H4)2PdPt[P(i-C3H7)3]2 are also reported.
Darstellung und Struktur des Komplexes [C5H5Cr(NSiMe3)2]2 (Zur Reaktion von Cyclopentadienylmetallchloriden mit Bis(trimethylsilyl)diazen)/Preparation and Structure of the Complex [C5H5Cr(NSiMe3)2]2 (Reaction of Cyclopentadienylmetal Chlorides with Bis(trimethylsilyl)diazene)
Authors: Wiberg Nils , Häring Heinz-Wolfgang , Schubert Ulrich
Published: February 2015

Bis(trimethylsilyl)diazene reacts with cyclopentadienyl metal chlorides with reduction followed by addition. According to X-ray analysis the chromium complex [C5H5Cr(NSiMe3)2]2, formed by the reaction of C5H5CrCl2 with azosilane, contains tri-methylsilylazene ligands. The addition of Me3Si-N = N-SiMe3 to chromium is therefore connected with a cleavage of the azo group in this case.
Tri(tert-butyl)phosphinimin / Tri(tert-butyl)phosphine Imine
Authors: Wolfsberger Werner
Published: February 2015

Tri(tert<-butyl)phosphine imine has been prepared by desilylation of the corresponding N-trimethylsilyl compound. The imine, which is stable against water, oxygen, sodium, and lithium hydride, can be protonated by hydrogen halides, methylated by methyl iodide, and lithiated by lithium methyl. The pyrolysis at about 200 °C leads to tri(tert-butyl)- phosphine. From N-lithium tri(tert-butyl)phosphine imide N-substituted derivatives can be obtained.
Siliciumverbindungen mit starken intramolekularen sterischen Wechselwirkungen, VIII [1]. Neue Siloxanverbindungen einiger Übergangsmetalle / Silicon Compounds with Strong Intramolecular Steric Interactions, VIII [1]. New Siloxane Compounds of Some Transition Metals
Authors: Weidenbruch Manfred , Pierrard Claude , Pesel Helge
Published: February 2015

Tri-tert-butylsiloxane compounds of transition metals are obtained by two different routes, one of these involves condensation of tri-tert-butylsilanol with the binary oxides V2O5, CrO3, MoO3, and Re2O7, while the other proceeds via a similar reaction between the chlorides VOCl3, NbCl5, TaCl5, CrO2Cl2, and the silanol. The new compounds, having good thermal stability and remarkable resistence to hydrolysis, are characterized by IR, 1H NMR, and mass spectra.
Halogen-Elpasolithe, IV [1]. Über Brom-Elpasolithe Cs2BIMIIIBr6 BI = Li, Na; MIII = Sc, Y, La-Lu, In, V, Cr) / Halo-Elpasolites, IV [1]. On Bromo-Elpasolites Cs2BIMIIIBr6 BI = Li, Na; MIII = Sc, Y, La-Lu, In, V, Cr)
Authors: Meyer Gerd , Gaebell Hans-Christian
Published: February 2015

Bromo-Elpasolites of formulae Cs2LiMBr6 and Cs2NaMBr6 (M = Sc, Y, La-Lu, In, V, Cr) were prepared and investigated by powder X-ray diffraction. The compounds Cs2NaMBr6 (M = Ce-Lu, Sc, Y, In) as well as Cs2LiMBr6 (M = La-Er, Y) crystallize cubic facecentered (elpasolite type of structure); Cs2NaLaBr6 and low temperature forms of Cs2NaMBr6 (M = Ce-Gd) are tetragonal. Several hexagonal crystal structure types (HT-K2LiAlF6, Cs2NaCrF6, Cs2LiGaF6) are observed for Cs2LiMBr6 (M = Tm, Yb, Lu, Sc, In, V, Cr).
Kinetic Study of the Acid Hydrolysis of Ethyl Hydrogen Succinate in Binary Solvent Mixtures
Authors: Khalil Fayez Y. , Hanna M. T.
Published: February 2015

The specific rate constants for the acid-catalysed hydrolysis of ethyl hydrogen succinate in water and in a series of acetone-water and dioxane-water mixtures were determined at 30-45 °C. The solvent composition covered the range 0-90% by weight of the organic solvent. The rate was found to decrease to a minimum at about 80% of the organic solvent then to increase again with successive addition of the latter. In dioxane-water medium a slight initial increase in rate on the first addition of dioxane to water was observed and attributed to an increase in the number of "free" water molecules. The activation energy showed only slight dependence on solvent composition. The radius of the activated complex was calculated in the two media. The thermodynamic parameters were evaluated and discussed in terms of solvent composition. The reaction proved to be essentially an ion-dipole rather than an ion-ion interaction. A comparative discussion of the specific solvent effects of the two solvent systems under consideration is presented, based on the respective bond energies as given by the heats of mixing of the solvent components.
NMR-Untersuchungen an Organoelement(IVb)-phosphinen, V [1]. 59CO-NMR-, IR-und UV-spektroskopische Untersuchungen an Organoelement(IVb)-phosphin-substituierten Komplexen des Tricarbonylnitrosylcobalt / NMR Studies on Organoelement(IVb)-phosphines, V [1]. 59Co-NMR, IR and UV Spectroscopic Investigations on Organoelement(IVb)Substituted Complexes of Tricarbonylnitrosylcobalt
Authors: Schumann Herbert , Meissner Manfred , Kroth Heinz-Jürgen
Published: February 2015

59Co NMR chemical shifts are reported for complexes of the type [(CH3)3M]n[tC4H9]3-nP(CO)-2(NO)Co (M = Si, Ge, Sn; n = 1, 2, 3) and related to some IR and UV spectral data of the same compounds.
Synthesis of New Furobenzoxazole and Furoflavone Derivatives
Authors: Hishmat Orchidée H. , Khalil Khairia M. , El-Ebrashi Nabila M. A. , Khodeir Mohamed N. M.
Published: February 2015

The synthesis of visnaginone-oxime (2 a) and khellinone-oxime (2 b) is reported. Beckmann rearrangement of 2 a and 2b using different cyclising agents was studied. Structure assignement for the produced benzoxazole derivatives and benzisoxazole derivatives was confirmed by chemical and spectral evidences. Utilization of visnaginone (la) and khellinone (lb) for the synthesis of new furoflavone derivatives was also undertaken.
Studies on Ferrocene and its Derivatives, VI. Cyclocondensation Reactions of Some Ferrocenyl Anils
Authors: Hassan Kh. M.
Published: February 2015

Ferrocenealdehyde have been condensed with some amines giving the corresponding Schiff bases. Cyclocondensation reaction of chloroacetylchloride (or thioglycolic acid) on ferrocenyl Schiff bases yielded ferrocenyl-β-lactams and ferrocenylthiazolidinones.
Synthesis of Some New Spiro Heterocyclic Nitrogen Compounds, II
Authors: Hassan Kh. M. , El-Shafei A. K. , El-Kashef H. S.
Published: February 2015

The synthesis of spiro-γ-amino(or γ-chloro)-β lactams and spiro-4-thiazolidones by the cycloaddition reaction of 3-isatylidene anil derivatives, phthalylglycyl chloride (or chloroacetyl chloride) and/or mercaptoacetic acid has been investigated. 3-Isatylidene anils were prepared by the reaction of isatine with substituted aniline, a-naphthylamine, 2-aminothiazoles, 2-aminothiadiazoles and 2-aminopyridine, respectively.
Über den Farbstoff der Gramfärbung von Bakterien / On the Pigment of the Gram Staining of Bacteria
Authors: Lecea M. J. Volz-de
Published: February 2015

Tris-(4-dimethylaminophenyl)-carbenium-triiodid, a salt of crystal violet, is determined as probable structure of the Gram Staining of Bacteria. A mechanism of it is proposed based on the chemical properties of this salt.
Hydrazine Derivatives of β-Dicarbonyl Compounds, Part I. Studies on Some Benzoylacetaldehyde Aroylhydrazones
Authors: Rateb Latif , Azmy B. , Nashed M. A. , Iskander M. F.
Published: February 2015

A series of benzoylacetaldehyde benzoylhydrazones were prepared and characterised. Their UV, IR, and 1H NMR spectra suggest the enol-imine structure rather than the keto-imine form of analogous Schiff bases. The pKa values of these aroylhydrazones were also measured and correlated with the Hammet substitution constants.

Attempted cyclizations of these open-chain aroylhydrazones afforded the corresponding 5-hydroxy-2-pyrazoline compounds rather than the expected pyrazoles.
13 C NMR Spectra of Chromeno-and Prenylated Flavones Structure Revision of Mulberrin, Mulberrochromene, Cyclomulberrin and Cyclomulberrochromene
Authors: Chari V. Mohan , Ahmad Saboor , Österdahl Bengt-Göran
Published: February 2015

Reappraisal of the 13C NMR data for mulberrin and mulberrochromene indicate a revision of structure for these two compounds as well as for cyclomulberrin and cyclo-mulberrochromene .
Eine ungewöhnliche intramolekulare Photoreaktion eines Hexachlorhexahydromethanonaphthalins / An Unusual Intramolecular Photoreaction of a Hexachlorohexahydromethanonaphthaline
Authors: Parlar H.
Published: February 2015

Photoreactions of 2-exo-bromo-5,6,7,8,9,9- hexachloro-1,2,4 a, 5,8,8 a-hexahydro-5,8-methanonaphthaline (1) were studied in the presence of acetophenone. With the help of column chromatography an unusual isomerisation product (3) was isolated, whose structure was established by spectral data obtained by mass spectrometry, infrared spectroscopy, and 1H nuclear magnetic resonance measurements.
Ternäre Phasen im System Eisen-Thallium-Schwefel/Ternary Phases in the System Iron Thallium-Sulfur
Authors: Zabel Manfred , Range Klaus-Jürgen
Published: February 2015

The Compound TlFeS2 was synthesized from TlS/Fe/S-mixtures. Crystals are mono-clinic (space group C2/m) with a = 1164.4(6) pm, b = 530.8(3) pm, c = 1050.9(5) pm, β = 144.58° and Z = 4. The structure comprises [FeS2-]∞-chains parallel b, built from edge-shared FeS4-tetrahedra. Relations between TlFeS2 and orthorhombic CsFeS2 are discussed. Tetragonal or monoclinic distorted tetragonal ternary phases occur with composition FexTl2S4 (2.6 < x < 3.6 ).
Methylmetallbromo-und -iodokomplexe des Galliums und Indiums/Methyl Metal Bromo and Iodo Complexes of Gallium and Indium
Authors: Widler Hans-Jörg , Weidlein Johann
Published: February 2015

The interaction of (CH3)3MIII or (CH3)2MIIIHal with (CH3)3MV Hal2 and (CH3)4MVHal, respectively, yields methylhalogeno metalates of the general composition [(CH3)4MV]+[(CH3)4-xMIIIHalx]-. (With MV = As, Sb; MIII = Ga, In; Hal = Br, I and x = 1-3.) The vibrational spectra of these ionic compounds are reported and discussed.
Phosphorus-Nitrogen Compounds, Part XLV Friedel-Crafts Reactions of Some Aminochlorocyclotriphosphazatrienes
Authors: Das Sunil Kumar , Masood-Ul-Hasan  , Shaw Robert A. , Smith Barry C. , Woods Michael
Published: February 2015

Chloroaminocyclotriphosphazatrienes, N3P3Cl6-nRn [R = NHMe (n = 2), NHEt (n= 1, 2), NHPrn (n = 4), NHPri ( n = 1, 4), NHBut (n = 2, 4), NHCH2Ph ( n = 1), NEt2 (n= 1, 2, 3), N(CH2Ph)2 (n = 1)] react with benzene in the presence of anhydrous aluminium chloride to give phenylated products: phosphazenes and/or hydrocarbons. The structures of the phenylphosphazenes are assigned from their NMR spectra. Reactions of N3P3Cl5R (R = NMe2, NC5H10) have been reinvestigated. The influence of the amino groups on rates and products is discussed.
Substituent and Solvent Effects on HCN Elimination from 1-Aryl-1,2,2-tricyanoethanes
Authors: Fouad Fouad M. , Farrell Patrick G.
Published: February 2015

The elimination of HCN from 9-dicyanomethyl-fluorene (2), 1,1-diphenyl-1,2,2-tricyanoethane (3), and 2-phenyl-1,1,2-tricyanopropane (4) in anhydrous methanol has been studied and shown to occur via an (E l)anion mechanism. Elimination of HCN from 2 in acidic, buffered and MeO-/MeOH solutions have also been studied. Addition of water or benzene to the reaction medium shifts the mechanism to (E 1 CB)ʀ. Elimination of HCN from N,N-dimethyl-4-(1,1,2-tricyanoethyl) aniline (5) in anhydrous methanol occurs via an (E 1 cB)ʀ mechanism and the kinetics indicate that addition of HCN to the product alkene occurs. Activation parameters, isotope effects and solvent effects have been examined in an effort to obtain information about the nature of the transition states of these reactions.
Synthesis of Hexahydro-bis[benzo-dipyrazolones, benzo-diazepinone] and Dithiopyrimidoquinazolinetetrone
Authors: Amer Fathy Abdel Kader , Afsah El-Sayed , El-Zimaity Mohamed Tawfik , Metwally Mohamed Abbas
Published: February 2015

A new series of hexahydro-bis-benzodipyrazolones (2a-e) were obtained by the inter-action of 1 with hydrazines. These pyrazolones underwent coupling reaction with different diazonium salts to give 7a-g. Compound 1 when treated with acid hydrazides gave 3 a, b, and when subjected to Japp-Klingemann reaction in alkaline medium gave 6a-e. The hexahydro-bis-benzodiazepine (8), and dithiopyrimidoquinazolinetetrone (10) were obtained by the interaction of 1 with o-phenylenediamine and thiourea respectively.
A Convenient Synthesis of Naphth[2′,3′ : 5,6]- and [1′,2′ : 5,6]-1,3-oxazino[3,2-b]benzimidazoles and Benzoxazolo[3,2-b] [l,3]quinazolone - Mechanism of Thiophosgene Heteroeyelisation [1]
Authors: Dubey S. K. , Sharma Satyavan , Iyer R. N.
Published: February 2015

Reaction of thiophosgene or phosgene on 2′-aminonaphthanilides (2, 5) gave the corresponding 2-substituted-6-oxonaphth[2′,3′: 5,6]-1,3-oxazino[3,2-b]benzimidazoles (3) and 6-oxonaphth[1′,2′:5,6]-1,3-oxazino[3,2-b]benzimidazoles (6) respectively. The mechanism of such reactions has been studied by carrying reaction between 2′-hydroxy - anthranilide (7 a) and thiophosgene in acidic and basic media.
Darstellung und Raman-Spektrum Preparation and Raman Spectrum of ReO3Cl·SbCl5/ Preparation and Raman Spectrum of ReO3Cl·SbCl5
Authors: Dehnicke Kurt , Liese Werner
Published: February 2015

Rheniumoxychloride forms with antimony pentaehloride a donor-acceptor complex, ReO3Cl·SbCl5. According to the Raman spectrum the complex contains a Re-O-Sb bridge.
Neue Phasen im System Thallium-Eisen-Schwefel/New Phases in the System Thallium-Iron-Sulphur
Authors: Sabrowsky Horst , Mirza Jahangir , Methfessel Christoph
Published: February 2015

The structure and magnetic properties of the new ferromagnetic compounds TlFe1+xS2 (0,25 ≤ x ≤ 0,85) were investigated. A new monoclinic phase Tl3Fe2S4 (a = 1303, b = 1114, c = 738,3 pm, β= 124,5°, Z = 4, space group C5
2h) was characterized by single crystal X-ray techniques.
The Molecular Structure of Allenes and Ketenes, XIII Correlations of Carbon-Proton Spin-Spin Coupling Constants in Allenes with ab initio STO-3G Overlap Populations
Authors: Runge Wolfgang
Published: February 2015

It is shown that substituent effects on one-bond and long-range carbon-proton coupling constants in monosubstituted allenes parallel quantitatively ab initio STO-3G carbon 2s-hydrogen 1 s overlap populations, irrespectively of whether the substituents are bonded to the allenic skeleton via first-row (C, O) or second-row (Si, S, Cl) atoms.
Benzo(c)-1 λ4.2-thiazol, ein neues bicyclisches 10π-System/ Benzo(c)-1 λ4 ,2-thiazol. a New Bicyclic 10π-System
Authors: Klingebiel Uwe , Bentmann Dieter
Published: February 2015

In the reaction of lithiated N-(fluorodimethylsilyl)-2,4,6-trimethylaniline with bis(trimethylsilyl)-sulfurdiimide LiF is eliminated and a benzo(c)-1 λ4 ,2-thiazol is formed. Trifluoroacetic acid reacts with this thiazol to give the trifluoroacetate.
Darstellung und Kristallstruktur von CsAlF4 / Preparation and Crystal Structure of CsAlF4
Authors: Lösch Roland , Hebecker Christoph
Published: February 2015

Single crystals of CsAlF4 have been prepared from a mixture of CsF and AlF3 and investigated by X-ray methods, CsAlF4 crystallizes hexagonally (isostructurally to the new CsCrF4-type) with a = 9.500, c= 3.713 Å, Z= 3, space group P62m-D3h
3, No. 189. AgAlF4 crystallizes orthorhombically (isostructurally to a-RbFeF4) with a = 7.108, b = 7.111, c = 5,568 Å, Z = 4.
Basic Chromium(III) Formate: Reaction of Chromiiim(III) Chloride with Formic Acid
Authors: Paul R. C. , Kapoor P. , Baidya . B. , Kapoor R.
Published: February 2015

Chromium(III) Chloride, Basic Chromium(III) Formate, IR, Thermogravimetry, Magnetic Moment Chromium(III) chloride reacts with anhydrous formic acid to give basic chromium(III) formate [Cr3O(OOCH)6(H2O)2(HCOOH)](OOCH), HCOOH. Its reactions with bases (B) give compounds of the general composition [Cr30(C00CH)6(B)3](00CH). The title compound has been characterized by infrared spectral data, temperature range (266-110K) magnetic moment and thermogravimetry.
Über Additionsreaktionen von zinnorganischen Verbindungen mit N.N′ -Bis(pentafluorphenyl)-sehwefeldiimid / Addition Reactions of Tinorganic Compounds with N,N′-Bis(pentafluorophenyl)sulfurdiimide
Authors: Roesky Herbert W. , Schmieder Wilfried , Ambrosius Klaus
Published: February 2015

The reactions of N,N′ -bis(pentafluorophenyl)sulfurdiimide with [(CH3)3Sn]2NCH3, [(CH3)3Sn]3N and [(CH3)3Sn]2NC6F5 yiels the 1:1 adducts 1-3. 1H and 19 F NMR investigations show, that fluorine atoms in the ortho position of the phenyl ring coordinate to the tin atom. This causes an increase of electron density at tin. A similar interpretation is given for the adduct 4 of N,N′-bis(p-chlorophenylsulfonyl)sulfurdiimide and [(CH3)3Sn]2NCH3, where an oxygen atom of the sulfonyl group is bonded to tin.
The Isolation and Characterization of Molecular Complexes Produced from the Reaction of Nitrophenols with Divalent Metal Oxinates
Authors: Aly M. M. , Shalaby A. M.
Published: February 2015

The reaction of nitrophenols (picric acid, 2,6-dinitrophenol, and 2,4-dinitrophenol) with divalent metal oxinate (metal = Cu, Co, Ni, Mn, and Zn) produced a type of molecular complex, which comprises two molecules of the metal oxinate and one molecule of the nitrophenol. In the case of the Mg complex the ratio is 1:1. A definite charge-transfer band is detected for the Co(II) complex. A hydrogen bonding system O1...H+...O2 is suggested. This includes the proton of the nitrophenol and two oxygen atoms; each is related to a coordinated oxinate of two different metal oxinate molecules. Analytical and spectral evidence are in accordance with the tentatively suggested formulations.
Zur Strukturchemie der Diperoxovanadate(V): Das μ-Hydroxo-bis [oxo-diperoxovanadat(V)] Anion / Studies on Diperoxovanadates: The μ-Hydroxo-bis [oxo-diperoxovanadate(V)] Anion
Authors: Wieghardt Karl , Quilitzsch Udo
Published: February 2015

Depending on the pH and the respective concentrations of solutions containing NH4+/NH3/H2O2/NH4VO3 three yellow ammonium salts can be isolated:

(NH4)4[O(VO(O2)2)2], NH4[VO(O2)2NH3]; and the novel (NH4)3[HV2O11] · 2 H2O. A cesium and potassium salt of the latter anion have been prepared. The infrared spectra of these salts are interpreted assuming a μ-hydroxo-bis[oxo-diperoxovanadate(V)] structure in the solid state.
Photoredox Reaction of trans-4-Stilbenecarboxylatopentaamminecobalt(III)
Authors: Vogler Arnd , Kern Alfred
Published: February 2015

The irradiation (λ = 313 nm) of aqueous [Co(III)(NH3)5TSC]2+(TSC-= trans-4-stilbenecarboxylate) leads to a redox reaction with formation of Co2+ as has been shown previously. The TSC-ligand is oxidized to the radical in the primary photoreaction. At higher complex concentrations (～10-2 M) this TSC radical is oxidized to stable products (Φ = 0.09 ± 0.02) by [Co(NH3)5TSC]2+,which is reduced to Co2+ leading to release of the TSC- ligand (Φ = 0.07 ± 0.02). Co2+ is thus formed by both the secondary and the primary photo chemical reaction (Φ overall = 0.16). At low complex concentrations (< 10-4 M) in the presence of air, the primary TSC radical is scavenged by O2. Benz-aldehyde is an oxidation product. This reduces the formation of Co2+ to Φ = 0.09 ± 0.02, which is taken to be the efficiency of the primary photo chemical step. It is suggested that the photoredox reaction is initiated by an electron transfer from the first excited singlet of the TSC- ligand. As shown by sensitization experiments, the population of the lowest TSC-triplet leads to the usual trans/cis isomerization of the TSC-ligand, but not to the redox reaction.