bluuebunny/crossref_metadata_2025 huggingface dataset:
Vergleich der Hydrierung ungesättigter Verbindungen mit einem homogenen und heterogenen Platin-Katalysator in Essigsäure.
Authors: Strohmeier Walter , Pföhler Magdalena
Published: March 2015

Catalytical hydrogenation of unsaturated compounds in acetic acid with the homogeneous catalyst prepared from H2PtCl6 + SnCl2 • 2 H2O and the heterogeneous catalyst, prepared from H2PtCl6 and H2, were carried out. A comparison of the results reveals two types of substrates, some are readily hydrogenated by the homogeneous the other ones by the heterogeneous system. Turnover numbers up to 1500 were observed. With the heterogeneous catalyst ethylbenzene is hydrogenated to ethylcyclohexane under mild conditions.
Die Kristallstruktur des Spirophosphorans (HOCH2 · C6H3 · CH2O)2PPh.
Authors: Hellwinkel D. , Krapp W. , Schomburg D. , Sheldrick W. S.
Published: March 2015

The title compound crystallises in the monoclinic space group, Cc, Z = 4, with a = 12.370(1), b = 19.447(1), c = 7.786(1) Å, β = 90.82(1)°.

The structure was solved by direct methods and refined to R = 0.070 for 2163 independent reflections.

Trigonal-bipyramidal geometry is observed at phosphorus with the ring oxygens occupying the axial sites. The plane of the phenyl substituent makes a dihedral angle of 20.2° with the equatorial plane. The molecules are linked into infinite chains in the [010] plane through (CH2)O ••• H—O(CH2) hydrogen bonds of length 2.77 A.
Notizen: Eine neue Totalsyntese von Methionin-Enkephalin.
Authors: Voelteb Wolfgang , Kalbacheb Hubert , Pietrzik Emanuel
Published: March 2015

A new improved synthesis of methionineenkephalin is described. For methionineenkephalin the structure

L-Tyr-Gly-Gly-L-Phe-L-Met-OH has been suggested most recently. The peptide is synthesized from Boc-Gly-Gly-OH, H-L-Phe-OMe, Boc-L-Tyr(Bzl)-OH and H-L-Met-OMe by means of “classical” methods.
Verbindungen mit Tellur in niedrigen Oxidationsstufen, Ø Reaktion von Diarylditelluriden mit Aryltellurtrihalogeniden.
Authors: Dorn Wolf L. , Knöchel Arndt , Schulz Petra , Klar Günter
Published: March 2015

The conproportionation of diaryl ditellurides and aryltellurium trihalides resulting in aryltellurenyl halides has been investigated using conventional and isotopo tracer methods. The aryltellurenyl halides are in general unstable and disproportionate to diaryltellurium dihalides and elementary tellurium.
Potentiometric Determination of Stability Constants of Trivalent Metal Ion Complexes with Di-p-tolyl-thiovioluric Acid
Authors: Mathur Pavan , Goel D. P. , Singh R. P.
Published: March 2015

The consecutive formation constants of 1:1, 2:1, 3:1 chelate species formed by the interaction of di-p-tolyl-thiovioluric acid (D-p-TOTVA) with the tripositive lanthanons and yttrium cations were determined potentiometrically at 0.1 µ (NaClO4) at 30± 1°C, in 75% aqueous dioxan.

The 1:1 formation constants (log K1) for the complexes increase with the increase in the atomic number of the lanthanon (3), with a break at gadolinium.

The results indicate that the ligand bonds bidentately to heavier lanthanons (smaller ionic radii). However, definite dentate character of bonding to lighter (larger ionic radii) lanthanons could not be established.
Halogenokomplexe von Osmium(III) mit Pyridin, Pyrazin, Pyrimidin und einigen Methylhomologen.
Authors: Scheffler A. , Preetz W.
Published: March 2015

The preparation of mer-[OsX3B3], X = Cl, Br, I; B = pyridine, 3-resp. 4-picoline, pyrimidine, pyrazine, methylpyrazine, and the chromatographic isolation of four basemixed stereoisomers mer-[OsX3(py)n(mepyz)3-n], n= 1, 2, as solid crystalline products is described. Mass spectra and ligand exchange reactions confirm the structure of these complexes. The UV and IR spectra are discussed.
IR- und NMR-spektroskopische Untersuchungen an Rubazonsäuren.
Authors: Bratan-Mayer Silke , Strohbusch Frank , Hänsel Wolfram
Published: March 2015

The IR and NMR spectra of rubazonic acids 1 and 2 show that these compounds form only OH tautomers in nonpolar solvents and in the crystalline state. They are stabilized by a strong intramolecular hydrogen bond in an eight-membered ring. The IR and NMR spectra show that they exhibit a symmetrical structure. The hydrogen bond has a double minimum potential. Alteration of the symmetry of substitution in 1- and 1′-positions markedly influences the signal of the OH proton. This symmetry effect is discussed.
Beiträge zur ökologischen Chemie, CXIII1
Photoinduzierte Desaminierungsreaktion an 4-Amino-3-methylthio-1.2.4-triazin-5(4H)-onen.
Authors: Bartl P. , Parlar H. , Korte F.
Published: March 2015

Photokinetic experiments show that the deamination reaction of a series of 4-Amino-3-methylthio-1.2.4-triazin-5(4 H)-ons (1 a—e) is dependent on oxygen and nature of solvent. Experiments with a series of 6-tert-Butyl-3-methylthio-1.2.4-triazin-5(4 H)-ons (3 a—e) indicate that the formation of 6-tert-Butyl-3-methylthio-1.2.4-triazin-5-ons (2 d) occurs only in the case of an N—N-bond, but is, however, completely independent of the substituent on the nitrogen atom which is split off.
Notizen: Zur Stereochemie der Phosphinoxidspaltung chiraler acyclischer Phosphoniumsalze.
Authors: Luckenbach Reiner
Published: March 2015

The stereochemistry of the ‘phosphine oxide cleavage’ of 37 different chiral acyclic quaternary phosphonium salts under various reaction conditions is presented and discussed.
Zur Reaktivität von C=N-Doppelbindungssystemen, IX1 Reaktionen mit Harnstoff, Thioharnstoff, N.N-Dimethylsemicarbazid bzw. Cyanamid.
Authors: Ziegler Erich , Zwainz Johannes G.
Published: March 2015

Benzylidene aniline reacts with Ac2O/AcOH yielding 2-phenylperhydro-s-triazin-4,6-dione (“benzalbiuret”). Thiourea or N,N-dimethylsemicarbazide give the corresponding 8-triazines in a similar way. However, the reaction with cyanamide leads to N-benzylidene carbamic acid nitriles.
Notizen: SrSb2, eine neue Zintlphase.
Authors: Deller Klaus , Eisenmann Brigitte
Published: March 2015

The new intermetallic compound SrSb2 has been prepared and its crystal structure determined. The “anionic” part of the structure consists of (Sb-)-zigzag-chains, so the compound belongs to the “Zintl-phases”.
Photoelektronenspektroskopie an den Alkalimetallen Rb und Cs und deren metallreichen Oxiden / Photoelectron Spectroscopy of the Alkali Metals Rb and Cs and their Metal Rich Oxides
Authors: Ebbinghaus G. , Braun W. , Simon A.
Published: March 2015

The alkali metals Rb and Cs and their suboxides Cs11O3, Cs7O (≙ [Cs11O3]Cs10) and [Cs11O3]Rb7 have been investigated by UPS (HeI).

Extremely narrow O2p levels are observed, as well as significant differences in the binding energies of the 5p levels of chemically different Cs-atoms. From energy loss structures (surface plasmons) electron concentrations are determined.

The results are discussed in terms of structurally derived bonding models. The alkali metal suboxides are of importance in IR-sensitive Ag/Cs/O-photocathodes.
ESR-Untersuchungen von Nitroxyl-Radikalen / ESR Studies of Nitroxyl Radicals
Authors: Scheffler K. , Schuler P. , Sosnovsky G.
Published: March 2015

Mono-, di- and trinitroxylradicals are investigated in solution by ESR spectroscopy. The ESR spectra of all multispin systems studied can be interpreted under the assumption of an exchange interaction of the radical electrons. The exchange energies J are evaluated by comparison of experimental and theoretical line positions. The temperature dependence of J leads to activation energies around 1.5 Kcal/Mol. The analysis of proton hfs of the biradicals indicates the existence of two radical species which slow and fast exchange rates.
Notizen: Infrarotabsorption von AlCl und AlBr in festen Edelgasmatrizen.
Authors: Schnöckel Hg.
Published: March 2015

The vibrational frequency of Al35Cl in solid neon and argon has been measured to be 470 cm-1 and 455 cm-1. The 35Cl/37Cl isotopic splitting is 5.4 ± 0.2 cm-1 in argon matrix. The IR absorption of AlBr has been recorded in neon, argon and nitrogen matrices (370, 357, 349 cm-1). In solid argon the frequency shift due to 81Br/79Br isotopes could be resolved (0.95 ± 0.2 cm-1). The fundamental v3 of monomeric AlBr3 is observed at 508.4 cm-1 in an argon matrix.
Notizen: Di-tert-butylchlorthioarsoran / Di-tert-butylchlorothioarsorane
Authors: Ross B. , Marzi W. , Wilhelm G.
Published: March 2015

The preparation of the first chlorodiorganylthioarsorane is reported. Amidodi(tertbutyl)arsine and sulfur react to give amidodi(tert-butyl)thioarsorane, which is converted into chlorodi(tert-butyl)thioarsorane by a solution of HCl in ether. Some reactions of chlorodi(tert-butyl)thioarsorane are described.
Die elektrische Leitfähigkeit hydratisierter Sulfate zwei- und dreiwertiger Kationen.
Authors: Fritz Heinz P. , Laschka Dagmar
Published: March 2015

The electrical conductivity of polycrystalline pellets of ZnSO4 · 7 H2O, MgSO4 · 7 H2O, CuSO4 · 5 H2O, KAl(SO4)2 · 12 H2O, NH4Al(SO4)2 · 12 H2O and KCr(SO4)2 · 12 H2O was measured. By coulometry the role of protons as charge carriers was determined. A correlation is given between the strength of hydrogen bonds and the activation energies for the proton conductivity.
Darstellung und Kristallstruktur des Na2Ga2Se3.
Authors: Weis Jürgen , Schäfer Herbert
Published: March 2015

Na2Ga2Se3 crystallizes trigonal/rhomboedric with a = 3.96 ± 0.02 Å and c = 25.01 ± 0.006 Å, c/a = 6.31. Na-atoms and Ga2-dumbbells occupy distorted octahedral sites in a close-packed ... ABCABC ... arrangement of Se-atoms. The final R-value is 0.143.
Untersuchung des M2/M3-Phasenübergangs in V1-xFexO2 mit x = 0,024.
Authors: Pebler J. , Schmidt K. , Wasinski H.
Published: March 2015

The Mössbauer investigations of V1-xFexO2 with x = 0.024 indicate that Fe enters two cation positions of M2 and M3. At the phase transition the two quadrupole splittings show a discontinuous behavior whereas the isomer shift changes continuously with a crossingover at the M2, M3 transition (Tt′ = 275 K). Generally a first order phase transition is accompanied by a change of the cell volume V and a change of the isomer shift. The observed continuous behavior of the isomer shift points to a first order transition with δV ≠ 0.
Synthesen von TRH-Derivaten des Typs L-Pyr-L-His-L-Pro-NH-(CH2)n-NHa (n = 4, 7,10).
Authors: Fuchs Stefan , Voelter Wolfgang
Published: March 2015

Synthetic routes to a new class of biologically active TRH derivatives of the general structure L—Pyr—L—His—L—Pro—NH—(CH2E)n—NH2 are described.
Notizen: Die Anwendung von Parametern der gegenseitigen Wechselwirkung in der 29Si-Resonanz.
Authors: Vongehr M. , Marsmann H. C.
Published: March 2015

Silicon 29-chemical shifts can be described in some cases in terms of pairwise interaction parameters, although the influence of higher order effects is always perceptible. These are especially significant where fluorine or oxygen are the ligands around the silicon. Parameter of pairwise interaction for a number of ligands are given.
Notizen: Hochenergetische Moleküle. Synthese von Tetramethyl-1.2-dioxa-4.5-diazin durch Photooxidation von Acetonazin.
Authors: Lechtken P.
Published: March 2015

By photooxidation of acetoneazine the unstable tetramethyl-1,2-dioxa-4,5-diazine and the trimeric acetoneperoxide are obtained. The dioxadiazine cleaves into acetone and nitrogen with a half live of ~ 20 min at 40°C (in CH2Cl2) and induces luminescence in added fluorescent dyes.
Neue intermetallische Verbindungen im anti-Ce2O2S-Strukturtyp. / New Intermetallic Compounds in the anti-Ce2O2S-Structure Type
Authors: Cordier Gerhard , Schäfer Herbert
Published: March 2015

The new intermetallic compounds CaMn2Sb2, SrMn2Sb2 and CaMn2Bi2 have been prepared and structurally characterized. They are isotypic and crystallize trigonal in the anti-Ce2O2S-structure with the lattice constants:

CaMn2Sb2: a = 4.54(1), c = 7.48(1), c/a = 1.65.

SrMn2Sb2: a = 4.56(1), c = 7.70(1), c/a = 1.69.

CaMn2Bi2: a = 4.63(1), c = 7.64(1), c/a = 1.65.
Specific Rate Constants of Hydroxyl Radical and Hydrated Electron Reactions Determined by the RCL Method
Authors: Prütz W. A. , Vogel S.
Published: March 2015

Relative rate constants of OH radical and eaq
- reactions have been determined by comparing, under steady x-irradiation, the effect of various solutes upon the radiationinduced chemiluminescence (RCL) of aqueous dye (DH) solutions, [DH + ·OH] + eaq
- → DH* + OH-. The results abundantly confirm other published data. RCL changes upon addition of phosphates indicate prototropic reactions with the oxidized dye, D·+ H2PO4
- ⇌ DH·+ + HPO4
2-, promoting or inhibiting the formation of semioxidized dye (DH·+) as the most efficient RCL precursor. The RCL enhancement commonly observed upon addition of halides and pseudo halides is discussed at some length on the base of previous and present results in order to focus attention to the possible correlation between such RCL enhancement and the effect of halogen-sensitization in radiobiology. RCL results suggest that the halide transients formed from OH radicals, X- + ·OH → X· + OH-, are very powerful oxidizing agents reacting with aromatics by electron-abstraction rather than by addition or H-abstraction. The common application of I- and SCN- as competitors for the estimation of OH radical reactivities is being commented in the context
Zur Reaktivität von C=N-Doppelbindungssystemen, X Synthesen von kondensierten Heterocyclen. / The Reactivity of C=N-Double Bond Systems, Χ Synthesis of Condensed Heterocycles
Authors: Wolfbeis Otto S. , Ziegler Erich
Published: March 2015

The combined action of orthoformate and aniline upon cyclohexanedione-1,3 yields anilinomethylene-cyclohexanedione-1,3, which react with cyanoacetate or malodinitrile in DMF in the presence of KOH to give ethyl-1-phenyl-2,5-dioxo-1,2,5,6,7,8-hexahydroquinoline-3-carboxylates (or -carbonitrils)
Mössbauer Spectra of Substituted Pentacyanoferrates(II) Containing Monoprotonated Diamines or Nitrogenated Heterocycles
Authors: Aymonino Pedro J. , Blesa Miguel A. , Olabe José A. , Frank Enrique
Published: March 2015

Mössbauer parameters (IS and NQS) for a series of hydrated sodium pentacyano-L ferrates(II) (L = monoprotonated diamines or nitrogenated heterocycles) are presented. Results are discussed in terms of electronic properties of the ligands. A tentative distinction between σ-and π-bonding effects is shown and comparisons are made with previous results reported for related substances
Notizen: Elektrovalente temarnäre Phasen des Natriums bzw. Kaliums mit 2 B- und 5 B-Elementen / Ternary Phases of Sodium or Potassium with Elements of the 2 b- and 5 b-Group
Authors: Kahlert Holger , Schuster Hans-Uwe
Published: March 2015

In the systems Na(K)-Zn(Cd)-As(Sb) we found the following phases: NaZnAs, NaZnSb,

KCdAs, KCdSb (tetragonal symmetry);

KZnAs, KZnSb (hexagonal symmetry);

NaCdAs, NaCdSb (orthorhombic symmetry)
Notizen: Bildung eines Derivats von 1-Aza-8-sila-bicyclo [4.2.0] oktan unter C-H-Spaltung. / Formation of 1-Aza-8-sila-bicyclo[4,2,0]octane under Cleavage of a C-Η Bond
Authors: Klingebiel U. , Meller A.
Published: March 2015

The reaction of tert-butylamino-fluoro-phenyl -tetramethylpiperidino-silane and butyllithium takes places under LiF- and C4H10-elimination. The proton, required for the formation of butane, is not transferred from the amino but from one of the methyl substituents of the piperidino ring under formation of a bicyclic structure
Notizen: NdI2-II, eine metallisch leitende Hochdruckmodifikation ? / NdI2, a Metallic High Pressure Modification ?
Authors: Beck H. P.
Published: March 2015

NdI2, which crystallizes in the SrBr2-type arrangement, has been transformed into a high pressure modification having the same MoSi2-type structure as the metallic diiodides of La, Ce and Pr
Darstellung und Kristallstruktur von Ca3Al2Ge2, Sr3Al2Ge2 und Ba3Al2Ge2 / Preparation and Crystal Structure of Ca3Al2Ge2, Sr3Al2Ge2 and Ba3Αl2Ge2
Authors: Widera Axel , Eisenmann Brigitte , Schäfer Herbert , Turban Karlheinz
Published: March 2015

Ca3Al2Ge2, Sr3Al2Ge2 and Ba3Al2Ge2 have been prepared and their structures determined. They crystallize orthorhombicly in an ordered variant of the Ta3B4 structure type with the following constants :

Ca3Al2Ge2: a = 4.08(1) Å, b = 18.54(2) Å, c = 4.58(1) A,

Sr3Al2Ge2: a = 4.22(1) Å, b = 19.21(2) Å, c = 4.86(1) A,

Ba3Al2Ge2: a = 4.34(1) A, b = 19.82(2) Å, c = 5.09(1) A.
Isomere und tautomere Formen substituierter 1.5-Diphenyl-3-phenylcarbamoylformazane / Isomeric and Tautomeric Forms of Substituted 1,5-Diphenyl-3-phenylcarbamoylformazanes
Authors: Kettrup Antonius , Grote Manfred
Published: March 2015

The coupling of aryldiazonium salts to malonanilic acid gives formazanes with a phenylcarbamoyl group attached to the C-atom. One of these compounds has been 15N-labelled. IR and NMR spectroscopic investigations show that the formazanes exist in the solid state and in solution as mono- and bischelated isomers.

The influence of solvents on the rate of isomers and on the chemical shifts has been examined. Approximately linear relationships are given between the δ-values of NH-protons, parameters ET and Hammett σ-values.
Notizen: Zur Kenntnis von Bi2PdO4 / About Bi2PdO4
Authors: Arpe R. , Müller-Buschbaum Hk.
Published: March 2015

Bi2PdO4 was prepared and investigated by X-ray single crystal methods (a = 862.3; c = 590.9 pm, space group C4V
10—I4 cm). It shows isolated coplanar oxygen polyhedra around Pd2+ with an identical construction to that of Bi2CuO4.
Notizen: Darstellung von Siliziumhomologen der “Methylidyn-Cluster” / Preparation of Silicon Homologues of the “Methylidyneclusters”
Authors: Haustein Hans J. , Schwarzhans Karl E.
Published: March 2015

Silicon homologues of the methylidyneclusters have been prepared. The configuration of these complexes has been derived by IR and mass spectrometric measurements.
Die Kristall- und Molekülstruktur von Tetrapyridin-di-(dijodthiocyanato)-kobalt(II), [Co(py)4(NCS · I2)2] / Crystal and Molecular Structure of Tetrapyridine-di-(diiodothiocyanato)-cobalt(II), [Co(py)4(NCS · I2)2]
Authors: Hartl Hans , Steidl Sigrid
Published: March 2015

Co(py)4(NCS · I2)2 crystallizes in the triclinic space group P1̅ with a = 10.556(4) Å, b= 9.630(4) A, c = 8.897(3) Å, α = 89.28(4)°, β = 100.51(4)°, γ = 122.51(3)° and Ζ = 1. The thiocyanate ions act as bidentate ligands with N coordinated to Co(py)42+ and S forming a C. T. bond to I2. The compound can be considered as a Co complex with the “pseudotrihalide anion” [NCS · I2]- as ligand.
Photochemische Telomerisation von Äthylen mit Malonsäurediäthylester / Photochemical Telomerization of Ethylene with Malonic Acid Diethylester
Authors: Kaefer P. , Saus A. , Dederichs B.
Published: March 2015

Under the influence of UV light (HPK 125, Philips) and in presence of diethylketone, benzophenone or acetophenone ethylene and malonic acid diethylester telomerize to give even-numbered n-alkyl-n-butylmalonic acid diethyl esters, which are formed by an 1,5-rearrangement. Low pressure of ethylene favours the rearrangement reaction and the production of short-chained telomers. High concentration of the forementioned ketones effects the reversibility of Η-abstraction, which leads to low overall yields, high yields of n-butylmalonic acid diethylester and low yields of telomers produced by rearrangement reactions. The reversibility of the Η-abstraction depends upon the applicated ketone.
Notizen: Spiro-bi-[1.1-dioxo-2.4-bis(trimethylsilyl)-1λ62,4,3-thiadiazasiletidin], ein neues Spirosilazan / Spiro-bi- [1,1-dioxo-2,4-bis(trimethylsilyl)-1λ62,4,3-thiadiazasiletidin], a New Spirosilazane
Authors: Appel Rolf , Montenarh Mathias
Published: March 2015

N, N, N′, N′ - Tetrakis [ trimethylsilyl] sulfamide (1) or dilithium-N,N′-bis[trimethylsilyl]sulfamide reacts with tetrachlorosilane to give the spirosilazane (3).
Notizen: Eine Synthese von Fucoserraten, dem Gametenlockstoff der Braunalge / Fucus serratus L. / A Synthesis of Fucoserraten, the Female Sex Attractant of Fucus Serratus L.
Authors: Wiedenmann Brigitte , Hopf Henning
Published: March 2015

1,3-trans, 5-cis-Octatrien (1, Fucoserraten) is prepared by a novel three-step-sequence starting from the readily available 1,5-hexadiyne (7).
Über Oxocuprate, XX Ein Erdalkalioxocuprat(II) mit geschlossenen Baugruppen: BaCuO2 / About Oxocuprates, XX Alkaline-earth Oxocuprate(II) with Closed Structural Groups : BaCuO2
Authors: Kipka R. , Müller-Buschbaum Hk.
Published: March 2015

The new alkaline-earth oxocuprate(II) BaCuO2 was prepared and investigated by single crystal X-ray methods. (Space group : Oh
9-Im 3 m, lattice constant: a = 1827 pm.) The distribution of 360 atoms per unit cell leads to a complicated polyhedral framework with Cu2+ in well known square coordination. One of the Ba2+ positions has the extraordinary coordination number 24.
N-Trimethylgermyl-triorganophosphinimine / N-Trimethylgermyl Triorganophosphine Imines
Authors: Wolfsberger Werner
Published: March 2015

A series of N-trimethylgermyl triorganophosphine imines have been prepared by three different routes, (1) from tertiary phosphines and trimethylgermyl azide, (2) from triorganophosphine imines and trimethylgermyl chloride and (3) by methylation of N-trichlorogermyl phosphine imines. With one exception all phosphine imines react with trimethylaluminium to yield 1/1-adducts. The new compounds were characterized by elemental analyses, molecular weight determinations, IR and 1H and 31P NMR spectra.
Preparation and Properties of Some Mixed Amino-hydrazino-boranes
Authors: Christmas B. K. , Niedenzu K.
Published: March 2015

The three compounds N-2-(1,3-dimethyl-1,3,2-diazaboracyclopentyl)-N′,N′-dimethylhydrazine, (-CH2-NCH3-)2B-NH-N(CH3)2,N,N-bis-2-(1,3-dimethyl-1,3,2-diazaboracyclopentyl) -N′,N′-dimethylhydrazine, [(-CH2-NCH3-)2B]2N-N(CH3)2, and N,N′-bis-2-(1,3-dimethyl-1,3,2-diazaboracyclopentyl)hydrazine,

(-CH2-NCH3-)2B-NH-NH-B (-NCH3-CH2-)2,

have been synthesized and characterized. The compounds can be viewed as mixed aminohydrazino-boranes; they exhibit relatively high chemical and thermal stability which appears to be due to the incorporation of the boron into the heterocyclic system.
Notizen: Phosphazenylcyclophosphazene Syntheses Using Silylmonophosphazenes ,
Authors: Dahmann Dirk , Rose Hans , Shaw Robert A.
Published: March 2015

The reactions of the halogenocyclotriphosphazatrienes N3P3Fe6 and N3P3Cl6 with the reagentsMe3SiR [R = NP(NMe2)3, NPMe3, NPMe2Ph, NPMePh2, NPPh3, and NP(OEt)3] are discussed, and conclusions are drawn about some of the factors controlling the course and rate of these reactions. Some novel phosphazenyl-derivatives, N3P3X5R [X = F or Cl, R = NP(NMe2)3; X = F, R = NP(OEt)3] are reported.
Darstellung und Reaktionen des Tetramethylammonium-4.6-dimethyl-1.3.3.5.5-pentaoxo-1 λ63 λ65 λ62,4,6-perhydrotrithiatriazin-1-olats / Preparation and Reactions of Tetramethylammonium-4,6-dimethyl-1,3,3,5,5-pentaoxo-1 λ6, 3 λ6, 5 λ6,2,4,6-perhydrotrithiatriazin- 1 -olat
Authors: Wagner Diec-Lang , Wagner Hartmut , Glemser Oskar
Published: March 2015

Reaction of 2,4,6-trimethyl-1,1,3,3,5,5-hexaoxo-1 λ6-,3 λ6-,5 λ6-,2,4,6-perhydrotrithiatriazin, (CH3NSO2)3 (2), with trimethylamin forms a tetramethylammonium salt

N(CH3)4⁺[(CH3NSO2)2(NSO2)]- (3).

From 3 a silver-salt can be obtained which reacts with ethyl-iodide to form a mixed alkylated covalent derivative of 2.
MICHAEL Condensation Reactivity of 2-Cinnamoyl-5,6,7,8-tetrahydronaphthalene towards Acetylacetone, Ethyl Acetoacetate, Cyclohexanone and Malononitrile
Authors: Zoorob H. H. , Michael J. M.
Published: March 2015

The reactivity of 2-cinnamoyl-5,6,7,8-tetrahydronaphthalene (1) towards MICHAEL condensation with acetylacetone, ethyl acetoacetate, cyclohexanone and malononitrile were studied. Also, the reaction of hydrazine hydrate, phenylhydrazine, hydroxylamine, with 2 were accomplished. Moreover, cyclization of 9 and 11 were performed.
A Convenient Route to N-Acetyl-D-glucosamine-2-C-d and N-Acetyl-D-mannosamine-2-C-d
Authors: Szilágyi L. , Herczegh P. , Bujtás Gy.
Published: March 2015

Title compounds were prepared through epimerisation of 2-acetamido-2-deoxy-D-glucose in NaOD. The isotopic purity of the products was determined by NMR and mass spectroscopy. The mechanism of epimerisation is briefly discussed.
Preparation of Triacetoneamine, II
Authors: Sosnovsky G. , Konieczny M.
Published: March 2015

The preparation of triacetoneamine (1) by the condensation of acetone with ammonia in the presence of calcium chloride is investigated. The progress of the reaction is monitored by gas chromatography. The effects of added ammonium chloride, the total amount of ammonia introduced, and the temperature of the reaction on the weight yield and purity of 1 are investigated. The optimized conditions for the preparation of 1 at 59 °C are described.
Notizen: Das IR-Spektrum von Scandium-Orthovanadat / IR Spectrum of Scandium Orthovanadate
Authors: Escobar Marta E. , Baran Enrique J.
Published: March 2015

The infrared spectrum of ScVO4 is reported and discussed in comparison with those of YVO4 and of the lighter lanthanide orthovanadates. In order to facilitate the vibrational assignment the spectra of a series of solid solutions of the type Sc(VO4)1-n(PO4)n are also measured and analyzed.
Metal Complexes with Biologically Active Substituted Hydroxy Compounds
Authors: Singh D. , Singh H. B.
Published: March 2015

The synthesis of Cu(II), Mn(II), Fe(III), Ti(IV), Zr(IV), Ce(IV), Th(IV) and UO2(II) complexes with 4-methyldaphnetin and 4-methylesculetin is described. Structural information on coordination of the ligand with metals has been obtained from infrared spectroscopy. Results of thermal analysis and magnetic measurements of some of these complexes are reported.
Organic Reaction Schemes and General Reaction-Matrix Types, II Basic Types of Synthetic Transformations
Authors: Bart Jan C. J. , Garagnani Enea
Published: March 2015

Organic synthetic transformations are described in terms of a set of 43 distinct general reaction-matrix types, of which ten account for rearrangement reactions only. The schemes identified conform partially to the semi-empirical rules governing synthetic transformations, as previously defined by UGI et al. 30.
Organic Reaction Schemes and General Reaction-Matrix Types, III A Quantitative Analysis
Authors: Garagnani Enea , Bart Jan C. J.
Published: March 2015

A specialized set consisting of about 1,900 organic reactions has been analyzed to determine the distribution of reaction matrices R̃ according to a mathematical model of chemistry. The dynamical properties of the data-base have a very uneven (exponential) distribution. The results conform to the overall pattern of previous more restricted random sample analyses. A subset of ten R̃-matrices accounts for over 92% of the one-step interconversions between chemically stable or well-defined species which describe a reaction sequence. The implications of the findings for synthesis-planning are set out.
Notizen: Die Struktur des β-NaSn / The Crystal Structure of β-NaSn
Authors: Müller Wiking , Volk Klaus
Published: March 2015

The crystal structure of β-NaSn (low temperature modification) has been determined. It crystallizes tetragonally, a= 1046 ± 2, c = 1739 ± 3 pm, isotypic with NaPb. The short distance between Sn-atoms of different Sn4-groups is discussed.
Notizen: Methylhydrazinderivate des Phenoxythioxophosphoryldichlorids / Methylhydrazine Derivatives of Phenoxythioxophosphoryl Dichloride
Authors: Engelhardt Udo , Merrem Hans-Joachim
Published: March 2015

PhOP(S)Cl2 reacts with methylhydrazine to give three dihydrazido derivatives. The NMR and IR Data are given. By the further reaction with PhOP(S)Cl2 2,5-dimethyl-1,4-diphenoxy-1,4-dithioxo-2,3,5,6-tetraza-1,4-diphosphacyclohexane is obtained.
Notizen: Darstellung von Halogensulfensäurederivaten des räumlich anspruchsvollen 2.2.6.6-Tetramethylpiperidins / Synthesis of Halogen Sulfenic Acid Derivatives of the Bulky 2,2,6,6-Tetramethylpiperidine
Authors: Röschenthaler Gerd-Volker , Starke Roswitha
Published: March 2015

Chloro- and bromosulfenic acid 2,2,6,6-tetramethylpiperidides were obtained by S–S bond cleavage of the corresponding disulfide with chlorine or bromine. Fluorination of the chlorosulfenic acid amide with cesium fluoride yielded the fluoro derivative.
Synthese und Eigenschaften von Rhenium-Komplexen mit N2-, N2H2-, N2H4- und NH3-Liganden / Synthesis and Properties of Rhenium Complexes with N2, N2H2, N2H4 and NH3 Ligands
Authors: Sellmann D. , Kleinschmidt E.
Published: March 2015

UV irradiation of C5H5Re(CO)3 in tetrahydrofuran (THF) yields the THF complex C5H5Re(CO)2THF and traces of [(C5H5)2Re2(CO)5]. C5H5Re(CO)2THF is stable at room temperature, its reaction with N2/100 bar yields C5H5Re(CO)2N2, which also forms in the reaction with N2O whereby the THF complex is partially oxidized and decomposed. The reaction with an excess of N2H4 yields C5H5Re(CO)2N2H4, the oxidation of which leads to C5H5Re(CO)2N2 and the by-product trans-N2H2[C5H5Re(CO)2]2, in which the under ambient conditions unstable HN=NH molecule could be stabilized in a rhenium complex for the first time. In contrast to the analogous manganese complex C5H5Re(CO)2N2H4 disproportionates easily to C5H5Re(CO)2N2 and C5H5Re(CO)2NH3 at room temperature; the NH3 complex can be synthesized directly only by irradiating C5H5Re(CO)3 in hexane in the presence of NH3. The complexes are characterized spectroscopically and by elemental analyses; the different electronic influence of the nitrogen ligands on the C5H5Re(CO)2 system is discussed.
Notizen: Zur Darstellung und Kristallstruktur von Ba2MnTe3 / Preparation and Crystal Structure of Ba2MnTe3
Authors: Matje Peter , Müller Wiking , Schäfer Herbbert
Published: March 2015

Ba2MnTe3 has been prepared and analytically and structurally characterized. It crystallizes orthorhombic with a = 972(2) pm, b = 473(1) pm, c = 1898(4) pm, Pnma and is isotypic to Ba2MnS3 and Ba2MnSe3.
Notizen: Structures, Energies, and Reactivities of Bridgehead Olefins
Authors: Ermer Otto
Published: March 2015

Force field calculations of a series of bridgehead olefins give nonplanar double bond deformation energies which are correlated with chemical stability (reactivity) properties. Minimum potential energies allow an interpretation of experimental relative yields of isomeric bridgehead olefins with the same carbon skeleton. Pyramidal distortions (outof-plane bending) at the sp 2-carbon atoms are often found to contribute more prominently to the non-planar double bond deformations than pure twisting. Qualitative rules proposed in the past as to reactivity, thermodynamic stability, and structure of bridgehead olefins do not always agree with the computational results.
Vier- und fünfgliedrige Phosphorheterocyclen, XVIII [1.3.2.4]Diazadiphospheto[2.1-b : 4.3-b]bis[1.3.4.25λ]oxadiazaphosphole / Four- and Five-Membered Phosphorus Heterocycles, XVIII [1,3,2,4] Diazadiphospheto [2,1-b : 4,3-b′]bis[1,3,4,2λ5]oxadiazaphospholes
Authors: Schmidpeter Alfred , Luber Jörg , Criegern Thomas von
Published: March 2015

The title compounds 3 a-g are obtained from acetyl- and benzoylhydrazine with PCl5, with methyl- and phenylchlorophosphoranes, and with phosphonic and thiophosphinic chlorides. The monomeric oxadiazaphosphole proposed as an intermediate has been trapped in one case by methyl isocyanate in a 2 + 2 cycloaddition.

Compounds 3 with Cl at P can undergo nucleophilic substitutions. HCl degrades 3 in a slow reaction after an initial addition to the intact tricyclic system.
Darstellung und Eigenschaften des Tetrabutylammonium-iso-oktamolybdats [N(C4H9)4] 4Mo8O26 / Preparation and Properties of Tetrabutylammonium iso-octamolybdate [N(C4H9)4]4Mo8O26
Authors: Fuchs Joachim , Brüdgam Irene
Published: March 2015

From weakly acidified solutions of sodium molybdate by addition of tetrabutylammonium ions an iso-octamolybdate [N(C4H9)4]4Mo8 O26 is formed whose anion has a structure different from the known alkali or ammonium octamolybdates. Single crystals are obtainable by reaction in organic solvents. The IR and Raman spectra are presented. The decomposition of the anion by aging in dichloroethane in solution was investigated by UV spectroscopy. This study offers new aspects concerning the mechanism of polymolybdate ion formation.
Neue Spirogermasilazan-Systeme / Novel Spiro Germasilazane Systems
Authors: Wannagat Ulrich , Seifert Reinhard , Schlingmann Merten
Published: March 2015

The formerly unknown spiro systems Α-E with Ge, Si, N and O in the framework could be synthesized by reactions 1-6 and confirmed in their structure by elemental analysis, NMR, IR and Raman spectra (Tables I-IV).
Nachweis der Atropisomerie peri-substituierter Naphthalin-Derivate durch dynamische 1H-NMR-Spektroskopie / Dynamic 1H-NMR-Spectroscopic Evidence for the Atropisomerism of Perisubstituted Naphthalene Derivatives
Authors: Luckenbach Reiner , Jensen Axel
Published: March 2015

The preparation of the perisubstituted naphthalene derivatives 1-8 is described for the first time, and possible axial or axial and planar chirality of these compounds is investigated by means of dynamic 1H NMR spectroscopy. Molecular chirality, caused by hindered rotation, can be proven for compounds 1 and 3 at room temperature and for 2 at 193 K by the observation of magnetic inequivalence of isochronous protons in a diastereotopic environment. Temperature-dependent 1H NMR spectra indicate that for 2 the coalescence temperature lies between 193 K and 213 K, and above 320 K for 3. By assuming Tcoal- = 200 K for 2 and Tcoal. > 320 K for 3 the following ⊿G≠-values were estimated with the aid of known approximations from the 1H NMR spectral parameters Δν = νA-νB and JAB for the methylene and methyl groups of the oxazoline system present in these species: ⊿G≠ (2) = 10.1 kcal/mole (at 200 K), ⊿G≠ (3) = 17.3 (16.2) kcal/mole (at 320 K). These ⊿G≠-values represent the energy barriers of a dynamic intramolecular process, presumably according to a more or less hindered rotation in the purely axially chiral molecules 2 and 3. With the aid of these ⊿G≠-values and model considerations a description of the energy profile diagram of the hindered rotation in compounds 2 and 8 is attempted.
The Synthesis of Dimethylchlorflavonin
Authors: Ahmad Saboor , Razaq Shamim
Published: March 2015

The first synthesis of dimethylchlorflavonin (1; R = R′= CH3), a derivative of naturally occurring rare fungal flavonoid chlorflavonin (1; R = R′= H) has been achieved.
Mikrobielle Produkte, I NMR-Spektren von Nocardamin und Massenspektrum des Tri-O-methyl-nocardamins / Microbiological Products, I NMR Spectra of Nocardamine and Mass Spectra of Tri-O-methyl-nocardamine
Authors: Maehr Hubert , Benz Wolfgang , Smallheer Joanne , Williams Thomas H.
Published: March 2015

Nocardamine was isolated from an unidentified Streptomyces, species X-14568, and its 1H NMR and 13C NMR spectra are assigned in detail. Reaction with iodomethane and silver oxide converts nocardamine to the tri-O-methyl ether which is a suitable derivative for electron-impact mass spectrometry. Fragmentation mechanisms of tri-O-methylnocardamine are discussed.
Chemical Reactivity of 2-Thiohydantoin Derivatives
Authors: Shalaby A. F. A. , Daboun H. A. , Abdel Aziz M. A.
Published: March 2015

Treatment of 5-arylazo-2-thiohydantoins (2 a-c) with formaldehyde and the appropriate amine in ethyl alcohol led to the formation of the corresponding Mannich bases 3a-i. 2 a-c reacted with methyl bromoacetate and/or chloroacetic acid to give the esters 5 a-c and/or the free acids 5d-f, respectively. 5e also obtained by treating 5 b with aqueous sodium hydroxide (2%). 5 a-c were cyclised with acetic anhydride to give the bicyclic products 6 a-c. 5-Arylidene-2-thiohydantoins (7 a-e) reacted with acrylonitrile in pyridine to give 5-arylidene-3-β-cyano-ethyl-2-thiohydantoins (8a-e). 8 a-c were hydrolysed with a mixture of acetic-hydrochloric acid to give the corresponding acids 8f-h. Compounds 8a, b, d were alkylated with alkyl halides to give 10 a-e which when hydrolysed with acids gave compounds 13 a-c.
Mössbauer-Spektroskopische Untersuchungen an der high/low spin Eisen(II)-Verbindung Cs2FeHFeL(CN)6 / Mössbauer Spectroscopic Investigation of the High/Low Spin Iron(II) Compound Cs2FeHFeL(CN)6
Authors: Griebler W. D. , Pebler J. , Schmidt K. , Babel D.
Published: March 2015

By Mössbauer spectroscopy the cubic compound CsFe(CN)3, α = 5.208 Å, is shown to contain high and low spin iron(II) in 1:1 proportion independant of temperature 4.2 ≦ T ≦ 600 K. This gives evidence of isomorphism with the elpasolite Cs2MgFe(CN)6. The quadrupol splitting of the high spin iron(II) spectra strongly depends on temperature and vanishes beyond 400 K. This behaviour is interpreted in terms of static Jahn Teller distortion in the low temperature range, also indicated by the splitting of the IR absorption associated with the Fe-N stretching frequency.

The data of Mössbauer and IR spectra, as well as of magnetic susceptibility measurements are given and discussed.
Verbesserte Synthesen von Vanadocenen und Chromocenen / Improved Syntheses of Vanadocenes and Chromocenes
Authors: Köhler Frank H. , Prössdorf Wolfram
Published: March 2015

In order to improve the poor yield of the vanadocene and chromocene syntheses VCl2 · 2 THF has been prepared by reduction of VCl3 · 3 THF with zinc and CrCl2 · THF by action of hydrogen chloride on chromium. The metal(II) chlorides have been reacted with sodium methylcyclopentadienide and perdeuterocyclopentadienide to give the corresponding vanadocenes and chromocenes in yields up to 68% and 85%, respectively. The products have been characterized by paramagnetic 13C, 1H, and 2H NMR the latter being newly introduced in the class of organometallic π-radicals.
Enhydrazine, XVIII Einige weitere Indazol-Derivate / Enhydrazines, XVIII1 Further Indazol Derivatives
Authors: Sucrow Wolfgang , Fehlauer Axel , Sandmann Udo
Published: March 2015

3-(3,4-Dimethoxyphenyl)-1-methyl-1,5,6,7-tetrahydro-4H-indazol-4-one (1) is reduced to 2 a. Dehydration of 2 a gives 3 which is hydrogenated to 4 or dehydrogenated to 5. Regiospecific bromination of 1 gives the bromoketones 6 or 7, the latter is transformed into the phenol 11 a or into the indazoloquinone 13 which is brominated to 14 and converted into the aminoquinone 15.
Über die Reaktionen von Na2[M2(CO)10] (M = Cr, Mo, W) mit InX3 (X = Cl, Br, I) und über die Kristall- und Molekülstruktur von Cr(CO)5InBr · THF / On the Reactions of Na2[M2(CO)10] (M = Cr, Mo, W) with InX3 (X = Cl, Br, I), and the Crystal and Molecular Structure of Cr(CO)5InBr · THF
Authors: Behrens Helmut , Moll Matthias , Sixtus Eduard , Thiele Gerhard
Published: March 2015

The complexes (OC)5M-InX · THF are formed by the reactions of the disodium decacarbonyl dimetallates of VI b metals with InX3:

[xxx]

The structure of Cr(CO)5InBr · THF, which crystallizes in the space group Pbca-D15
2h has been determined by X-ray diffraction.
NaBeAs(Sb) – Ternäre Phasen im „aufgefüllten“ NiAs(Ni2In)-Typ / NaBeAs(Sb) – Ternary Phases in a „Filled“ NiAs(Ni2In)-Structure
Authors: Tiburtius Christoph , Schuster Hans-Uwe
Published: March 2015

NaBeAs and NaBeSb crystallize in a modified Ni2In-type-structure, space group P 63/mmc–D6h
4. Preparation and structure determination with powder and single crystal data are described. The bonds and the structure are discussed in comparison with corresponding compounds of the formula AMeIIX. The lattice constants are:

NaBeAs: α = 3,820(5), c = 8,948(9), c/α = 2,34;

NaBeSb: α = 4,144(5), c = 9,320(9), c/α = 2,25.
Homogene Olefinmetathese mit Wolfram-Germanium- und Wolfram-Zinn-Komplexakatalysatoren/ Homogeneous Metathesis of Olefins by Tungsten-Germanium and Tungsten-Tin-Catalysts
Authors: Warwel Siegfried , Laarz Wolfgang
Published: March 2015

Bimetallic tungsten-germanium and tungsten-tin compounds (e.g. π-C5H5(CO)3W-MR3; M=Ge, Sn; R=CH3, C6H5) upon activation with Cl2Al-i-C4H9/O2 (2:1) give highly active catalytic systems for the homogeneous metathesis of linear olefins with internal double bonds (2-hexene, 3-heptene, 4-octene). The activation procedure has a decisive influence on the reaction velocity and the distribution of products. Starting the reaction by addition of oxygen to the mixture of the other compounds, the metathesis leads selectively and slowly to the primary metathesis products. On the other hand the metathesis takes place rapidly if the olefin is added to the preformed catalytic system. In this case metathesis is accompanied by strong double bond isomerisation and yields broad range olefin mixtures.
Epoxide and Olefin Formation Via Arsonium Ylides
Authors: Tewabi R. S. , Gupta K. C. , Chaturvedi S. C.
Published: March 2015

Substituted methylenetriphenylarsenanes react with 2,7-disubstituted fluorenones to give exocyclic olefins, 9-arylidene-2,7-disubstituted fluorenes and/or exoxides, 2,7-disubstituted fluorene-9-spiro oxiranes. Spectral data for the resulting products were also incorporated.
Zur Kenntnis der Sulfite und Sulfithydrate des Zinks, Mangans, Magnesiums und Cobalts — Röntgenographische, spektroskopische und thermoanalytische Untersuchungen / Sulfites and Sulfite Hydrates of Zinc, Manganese, Magnesium and Cobalt-X-ray, Spectroscopic and Thermoanalytical Data
Authors: Lutz Heinz Dieter , El-Suradi Saleh M. , Engelen Bernward
Published: March 2015

IR, Raman, and X-ray data of ZnSO3 · 2½ H2O, ZnSO3 · 2 H2O, ZnSO3 ·½ H2O, ZnSO3, MnSO3 · 3 H2O, MnSO3 · H2O, MnSO3, MgSO3 · 6 H2O, MgSO3 · 3 H2O, CoSO3 · 3 H2O, CoSO3 · 2½ H2O, and CoSO3·2 H2O are presented. Except of MgSO3·6 H2O and ZnSO3 · 2½ H2O the crystal structures of these compounds are yet unknown. The following crystal data could be determined by single crystal measurements: ZnSO3 · 2 H2O (monoclinic, P21/n) : a = 642.1, b = 852.4, c = 757.4 pm, β = 98.93°, Z = 4, MnSO3 · 3 Η2Ο (monoclinic, Ρ21/n) : a = 665.0, b = 890.6, c = 879.3 pm, ß = 96.11°, Z = 4, MnSO3 · Η2Ο (orthorhombic) : a = 2565.1, b = 483.9, c = 576.0 pm, Z = 8, CoSO3 · 3 Η2Ο (orthorhombic, Pna21, isotype with MgSO3 · 3 H2O): a = 952.7, b = 942.0, c = 552.1 pm, Z = 4, CoSO3• 2½ H2O (tetragonal) : a = b = 946.4, c = 1021.1 pm, Z = 8, CoSO3 · 2 H2O (isotype with ZnSO3 · 2 H2O) : a = 639.7, b = 855.3, c = 753.7 pm, β = 98.85°, Z = 4. The IR spectra show that with exception of MnSO3· H2O strong hydrogen bonds are present in the sulfite hydrates. The decomposition of the sulfites has been examined by thermal analysis. Dehydration of the sulfite hydrates starts at 90 (ZnSO3 · 2½ H2O), 120 (ZnSO3 · 2 H2O), 175 (ZnSO3 · 1/2 H2O), 85 (MnSO3 · 3 H2O), 205 (MnSO3 · H2O), 70 (MgSO3 · 6 H2O), 130 (MgSO3 · 3 H2O), 120 (CoSO3 · 3 H2O), 140 (CoSO3 · 2½ H2O), and 150 °C (CoSO3 · 2 H2O). Decomposition of the anhydrous sulfites occurs at 300-350 (ZnSO3), 390-460 (MnSO3), and 400-530 °C (MgSO3).
Organophosphorus Compounds, XXVI * The Reaction of Diazoketones with Trialkyl Phosphites
Authors: Sidky M. M. , Soliman F. M. , Kateb A. A. El
Published: March 2015

Diazoketones 1, 8, 10 and 14 react with trialkyl phosphites to give different products depending upon the structure of the diazo compound, the type of the solvent and the nature of the phosphite ester used. Possible reaction mechanisms are discussed and the structural assignements are based on analytical, chemical and spectroscopic results.
Notizen: Zur Darstellung und Struktur von KSbSe2 / On the Preparation and Structure of KSbSe2
Authors: Dittmar Günter , Schäfer Herbert
Published: March 2015

KSbSe2, prepared by heating a mixture of the elements in a silica tube, crystallizes triclinic with the following constants

a = 1248.1(5) pm, α = 103.16(5)°,

b = 644.5(5) pm, β = 99.27(5)°,

c = 645.0(5) pm, γ = 99.44(5)°.

There are SbSe2
--chains, formed by Ψ-tri-gonal bipyramids, which are connected by sharing edges.
Über Tetraphenylphosphonium-Isopolywolframate / Tetraphenylphosphonium-Isopolytungstates
Authors: Grase Roger , Fuchs Joachim
Published: March 2015

From acidified sodium tungstate solutions mixtures of polytungstates are precipitated by addition of tetraphenylphosphonium ions. By separation with selective organic solvents five different polytungstates were obtained two of them represent a novel polyanion type. Their base to acid ratio is 2:11 respectively 1:6. The other three compounds were identified analytically and by their vibrational spectra as hexatungstate, [P(C6H5)4]2W6O19, as decatungstate, [P(C6H5)4]4Wio32, as well as dodecatungstate, [P(C6H5)4]5H3W12O40, with “Keggin-structure”.

The preparation of these compounds is reported and their IR, Raman and UV spectra are discussed.
Darstellung und Komplexverhalten von neuen Acrylsäurecopolymeren sowie deren Kopplung mit Insulin / Preparation and Complexation Behaviour of New Acrylic Acid Copolymers and their Coupling with Insulin
Authors: Biedermann Hans-G. , Eiband Manfred , Guntner Hans , Kolb Helmut
Published: March 2015

Acrylic acid copolymers with styrene, acryloylchloride, acryloylpyrrolidinone, acryloyloxypyridine, acryloylsuccinimid and acryloyltriazole are prepared and coupled with insulin.

Metal complexes with BaCl2, Cu(CH3COO)2, La(NO3)2, Pb(NO3)2 and Hg(NO3)2 of the acrylic acid acryloylpyrrolidinone and of the acrylic acid acryloylsuccinimid copolymer are formed and characterized.
Heterogene Hydrierung ungesättigter Verbindungen mit dem P-2-Ni Katalysator bei Umsatzzahlen UZ bis 90000 / Heterogeneous Hydrogenation of Unsaturated Compounds with Catalyst P-2-Ni with Turnover Numbers up to 90,000
Authors: Strohmeier Walter , Pföhler Magdalena , Steigerwald Hannelore
Published: March 2015

Unsaturated compounds are very rapidly hydrogenated with nickel-boride catalyst P-2-Ni without solvent under mild conditions (70-85 °C and 10 bar). Turnover numbers UZ up to 90,000 and space-time-yields of 7440 mmol product per 1 and 1 mgA Nickel in one hour with a mean catalyst activity ā = 124 were observed. This hydrogenation catalyst has a power, which is in the same magnitude of very active noble metal catalysts.
Pyridinium Chlorochromate Oxidation of Some Steroidal Systems. Regioselective Opening of Ring ‘F’ in Spirostan*
Authors: Dhar Durga Nath , Singh Anil Kumar
Published: March 2015

The oxidation of diosgenin (1), cholesterol (2), lanosterol (8), β-sitosterol (4) and stigmasterol (5) with pyridinium chlorochromate furnished the corresponding conjugated and unconjugated ketones i.e., Δ5(6)-3-one and Δ4(5))-3-one. In the case of diosgenin (1), besides the formation of the ketones, regioselective opening of the ring F has also been observed.
Notizen: Cyclisierung von Fluor-Silyl-Hydrazinen / Cyclisation of Fluoro-Silyl-Hydrazines
Authors: Klingebiel U. , Wendenburg G. , Meller A.
Published: March 2015

Fluorosilylhydrazines react with butyllithium under substitution or cyclisation. A fivemembered heterocyclus is obtained by the intramolecular reaction of N-tert-butyl-aminodimethylsilyl - N′ - fluorodimethylsilyl-N-phenyl-N′-trimethylsilylhydrazine with butyllithium.
The Crystal Molecular Structure of the Adduct of 2,2,2-Trifluoro-4,4,5,5-tetrakis(trifluoromethyl)-l,3,2A 5 -dioxaphospholane with Trimethylphosphine. A Strong P → P Coordinate Bond
Authors: Sheldrick W. S. , Gibson J. A. , Röschenthaler G.-V.
Published: March 2015

The adduct of 2,2,2-trifluoro-4,4,5,5-tetrakis(trifluoromethyl)-1,3,2 A 5 -dioxaphospholane with trimethylphosphine crystallises in the orthorhombic space group Pbcm, Z = 4, with a - 11.018(2), b - 12.978(4), c= 11.607(2) Å at -120 °C. The perfluoropinacolyl ring system lies in a crystallographic plane of symmetry. This ring conformation and the very long endocyclic C-C bond and average C-CF3 distances of respectively 1.59(1) and 1.59(1) A are presumably a consequence of very short F···F steric contacts. The P→P bond distance of 2.234(5) is very short for a coordinate bond being only 0.01-0.03 A longer than that typically observed for a a-bond. The tr-bond lengths to the hexacoordinate phosphorus are influenced by the nature of the Zrans-bond in the octahedron.
Thermal Analysis of the Cadmium and Manganese Hydrogen Orthoarsenate Monohydrates (M HAsO4 · H2O, where M = Cd, Mn)
Authors: Nabar M. A. , Dalvi A. P.
Published: March 2015

The dehydration decomposition of cadmium and manganese hydrogen orthoarsenate monohydrates was studied by static isothermal and differential thermoanalytical methods. It was found that the dehydration decomposition takes place in a single stage forming the respective diarsenate, the peak minimum temperature being 458 K for the cadmium and 466 K for the manganese salt.