bluuebunny/crossref_metadata_2025 huggingface dataset:
Silberhalogenid-Silberchalkogenidsysteme, II Dichten geschmolzener Silberhalogenid-Silberchalkogenidmischungen / Silver Halide-Silver Chalcogenide Systems, II Densities of Liquid Silver Halide-Silver Chalcogenide Mixtures
Authors: Blachnik Roger , Alberts Johann E.
Published: March 2015

The densities of liquid mixtures in the systems AgCl-Ag2S, AgCl-Ag2Se, AgCl-Ag2Te, AgBr—Ag2Te, AgJ–Ag2Te and AgJ–Ag2S have been determined as a function of composition and temperature by a dilatometric method. The molvoluminaisotherms of the systems AgJ—Ag2S and AgJ–Ag2Te show negative deviations from ideality, the other systems behave ideally.
Pt(NH3)2(SCN)2J: Ein Platinkomplex mit gemischter Wertigkeit / Pt(NH3)2(SCN)2I: A Mixed Valence Platinum Compound
Authors: Buse K. D. , Keller H. J. , Nöthe D.
Published: March 2015

Pt(NH3)2(SCN)2 dissolved in liquid SO2 reacts with molecular iodine to yield a green lustrous solid of stoichiometry Pt(NH3)2(SCN)2I. The compound is diamagnetic in the solid state and in solution and has to be taken for a platinum(II, IV) mixed valence compound, therefore. Chemical and physical evidence so far suggest a linear chain solid with either iodide-bridged metal complex chains or metal complex stacks with parallel triiodide chains.
Notizen: A New Type of Phenylpropane from the Essential Fruit Oil of Pimpinella anisum L.
Authors: Kubeczka K.-H. , Massow F. Von , Formacek V. , Smith M. A. R.
Published: March 2015

From the essential oil of Pimpinella anisum fruits a hitherto unknown type of phenylpropane was isolated. The mass, infrared, and 13C NMR spectra indicate, that the unknown is a 2-methyl-butyric acid ester of 2-hydroxy-5-methoxy-trans-propenylbenzene.
Photodebromination of Bromothiophenes
Authors: Jeffries Alfred T. , Párkányi Cyril
Published: March 2015

UV irradiation of 2-bromothiophene or 3-bromothiophene in various organic solvents produces thiophene as one of the reaction products. The likely mechanism in the case of 2-bromothiophene involves the formation of a π-complex between the thienyl radical and the bromine atom.
Schwefelradikale S3– in Natriumtetrasulfid bei erhöhter Temperatur.
Authors: Hermann Eysel Hans , Nöthe Dietrich
Published: March 2015

Raman EPR and visible absorption spectra of sodium tetrasulfide in the solid state and melts have been studied from room temperature up to 300°C. The above techniques provide strong evidence for breaking of the polysulfide chains resulting in the production of S3-radical ions. The existence of the radical ions in polysulfides at elevated temperatures is important for understanding the electrode processes in sodium sulfur batteries.
Zur Kenntnis der Organophosphorverbindungen, XVI Vinyl-aryldithiophosphinsäuren und einige ihrer Derivate.
Authors: Kuchen Wilhelm , Keck Helmut
Published: March 2015

Vinylaryldithiophosphinic acids RR′P(S)SH (R = vinyl; R′ = p-methoxyphenyl, p-ethoxyphenyl) were obtained as NH4-salts from the reaction of aryldithiophosphonic anhydride with CH2=CHMgBr. Alkali hydrolysis of the methylester RR′P(S)SCH3 (R′ = p-methoxyphenyl) gave β-methylnercaptoethyl-p-methoxyphenylthiophosphinic acid.
Metallkomplexe der Phosphinsäuren, XI. Metallvinylaryldithiophosphinate und polymere Komplexe polyfunktioneller Dithiophosphinsäuren 2.
Authors: Kuchen Wilhelm , Keck Helmut
Published: March 2015

Preparation and properties of several metal vinylaryldithiophosphinates (CH2=CH)RPS2M/n (R: p-methoxyphenyl; p-ethoxyphenyl) are reported. Copolymerisation of the ammonium salt (CH2=CH)RP(S)SNH4 (R = p- ethoxyphenyl) with methacrylic methylester gave polymers (M∼10,000) which acted as polyfunctional ligands thus giving soluble polymeric metal complexes (M ∼17,000) with Ni(II) and Co(II).
Notizen: Crystal Data of Cs2[Pt(CN)4] · H2O
Authors: Otto H. H. , Holzapfel W. , Yersin H. , Gliemann G.
Published: March 2015

Cs2[Pt(CN)4] · H2O is hexagonal with lattice constants α0 = 9.687(2) and c0 = 19.336(6) Å; the probable space groups are C6
2-P61 or C6
3-P65. The observed density yielded 3.67(4) g/cm3 and the calculated one 3.697 g/cm3 for two formula units per unit cell. X-ray powder data are given. The [Pt(CN)4]2- groups do not lie one above the other but form a helix along the c-axis.
Oxofluoro-oxalato-vanadate des vierwertigen Vanadins: Schwingungsspektrum und Struktur von Na3[VOF(C2O4)2] • 6 H2O.
Authors: Rieskamp Helmut , Mattes Rainer
Published: March 2015

The Na and NH4 salts of the [VOF(C2O4)2]3--ion have been prepared. The crystal structure of the former has been determined from X-ray diffractometer data. The crystals are triclinic, space group P

with Z = 2. The structure was solved by `direct methods' and refined to R 0.050 for 1749 reflections. In the anion, vanadium(IV) is octahedrally coordinated by a terminal oxygen atom, a fluorine atom in cis-position to the former, and two bidentate oxalate ligands. The terminal V—O-bond exhibits a strong ‘trans’ effect.
Oxotetrafluoro-vanadate(V): Die Kristallstruktur von [enH2] [VOF4(H2O)]2.
Authors: Rieskamp Helmut , Mattes Rainer
Published: March 2015

The crystal structure of [enH2][VOF4(H2O)]2 has been determined from X-ray diffractometer data. Crystals are monoclinic, space group C2/c with Z = 4 in a unit cell of dimensions a = 16.576(13), b = 7.781(4), c = 10.338(8) Å, β = 120.0(1)°.

The structure was refined by least-squares methods to R 0.053 for 1436 reflections. The structure contains monomeric [VOF4(H2O)]⁻-ions with the oxygen atoms in trans position. The bond distances are 1.577 Å (terminal oxygen) and 2.333 Å (H2O molecule), resp. The V–F distances vary between 1.769(2) and 1.858(2) Å for fluorine atoms involved in strong hydrogen bonds.
Gamma Radiolysis of Aerated Aqueous Solution of Cytosine, III.
Authors: Polverelli M. , Teoule R.
Published: March 2015

In gamma-irradiation of cytosine in aerated aqueous solution, two new radiolysis products were isolated and identified: 1-carbamoyl-5-hydroxyhydantoin and N-formylbiuret. This formation involves ring cleavage between C4 and C5 and belongs to the nondeamination pathway.
2 H-Pyrrolenin-N-oxid und N-Hydroxy-pyrrol.
Authors: Kreher Richard , Pawelczyk Hubert
Published: March 2015

Dehydrogenation of N-hydroxy-Δ3-pyrroline with mercuric oxide leads via the cyclic conjugated 2 H-pyrrolenine-N-oxide to the tautomeric N-hydroxy-pyrrole, which has pronounced reactivity towards dienophiles. With N-phenyl-maleic-imide the endoconfigurated Diels-Alder-adduct is formed, whose stability is increased by acylation of the N-hydroxy group. The O-acylated Diels-Alder adducts can be prepared independantly from N-acyloxy-pyrroles and the corresponding dienophile.
Dissociation Constants of Some Hydroxamic Acids
Authors: Agrawal Y. K.
Published: March 2015

The hydroxamic acids are useful chelating agents for inorganic and organic analysis. For their rational application the data on dissociation constants are desirable. In the present communication the thermodynamic dissociation constants of several hydroxamic acids have been determined at 25°C. The calculation method is described earlier1.
Notizen: Structural Studies on Polyvalent Compounds of Iodine
Authors: Prout Keith , Stevens N. Mark , Coda Alessandro , Tazzoli Vittorio , Shaw Robert A. , Demir Türsen
Published: March 2015

The structures of 1-chloro-4,5-benziodoxalin-3-one (1) and 1,2-dichloro-4,5-benziodazalin-3-one (2) have been determined by x-ray crystallography. These are compared with those of some compounds related to the former, as well as with I2Cl6. The bond of iodine to its exocyclic substituent appears to be very sensitive to environmental changes, as are the endocyclic iodine-oxygen and carbon-oxygen bonds (both where applicable) in the heterocyclic ring. The shapes of the molecules and their possible interactions with donor functions on adjacent molecules are discussed.
Notizen: Monomere Methylmetall-Diacetamidokomplexe des Galliums und Antimons / Monomeric Methyl Metal Diacetamido Complexes of Gallium and Antimony
Authors: Eberwein B. , Sille F. , Weidlein J.
Published: March 2015

The reaction of Ga(CH3)3 or Sb(CH3)5 with diacetamide leads to (CH3)2GaO2C2(CH3)2N or (CH3)4SbO2C2(CH3)2N. The behaviour, the 1H NMR and vibrational data of these covalent and monomeric compounds with an chelated O2C2(CH3)2N-ligand are discussed.
Über den Mechanismus der Bildung von Polyanionen in wäßriger Lösung. Zum Bildungsmechanismus eines Polytetramolybdations [Mo4O14
4-]n / On the Mechanism of Formation of Polyanions in Aqueous Solution. Concerning the Mechanism of Formation of a Polytetramolybdate Ion [Mo4O14
4-]n
Authors: Tytko Karl-Heinz
Published: March 2015

Possible structures and the pertinent reaction pathways for the polymetalate ion present in a slightly soluble polymetalate having the analytical formula A2O · 2 MOs have been derived on the basis of theoretical considerations. Structure and kind of combination of the tetrameric units of one of the possibilities are in agreement with the results of X-ray structure analyses. First the previously proposed planar tetrametalate ion [M4O12(OH)4]4--is formed by stepwise aggregation according to an addition mechanism. This species undergoes a rearrangement of the coordination sphere of two of the M atoms and is then subject to a polycondensation resulting in a polytetrametalate chain, [M4O14
4-]n.
Notizen: MnGa2Se4 und MnGa2Te4 / MnGa2Se4 and MnGa2Te4
Authors: Range Klaus-Jürgen , Hübner Heinz-Joachim
Published: March 2015

MnGa2Se4 and MnGa2Te4 were prepared by direct synthesis from the elements at 900-1000°C. MnGa2Se4 (Space group I 4, α = 5.676(2) Å, c = 10.760(3) Å, z = 2) is isotypic with CdGa2S4.
Notizen: Zur Strukturchemie von Übergangsmetallfluoriden ÜIIMIVF6[Ü: Cr bis Zn; M: Hf, Zr] / Preparation and Structure of Transition Metal Fluorides ÜIIMIVF6 [ÜII: Cr-Zn; MIV: Hf, Zr]
Authors: Steffens F. , Reinen D.
Published: March 2015

Compounds ÜIIMIVF6 [Ü: Mn—Ni, Zn] crystallize in the LiSbF6- or in the ordered ReO3-structure respectively. The influence of the Jahn-Teller ions Cr2+ and Cu2+ on these structure types is studied.
Über Galvinole und Galvinoxyle, III. EPR-Spektroskopie an regellos orientierten Bis-Galvinoxyl-Biradikalen in der Glasmatrix / On Galvinols and Galvinoxyls, III. EPR Study of Zero Field Splitting in Randomly Oriented Galvinoxyl Biradicals
Authors: Broser W. , Kirste B. , Kurreck H. , Reusch J. , Plato M.
Published: March 2015

ESR powder spectra of several differently bridged bis-galvinoxyl biradicals have been recorded. The spectra can be interpreted in terms of a weak electron-electron dipolar coupling between the unpaired spins of randomly oriented triplet molecules. Using MO-theory and a point charge model for atomic orbitals a detailed structural analysis is performed on the basis of quantum mechanical calculations. Taking into account the twist angles between the various aryl rings the experimental data can be explained satisfactorily.
Isomerisierungsreaktionen von cis- und trans-Dicarben-Komplexen des Typs M(CO)4L2 (M = Cr, Mo, W).
Authors: Öfele Karl , Roos Eva , Herberhold Max
Published: March 2015

A series of bis-carbene complexes cis-M(CO)4L2 (M = Cr, Mo, W) containing cyclic carbene ligands (L= 1,2-dimethyl-4-pyrazoline-3-ylidene, 1,3-dimethyl-4-imidazoline-2-ylidene, 2,4-dimethyl-1,2,4-triazoline-3-ylidene and 1,3-dimethyl-benzimidazoline-2-ylidene) was prepared, and the photo-induced conversion to the corresponding trans-isomers was investigated. The trane-M(CO)4L2 complexes were characterized by their IR and 1H NMR spectra, and their irreversible thermal isomerisation to the thermodynamically more stable cis-isomers was studied both in solution and in the solid state.
Notizen: Zur Metallverteilung in SrFe7Al5O19.
Authors: Pausch H. , Müller-Buschbaum Hk.
Published: March 2015

Single crystals of SrO - 3.5 Fe2O3 - 2.5 Al2O3 were prepared and investigated by X-ray diffraction. The atomic distribution differs from former investigations of magnetoplumbite compounds.
Die Kristallstrukturen von Tetramethylarsonium- und Tetramethylstibonium-monomethyltrichloroindat (CH3)4M+CH3InCl3
- (mit M = As, Sb).
Authors: Guder H. J. , Schwarz W. , Weidlein J. , Widler H. J. , Hausen H. D.
Published: March 2015

Tetramethylarsonium-, as well as tetramethylstibonium-monomethyltrichloroindate crystallizes in the monoclinic space-group Pc with two formula units in the cell.

In both structures we found isolated (CH3)4M+- and (CH3)InCl3
-- tetrahedra (M = As, Sb), from which the anionic one in markedly distorted. The distances between these isolated tetrahedral cations and anions are not equal.

The tetrahedrical cations and anions form double-layers.
Derivatives of cis-NPCl2(NSOCI)2 and (NPCl2)2NSOCl, V / Preparation of NPCl2(NSOPh)2 and (NPCl2)2NSOPh. Reactions of NPCl2(NSOPh)2 with Dimethylamine
Authors: Van Den Berg J. B. , De Ruiter B. , Van De Grampel J. C.
Published: March 2015

Reaction of (NPCl2)2NSOCl or (NPCl2)2NSOF with benzene in the presence of AlCl3 yields (NPCl2)2NSOPh. By the same procedure two isomeric forms of NPCl2(NSOPh)2 can be obtained from cis-NPCl2(NSOCl)2. The phenylated products were characterized by IR, mass and 31P NMR spectra.

Reactions of one of the isomers of NPCl2(NSOPh)2 with (CH3)2NH yield NPClN(CH3)2(NSOPh)2 (molar ratio 1:2) and NP[N(CH3)2]2(NSOPh)2 (molar ratio 1:6.8). The structures of the amino substituted derivatives were determined by means of 1H NMR measurements.
Notizen: Electrical Conduction in Thioxanthene
Authors: Pietra S. , Tenaglia A.
Published: March 2015

Electrical conductivity of thioxanthene single crystals has been observed. The electrons, injected from the electrodes or freed by sulphur atoms, are responsible for the electrical properties. The activation energy for the conduction is higher than in thianthrene, it depends maybe on the number of S atoms in the molecule.
Beiträge zur Chemie des Phosphors, 69 Über ein einfaches Verfahren zur Darstellung von Tri-t-butyl-cyclotriphosphan.
Authors: Baudler Marianne , Gruner Christian
Published: March 2015

A high yield synthesis of tri-t-butyl-cyclotriphosphane from magnesium and tertbutyldichlorophosphane is described.
Über Derivate des Hydrazins, VII Darstellung und Charakterisierung von Bis(trimethylsilyl)aminoisocyanid.
Authors: Wiberg Nils , Hübler Gerhard
Published: March 2015

By reaction of carbon tetrachloride with lithium tris(trimethylsilyl)hydrazide and then with lithium butyl a compound with formula (Me3Si)2N2C is formed. From the way of preparation, spectroscopic investigations, and chemical reactions the substance is characterized as bis(trimethylsilyl)aminoisocyanide (3). 3 hydrolyzes, and does not react with oxygen. The compound combines with chlorine and bromine forming aminoisocyanide dihalides, and with carbon disulfide forming an adduct. At higher temperatures 3 isomerizes to bis(trimethylsilyl)carbodiimide (1).
Einige neue kristallisierte 7.7.8.8-Tetracyanochinondimethan(TCNQ)-Verbindungen mit Tetramminplatin(II)-Dikationen als Gegenionen.
Authors: Endres H. , Keller H. J. , Moroni W. , Nöthe D.
Published: March 2015

New compounds of stoichiometry [Pt(II)L2](TCNQ)2, [Pt(II)L2](TCNQ)3 and [Pt(II)L2](TCNQ)4 (with L = one bidentate or two monodentate neutral nitrogen donor ligands like ethylenediamine (en), 1,10-phenanthroline (phen) or ammonia) have been prepared and characterized. The complexes of stoichiometry [Pt(II)L2](TCNQ)2 with only negatively charged TCNQ- units have relatively low conductivities (in the range of 10-7—10-8 Ω-1 cm-1) while the compounds [Pt(II)L2](TCNQ)3 containing one neutral TCNQ molecule per formula unit (“complex TCNQ-salts”) conduct much better (in the range of 10-2—10-3 [Ω-1 · cm-1] for pellets). Most of them show appreciable deviations from a Curie law behaviour. A sharp transition from an antiferromagnetic low temperature to a paramagnetic high temperature modification can be observed for [Pt(II)dipy2](TCNQ)2 (dipy = 2,2′-dipyridyl) at 87°C.
Synthetic Studies towards anti-Leukaemic Alkaloids, VIII
The Roads to Vinblastine
Authors: Rahman Atta-Ur , Basha Anwer , Ghazala Maryam , Waheed Nighat
Published: March 2015

Various synthetic approaches to the anti-cancer alkaloids vinblastine and vincristine are described. Methods for the generation of nine-membered nitrogen containing rings present in the indole moiety of vinblastine are discussed. Modes of joining the two moieties present in VLB in a natural configuration are presented.
Notizen: Photoreaktionen von 1-Hydroxy-1 H-benzotriazol und seiner Salze in Acetonitril.
Authors: Lüddecke Erik , Mauser Heinz , Polster Jürgen
Published: March 2015

The photoreactions of 1-hydroxy- 1 H-benzotriazole and its salts are spectrophotometrically analyzed dependent on oxygen concentration in acetonitrile. Quantum yields have been determined.
Übergangsmetallkomplexe mit N-haltigen Liganden, XI. Pentacarbonylchrom-Komplexe des s-Tetrazins und verwandte Verbindungen. / Transition Metal Complexes of N-Containing Ligands, XI. Pentacarbonylchromium Complexes of s-Tetrazine and Related Compounds
Authors: Herberhold Max , Süss-Fink Margot
Published: March 2015

Both mononuclear Cr(CO)5(C2H2N4) and binuclear [Cr(CO)5]2(C2H2N4) are formed when s-tetrazine (C2H2N4) is added to a photolysed solution of Cr(CO)6 in diethyl ether. A centrosymmetric structure is proposed for the binuclear, s-tetrazine-bridged complex [Cr(CO)5]2(C2H2N4). The corresponding molybdenum and tungsten compounds are also described
Carbon-Nitrogen Spin-Spin Coupling in Diazomethane
Authors: Runge W. , Firl J.
Published: March 2015

The one-bond carbon-nitrogen coupling constant of diazomethane is reported. Analogies with carbon-carbon coupling constants in allenes are emphasized. CNDO/S-calculations are used as a support of the suggestions the C-N coupling in diazomethane to be dominated by the Fermi contact mechanism and the sign of the carbon-nitrogen-15 coupling constant to be negative
Notizen: Über NaAg3O2. / On NaAg3O2
Authors: Jansen Martin
Published: March 2015

The new oxide NaAg3O2, which was prepared using oxygen pressures of 350 at, is isostructural to LiAg3O2: Ibam, a = 6.159, b = 10.439, c = 5.972 Å
Notizen: Die Kristallstruktur des SrAs3. / The Crystal Structure of SrAs3
Authors: Deller Klaus , Eisenmann Brigitte
Published: March 2015

The new intermetallic compound SiAs3 crystallizes monoclinic, space group C2/m (a = 9.61(1) Å, b = 7.63(1) Å, c = 5.88(1) Å, β = 112.9(1)°). The anionic part of the structure contains puckered layers of two- and threebonded As-atoms
Metallkomplexe des Dihydrazido-thiophosphorsäure-phenylesters und des Dihydrazido-thiophosphats / Metal Complexes of Dihydrazido-thiophosphoric Acid Phenylester and Dihydrazido-thiophosphate
Authors: Engelhardt Udo , Scherer Guido
Published: March 2015

Dihydrazido-thiophosphoric acid phenylester as a tridentate chelate ligand forms complexes with bivalent transition metals. The compounds [Ni(II)(L)2]Cl2, [Zn(L)2]Cl2 and [Cd(L)Cl2] are prepared and characterized by elemental analysis, IR, Raman, UV/VIS spectra and X-ray powder diagrams. The nickel possesses a slightly distorted octahedral coordination. The nickel(II) complex can be transformed to a carbon free inner complex salt of the formula [Ni(II){(NH2-NH)2Ρ(S)O-}2] by hydrolysis.
35Cl-, 75As-NQR- und 197Au-Mößbauer-Untersuchungen an Gold(I)-chlorid-Komplexen / 35Cl-, 75As-NQR- and 197Au-Mössbauer Investigations of Gold(I)-chloride Complexes
Authors: Schmidbaur H. , Koth D. , Wagner F. E.
Published: March 2015

35Cl and 75As NQR spectra have been recorded for six gold(I) chloride complexes with phosphine, arsine and sulfide ligands. Though no 197Au–NQR signals were detected, good 197Au-Mössbauer spectra could be obtained for the same compounds and some homologs. A discussion of the results has shown, that no consistent correlation is evident between the nature of the ligands and the 35Cl and 75As quadrupole coupling constants, 197Au isomeric shifts and quadrupole splittings.
Photoreaktionen 2-sulfinylsubstituierter Benzaldehydeeine neue photoinduzierte Sauerstoff-Transfer-Reaktion / Photoreactions of 2-Sulfinyl Substituted Benzaldehydes aNew Photoinduced Oxygen-Transfer Reaction
Authors: Lüdersdorf Reinhard , Praefcke Klaus
Published: March 2015

The photochemical conversion of 2-sulfinyl substituted benzaldehydes into benzoic acids in a new type of redox reaction is discribed in which a transfer of an oxygen atom, originally attached to sulphur, takes place by insertion into the C-Η bond of the aldehyde function located in ortho position. Influences of substituents at the sulfinyl group in this photoreaction which seems to be limitated to aldehydes are discussed briefly.
Notizen: Einkristalluntersuchungen von β-CaCr2O4.
Authors: Hörkner W. , Müller-Buschbaum Hk.
Published: March 2015

Single crystals of β-CaCr2O4 were prepared by solid state reaction (1300°C, 7d) of CaO-Cr2O3 mixture. The so far unknown parameters of the atomic positions show no distortion of the octahedral surrounding [Cr2O4]2- in respect to other compounds of this type.
KCu3S2, ein neues Thiocuprat / KCu3S2, a New Thiocuprate
Authors: Burschka Christian , Bronger Welf
Published: March 2015

KCu3S2 can be synthesized by fusion reactions of copper with K2CO3 and sulfur at temperatures between 780 and 850 °C. X-ray investigations on single crystals revealed its structure. The monoclinic unit cell contains four formula units, the space group is C2/m. KCu3S2 crystallizes in a layer-type structure and is isotypic with CsAg3S2.
Notizen: Pentaoxoiodate(VII)monoanion as an Intermediate in the Interconversion of Hexa- and Tetraoxoiodate(VII)monoanions in Aqueous Solution
Authors: Buist G. J. , Holloway C. J.
Published: March 2015

Results from temperature-jump relaxation measurements indicate the existence of an intermediate, the pentaoxoiodate(VII)monoanion, in the hydration-dehydration equilibrium between hexa- and tetraoxoiodate(VII)monoanions in aqueous solution. The interconversion is accompanied by a considerable reorientation of the water molecules solvating the monoanionic species, which play a crucial rôle in the mechanism of hydration and dehyd ation. This is the first definite evidence for the existence of a penta coordinated periodate species in aqueous solution.
Radiation Chemistry of Carbohydrates, X* γ-Radiolysis of Crystalline D-Glucose and D-Fructose
Authors: Dizdaroglu M. , Henneberg D. , Neuwald K. , Schomburg G. , Sonntag C. Von
Published: March 2015

α-D-Glucose and β-D-fructose were γ-irratiated in the solid (polycrystalline) state at room temperature at doses of 3.5 · 1020-4.2 · 1021 eV g-1 (dose rate 1.16 · 1018 eV g-1 min-1). Carbohydrate products containing ≤ 6 carbon atoms were identified and their G-values (in parentheses) measured.

Glucose: Dihydroxyacetone (1) (0.05), 3-deoxy-tetrose (2) (0.015), 1,4-dideoxy-2-pentulose (3) (0.05), 2,4-dideoxy-pentose (4) (0.085), 2,4-dideoxy-pentonic acid (5), 2,3-dideoxypentos-4-ulose (6) (together 0.035), threose (7), erythrulose (8), erythrose (9), erythronic acid (10) (together 0.04), 1-deoxy-2-pentulose (11) (0.005), 2-deoxy-ribose (12) (0.25), 3-deoxy-pentosulose (18) (0.02), 3,5-dideoxy-hexonic acid (14) (0.02), 2,3-dideoxy-hexonic acid (15) (0.01), arabinose (16) (0.25), ribose (17), ribonic acid (18) (together 0.02), 2-deoxy-2-C-hydroxymethyl-pentonic acid (19) (0.06), 5-deoxy-gluconic acid (20), 2deoxy-5-keto-glucose (21), 2-deoxy-gluconic acid (22), 2-deoxy-3-keto-glucose (28), 3-deoxy-glucosone (24), 3-deoxy-gluconic acid (25), 3-deoxy-4-keto-glucose (26), 3-deoxymannonic acid (27) (together 0.4). Identified but nor measured quantitatively were glucosone (28), 3-keto-glucose (29), 4-keto-glucose (30), 5-keto-glucose (31) and gluconic acid (82). G(H2) = 5.75; G(CO2) = 0.7.

Fructose: 7-9 (together 0.65), 3-deoxy-pentonic acids (37), 3-deoxy-pentosulose (88) (together 0.3), arabonic acid (89) (0.1), 18 (0.05), 6-deoxy-2,5-hexodiulose (40) (40). Identified but not measured quantitatively were glyceraldehyde (34), butanone-(3)-diol-(1,2) (35) and 2- and 3-deoxy-hexodiuloses. G(H2) = 4.75, G(CO2) = 0.05.

Reaction schemes are proposed to account for the formation of the products. The scission of the hemiacetal bond and of the C-Η and C-C bonds next to it appears to be typical for solid state irradiations. The formation of deoxy-compounds is observed both in the solid state and in aqueous solution. The formation of dideoxy-compounds is only prominent in the solid state. In polycrystalline fructose a chain reaction is induced leading to 6-deoxy-2,5-hexodiulose (40).
Elektrochemische Synthesen, XI Die anodische Reaktion verzweigter Alkane / Electrochemical Syntheses, XI The Anodic Reaction of Branched Alkanes
Authors: Fritz Heinz P. , Würminghausen Thomas
Published: March 2015

Preparative electrochemical oxidation of branched alkanes in trifluoroacetic acid yields — as function of the applied potential — mono- or bifunctionalized derivatives. Esters with rearranged skeleton (hydride or methyl shift) suggest carbenium ion intermediates. These are generated by oxidative elimination of a proton or fragmentation. A method is described to measure small differences in reactivity of alkanes.
Notizen: Ternäre Phasen in dem System Calcium-Nickel-Phosphor / Ternary Phases in the System Calcium-Nickel-Phosphorus
Authors: Mewis Albrecht
Published: March 2015

By investigations in the system Ca—Ni—P we found two ternary phases. CaNi1.95P2 crystallizes in a tetragonal lattice; a ThCr2Si2 type structure is supposed. Ca2.1Ni11.9P7 crystallizes in a hexagonal lattice.
Untersuchungen an biologisch wirksamen Ligandensystemen, XII1 Metallkomplexe des Maleinsäurehydrazids und ihre physiologische Wirkung auf Yoshida-Sarkom-Asciteszellen / Investigations of Biologically Active Ligands, XII1 Metal Complexes of Maleic Acid Hydrazide and their Physiologic Action on Yoshida-Sarcoma Ascites Cells
Authors: Fritz Heinz P. , Lippert Bernhard , Possinger Kurt , Hartenstein Reiner
Published: March 2015

The preparation and characterization of metal complexes of maleic acid hydrazide is reported, including Ca, Mn, Fe, Co, Ni, Cu, Zn and Pt-complexes, as well as the action of maleic acid hydrazide and one Pt-complex on Yoshida-ascites-sarcoma.
Stabilisierung eines Thio-oxim-Anions durch Koordination an Platin(II) / Stabilization of the Thio-oxime Anion by Coordination to Platinum(II)
Authors: Götzfried Franz , Beck Wolfgang
Published: March 2015

(Ph3P)2Pt(C2H4) reacts with bis(fluoren-9-ylidenamino)-disulfide (2) to give a stable fluorenonthio-oximato complex (3). A ketimido complex (4) results from the reaction of 2 with Pt(PPh3)4.
Gehinderte Ligandenbewegungen in Übergangsmetallkomplexen, XII1 Tricarbonyl-η6-N-carbäthoxyazepin-chrom(0), -molybdän(0) und -wolfram(0) / Hindered Ligand Motions in Transition Metal Complexes, XII Tricarbonyl-η6-N-carbethoxyazepine-chromium(0), -molybdenum(0) and -tungsten(0)
Authors: Kreiter Cornelius G. , Özkar Saim
Published: March 2015

Tricarbonyl-η6-N-carbethoxyazepine-metal(0) complexes of chromium, molybdenum and tungsten are formed, when tricarbonyl-trisacetonitrile-chromium(0), tricarbonyldiglyme-molybdenum(0) and tricarbonyl-trisacetonitrile-tungsten(0), respectively, are treated with N-carbethoxyazepine. According to the 1H and 13C NMR spectra of the N-carbethoxyazepine metal complexes two different ligand motions can be activated thermally. The carbethoxy group rotates around the C-N-bond (Δ G300
≠ = 64.6 to 66.1 kJ • mole-1) and the azepine ligand itself moves against the tricarbonyl metal groups (Δ G250≠ 45.6-52.1 kJ • mole-1).
The Phase Diagram of K3FeF6 to 35 kbar and 600 °C
Authors: Richter P. W. , Clark J. B.
Published: March 2015

The effect of pressure on the tetragonal/cubic phase transition in K3FeF6 was studied to 35 kbar. A new phase which also occurs in K3TiF6, exists over a small temperature region at low pressures. A strong possibility exists that the K3FeF6 tetragonal phase is isostructural with the corresponding phase found for the K3XF6 (X = Ln, Y) compounds.
Studies on the Mixed Ligand Complexes Involving Ligands of Biological Importance (Ni(II)/Zn(II)/Cd(II)-1,10-phenanthroline-2,2′ -bipyridyl-phenylalanine)
Authors: Malik G. S. , Singh S. P. , Tandon J. P.
Published: March 2015

pH-metric studies on the interaction of Ni(II), Zn(II) or Cd(II) with 1,10-phenanthroline (Phen) or 2,2′-bipyridyl (Bipy) in the presence of phenylalanine (Phe) indicate the formation of 1:1:1 mixed ligand chelates and their monohydroxo derivatives. The addition of Phe takes place after the combination of Phen or Bipy with the metal ion is complete. The formation constants of the resulting complexes have been determined at 30 ± 1 °C and ionic strength (µ) = 0.1 KNO3 and the ternary complexes involving Phen are found to be more stable than the corresponding complexes involving Bipy as primary ligand.
Reactions of Alloxan and Related Compounds
Authors: Said Akila , Fleita Daisy Hanna , Shinouda Hakim Grace
Published: March 2015

A detailed investigation has been carried out on the effect of alloxan, alloxanic acid and ninhydrin on the rate of disappearance of alanine in buffered aqueous solution at pH 7 and on amino acids in blood both in vitro and in vivo. The results obtained indicate the possibility that the interaction of alloxan and tissue amino acids might have an important role in the diabetogenic effect of alloxan.
Notizen: Übergangsmetall-Carbin-Komplexe, XXVIII Oxidative Abbaureaktionen von trans-Bromotetracarbonyl(phenylcarbin)chrom / Transition Metal Carbyne Complexes, XXVIII Oxidative Degradation Reactions of trans-Bromotetracarbonyl(phenylcarbyne)chromium
Authors: Fischer Ernst Otto , Ruhs Alexander , Kalder Hans Jürgen
Published: March 2015

The reaction of trans-bromotetracarbonyl-(phenylcarbyne)chromium with chlorine and bromine as well as cerium(IV) and manganese(III) compounds results in the complete degradation of the complex. Benzotrihalides or benzoic acid derivatives and, in some cases, also dibenzyl are isolated as products of the carbyne ligand.
Electronic Structure of Pseudotetrahedral Copper(II) Schiff Base Complexes
Authors: Wasson John R. , Richardson H. Wayne , Hatfield William E.
Published: March 2015

Copper(II) complexes with the Schiff bases formed by condensing t-butyl-, isopropyl-, cyclohexyl- and diphenylmethylamines with salicylaldehyde and 3-methoxy- and 5-nitrosalicyl-aldehyde have been prepared and characterized. The isotropic nuclear hyperfine coupling constants increase in the order t-butyl < isopropyl < cyclohexyl < diphenylmethyl for the N-substituents in the three series of complexes while isotropic g-values increased in the opposite direction. Spectra structure correlations were examined and discussed.
Ređuktone und Reduktonate, I Das Redoxpaar Dehydroascorbinsäure-Ascorbinsäure und ihre Anionen / Reductones and Reductonates, I The Redox Pair Dehydroascorbic Acid-Ascorbic Acid and Anions
Authors: Matusch Rudolf
Published: March 2015

On the basis of NMR spectroscopy (1H and 13C) it can be shown that in water, dimethylsulfoxide and p-dioxane only the tautomer 1 of L-ascorbic acid is found in a measurable amount. Upon formation of the mono-anion la deprotonation occurs on the hydroxyl group attached to C-3; in addition the hydroxyl group on C-2 is deprotonated in case of the di-anion 1b. Both anions do not open the lactone ring.

After oxidation with iodine in aqueous solution only the dimer of dehydroascorbic acid is detected. This is hydrolized with a half-life of three hours to the monomeric dehydro ascorbic acid dihydrate 7. In dimethylsulfoxide the oxidation rate is decreased, and therefore the formation of the monomeric non-hydratized dehydroascorbic acid 10 can be monitored. This undergoes ringclosure relatively fast to give the half-ketal 13, the reaction of which via 14 leads to the optical active dimeric dehydroascorbic acid 6. The L-ascorbic acid acetonide 15 is oxidised by iodine to 16 which undergoes racemization via the enol 17 to give 18. This forms an equilibrium with compound 19.
Notizen: Struktur und Eigenschaften des N-Salicylidenglycinato-thioharnstoffkupfer(II)-Komplexes / Structure and Properties of Salicylideneglycinato-thiourea-copper(II) Complex
Authors: Pavelčík F. , Krätsmár-Šmogrovič J.
Published: March 2015

Single crystals of [Cu(salalgly) (tu)] have been prepared. From a complete X-ray structure determination follows the square pyramidal structure of this magnetically diluted copprr(II) complex. The S-donor atom of thiourea is short bonded to the central atom, Cu ↔ S = 2.27 Å, “in plane”.
ESCA-Spektren heterocyclischer Immoniumealze / X-ray Photoelectron Spectra of Heterocyclic Immonium Salts
Authors: Knecht Josef , Klaus Hartmut , Grahn Walter
Published: March 2015

The X-ray photoelectron spectral data of a series of heterocyclic immonium salts are correlated with the CNDO/2-atomic charges of the nitrogen atoms and the molecular potential. The atomic charges of the nitrogen atoms are surprisingly close to zero.
Notizen: Übergangsmetall-Carbin-Komplexe, XXXI. Synthese von Carbonsäuren, Carbonsäureestern und Ketonen aus trans-Bromotetracarbonyl(aryl)carbinchrom und -wolfram / Transition Metal Carbyne Complexes, XXXI. Synthesis of Carboxylic Acids, Carboxylic Esters and Ketones from trans-Bromotetracarbonyl(aryl)carbyne Chromium and Tungsten
Authors: Fischer Ernst Otto , Lothar Tassilo
Published: March 2015

trans -Bromotetracarbonyl (aryl)carbyne chromium and tungsten react with KOH, NaOC2H5 and LiC6H5 to give carboxylic acids, carboxylic esters and ketones.
Hydrat und Thiohydrat des Propinals / Hydrate and Thiohydrate of Propynal
Authors: Wille Franz , Schwab Walter
Published: March 2015

Propynal (2 a) reacts with water at temperatures of about —18 °C to give a single crystallized hydrate 1 a with the structure [xxx]. It decomposes at

higher temperature into 2 a and water. No other hydrates of 2 a could be found. An analogous compound lb is obtained with H2S at about the same temperature. At room temperature it decomposes into H2S and 2 a, at higher temperatures into 3,3'-thiodiacroleine (6 a).
Übergangsmetall-Carbin-Komplexe, XXXIII1 Thermische Abspaltung von Carbinliganden aus trans-Bromotetracarbonyl(organylcarbin)chrom-Komplexen / Transition Metal Carbyne Complexes, XXXIII1 Thermal Cleavage of Carbyne Ligands from trans-Bromotetracarbonyl(organylcarbyne)chromium Complexes
Authors: Fischer Ernst Otto , Ruhs Alexander , Plabst Dieter
Published: March 2015

trans-Bromotetracarbonyl(phenyl- or -methylcarbyne)chromium react at elevated temperatures to yield tolane and dimethylacetylene, respectively. On warming trans-bromo-tetracarbonyl(phenyl- and -p-tolylcarbyne)chromium phenyl-p-tolylacetylene is formed as well as both the symmetrical alkynes tolane and di-p-tolylacetylene.
Kurzzeitpyrolyse, VI Ringverengungen durch CO-Eliminierung aus cyclischen Carbonylverbindungen / Short Time Pyrolysis, VI Ring Contractions by CO-Elimination from Cyclic Carbonyl Compounds
Authors: Schaden Gerhard
Published: March 2015

An one-step synthesis of benzocyclobutene (2) by gas-phase pyrolysis of indane-2-one (1) has been found. By the same method indane-1-one (3) and naphthoquinone(1,4) (5) gave indene-1 -one (4) and fluorene-9-one (7) formed biphenylene (8).
Correlations between the Stereochemistry and the Chemical Ionization Spectra of Epimeric 3,4-Dimethyl-1,2-cyclopentanediols
Authors: Van De Sande C. C. , Van Gaever F. , Hanselaer R. , Vandewalle M.
Published: March 2015

The eight epimeric 3,4-dimethyl-l,2-cyclopentanediols have been investigated as bistrimethylsilyl (TMS) ethers and as diacetates by means of isobutane chemical ionization (CI). Correlations between stereochemistry and CI spectra appear to be limited in the case of the TMS ethers. All eight diacetates, however, can be unequivocally identified from their isobutane CI spectra.
Titan- und zirkoniumorganische Verbindungen mit einfachen Phosphor-yliden / Titanium- and Zirconiumorganic Compounds of Simple Phosphorus Ylides
Authors: Schmidbaur Hubert , Scharf Wolfgang , Füller Hans-Joachim
Published: March 2015

TiCl4 and ZrCl4 were found to form a series of adducts with trimethyl(methylene)phosphorane, none of which is soluble in common inert solvents. With dimethylaminotitanium chlorides, a dinuclear ylide 10 was obtained, containing a dititanacyclobutane ring system, in which the metal atoms are bridged by [xxx] groups.

cp2TiCl2 and cp2ZrCl2 also form ylide adducts with (CH3)3P=CH2 in the ratio 1:2. The lithiated ylide converts both cp2TiCl2 and cp2TiCl into the cyclic ylide complex (C5H5)2Ti(CH2)2P(CH3)2 (13). With lithiated (CH3)3P=N–P(CH3)2=CH2, the related nitrido-bis-dimethylphosphoniummethylide derivative (15) could be isolated. 13 and 15 were characterized, inter alia by their ESR and mass spectra.
NMR-Untersuchungen an Organoelement(IV b)-phosphinen,IV Phosphor-Zinn-Kopplungskonstanten von Trimethylstannylphosphinen und ihren Übergangsmetallcarbonylkomplexen / NMR-studies on Organoelement(IVb)-phosphines, IV Phosphorus-Tin Coupling Constants of Trimethyltin Phosphines and their Transition Metal Carbonyl Complexes
Authors: Schumann Herbert , Kroth Heinz-Jürgen
Published: March 2015

Nuclear spin-spin coupling constants 1J (31P-117Sn) and 1J (31P-119Sn) are reported for trimethylstannyl phosphines of the type [(CH3)3Sn]3_nPRn (R = H, tC4H9, C6H5, Si(CH3)3, Ge(CH3)3; n = 0, 1, 2, 3) and for some transition metal carbonyl complexes having these phosphines as ligands. It is possible to calculate the value of1J (P-Sn) by the empirical method of increments, if there is a large number of similar compounds.
Die Kristallstruktur von B-Hexachlor-cyclotriborazan Cl6B3N3H6 / The Crystal Structure of B-Hexachloro-cyclotriborazane Cl6B3N3H6
Authors: Hess H. , Lux D. , Schwarz W.
Published: March 2015

Cl6B3N3H6 has been prepared by reaction of gaseous HCl with B-trichloroborazine in benzene. The compound crystallizes in the orthorhombic space group Pnma and four formula units in the cell. The structure was refined by least squares analysis to a R-value of 0.033. The molecules show a nearly ideal chair conformation. Interatomic distances (mean values) are: B-Cl 1.845 and B-N 1.575 Å.
Synthesis and Crystal Structure of the Hydrogen Bonded Complex of Tri-metatoluidylphosphazenyl Oxide with Bis-metatoluidine Hydrochloride
Authors: Stanley Cameron T.
Published: March 2015

The title complex was synthesised and its structure determined by x-ray crystallography. The structure contains two hydrogen bonds between the phosphoryl oxygen atom and the two meta-toluidinium ions. The P–N bond lengths are significantly different and the differences, attributed to varying p π-d π interactions along the bonds, confirm earlier observations on tri-para-toluidylphosphazenyl oxide.
Notizen: Darstellung eines 1-Aza-3.4-dioxa-2.5-diborolidins / Preparation of an 1-Aza-3,4-dioxa-2,5-diborolidin
Authors: Bablos K. , Nolle D. , Nöth H.
Published: March 2015

Bis(trimethylsilyl)peroxide was used as a reagent to prepare a novel ring system, 1-aza-3,4-dioxa-2,5-diborolidin by reaction with an appropriate diborylamine. No ring systems containing the peroxo group were obtained when oxidation predominates as shown for BBr3 and CH3BBr2.
Notizen: Darstellung und Kristallstruktur von Sr5Sn3 und Ba5Sn3 / Preparation and Crystal Structure of Sr5Sn3 and Ba5Sn3
Authors: Dörrscheidt Wolfgang , Widera Axel , Schäfer Herbert
Published: March 2015

Sr5Sn3 and Ba5Sn3 crystallize tetragonally in the Cr5B3 structure type with the following constants :

Sr5Sn3:

α = 854(1) pm, c = 1606(2) pm, c/α = 1.88,

Ba5Sn3:

α = 902(1) pm, c = 1678(2) pm, c/α = 1.86.
Notizen: Photodecomposition of 1,2-Dioxetanes
Authors: Neidland Cornelia , Stauff Joachim
Published: March 2015

Diadamantyldioxetane, trim ethyldioxetane and tetram ethyldioxetane were photolyzed b y light of A > 260 nm . The spectral distribution o f the quanta emitted during photoinduced decom position of dioxatenes was found to be different from fluorescence and phosphorescence o f ketones. Flash photolysis experim ents showed the absorption of an short-lived interm ediate. It was concluded, therefore, that photolysis o fdioxetanes is not a concerted process but involves at least one precursor o f the final product ketone.
Über Oxocuprate, XXIV Zur Kenntnis von Lu2Cu2O5 und Sc2Cu2O5 / On Oxocuprates, XXIV About Lu2Cu2O5 and Sc2Cu2O5
Authors: Freund H.-R. , Müller-Buschbaum Hk.
Published: March 2015

Single crystals of the compounds Lu2Cu2O5 (A) and Sc2Cu2O5 (B) were prepared by melting the oxide mixtures (2 CuO : 1 Lu2O3, 2 CuO : 1 Sc2O3) in a KF-flux. The crystal structures were investigated by single crystal X-ray data (Space group : C2V
9–P21nb, lattice constants (A): α = 1235.0, b = 1069.8, c = 340.5pm, (B): α = 1204.1, b = 1045.2, c = 322.0 pm). (A) and (B) are isotypic with Ho2Cu2O5 and differ from the Cu2In2O5 type in respect of the Cu2+-coordination.
Investigation of Inductive Effects on the Transphosphorylation Reaction of Spin-Labeled Phosphoryl Imidazolides, Part 1
Authors: Sosnovsky George , Konieczny Μaria
Published: March 2015

Spin-labeled phosphoryl imidazolides 3, 6, and 7 were prepared and compared to the unsubstituted compound 1 in reactivity towards hydroxy and amino compounds. The transphorphorylation reaction of compounds 3 and 6 was slower than that of 1. The

[xxx]

reaction of compound 6 was selective towards amines since no reaction occurred with hydroxy compounds. The reaction of compounds 7 was slow with hydroxy compounds and rapid with amines at room temperature. The transphorphorylation reaction of 1 was rapid with both hydroxy and amino compounds at 50-55 °C.
Über die Tricyanatomercurate KHg(NCO)3 und RbHg(NCO)3 — Synthesen, Kristallstrukturen und Schwingungsspektren / On the Cyanatomercurates KHg(NCO)3 and RbHg(NCO)3 — Syntheses, Crystal Structures and Vibrational Spectra
Authors: Thiele Gerhard , Hilfrich Peter
Published: March 2015

By mixing aqueous solutions of Hg(CH3COO)2 and KOCN the white precipitate K2Hg3(NCO)8 is formed. When recrystallised from CH3OH colorless crystals of the compound KHg(NCO)3 are obtained. The crystal structure analysis (space group Pnma; α = 1015.2(6) pm, b = 399.3(3) pm, c = 1772.9(9) pm) shows a distorted KCdCl3 arrangement with isolated Hg(NCO)2 molecules, K+ and NCO- ions. The vibrational spectra in the range of 250-3000 cm-1 are discussed. The rubidium compound is isotypous (a = 1019.0(6) pm, b = 411.6(4) pm, c = 1820.5(8) pm).
Reaktionen von Phosphoryliden mit Übergangsmetall-Verbindungen, II. Synthese von h5-C5H5Fe(CO)2-substituierten Phosphoniumsalzen / Reactions of Phosphorus Ylides with Transition Metal Compounds, II. Synthesis of h5-C5H5Fe(CO)2-substituted Phosphonium Salts
Authors: Knoll Lothar
Published: March 2015

Triphenylmethylene- and triphenylethylidenephosphorane react with h5-cyclopentadienyl-dicarbonylironiodide to yield the yellow stable complexes of the type

[h5-C5H5Fe(CO)2-CHRP(C6H5)3]I (R = H (1), CH3 (2)).

By reaction of 1 and 2 with AgBF4 the corresponding BF4-salts can be isolated. The new compounds are characterized by their 1H NMR, 31P NMR and IR spectra as well as by elemental analysis.
Dimethyl Phthalate, a Neutral Bidentate Oxygen-Donor Ligand to Divalent Metal Ions
Authors: Driessen W. L. , Everstijn P. L. A.
Published: March 2015

A series of new coordination compounds is reported with dimethyl phthalate (MPH) as the ligand, viz. [M(MPH)3](InCl4)2 with M=Mg(II), Ca(II), Mn(II), Fe(II), Co(II), Ni(II), and Zn(II). Each of the metal ions is bonded to three dimethyl phthalate molecules, the six carbonyl oxygens forming a regular octahedron. The carbonyl stretching vibration shifts to lower frequencies, the carbonyl bending vibration shifts to higher frequencies. The magnitudes of the shifts of these vibrations, the frequencies of the metal-ligand vibrations, and the melting points follow the Irving-Williams sequence.
Darstellung und Struktur weiterer ternärer Phasen mit modifizierter K8Ge46-Käfigstruktur / Preparation and Crystal Structure of Ternary Phases with a Modified K8Ge46 Clathrat Structure
Authors: Westerhaus Wolfgang , Schuster Hans-Uwe
Published: March 2015

In the systems K-Al, Ga, In-Si, Ge, Sn each phase of composition K8(3B, 4B)46 was prepared. The crystal structure for K8(Al, Ge)48 and K8(Ga, Ge)46 was determined by X-ray investigations. In the systems Na-Al, Ga-Si, Ge the compounds Na8(Al, Ge)46 (crystal structure determined), Na8(Ga, Si)46 and Na8(Ga, Ge)46 were prepared.
Die Kristallstruktur des Sr3As4 / The Crystal Structure of Sr3As4
Authors: Deller Klaus , Eisenmann Brigitte
Published: March 2015

The new intermetallic compound Sr3As4 has been prepared and structurally characterized by X-ray single crystal methods. Sr3As4 crystallizes orthorhombic with a = 1484 ± 2 pm, b = 1789 ± 2 pm, c = 597 ± 1 pm, space group Fdd2. Remarkable element of the structure are As4-chains.
Organoborierung von Alkinylstannanen, III1 Zur Reaktion von Trialkylboranen mit Monoalkinylstannanen / Organoboration of Alkynylstannanes, III The Reaction of Trialkylboranes with Monoalkynylstannanes
Authors: Menz Günther , Wrackmeyer Bernd
Published: March 2015

Organoboration, Alkynylstannanes, cis-Diborylalkenes, NMR

Trialkylboranes and 2-phenylborolane are reported to add to monoalkynylstannanes under mild reaction conditions. The structures of the organoboration products are discussed by means of 1H, 11B, 13C and 119Sn NMR spectroscopy. The reaction of the products with boronhalides yields cis-diborylalkenes.
Reaktionen koordinierter Liganden, V / Reactions of Coordinated Ligands, V
Authors: Stelzer Othmar , Eikmeier Hans-Bernhard , Johannsen Gerd
Published: March 2015

The azidophosphine complexes cis-Mo(CO)4(R2PN3)2 (R = Me, Ph) may be obtained by nucleophilic displacement reactions of chlorine by azide ion in complexes cis-Mo(CO)4(R2PCl)2. The thermal decomposition and Staudinger reactions were studied. Silylation of NH- or NH2-functional groups in aminophosphine and hydrazinophosphine complexes with Me3SiCl, Me2SiCl2 or Me2SiCl-SiClMe2 leads to a series of monodentate or bidentate silylaminophosphine complexes, e.g. (CO)4Mo(R2PNHSiMe3)2, (CO)4Mo-(R2PNH)2SiMe2, (CO)4Mo(R2PNH)2(SiMe2)2, (CO)4Mo[R2PN(SiMe3)(SiMe3)NPR2] or (CO)4Mo[R2P-N(SiMe3)SiMe2-SiMe2-N(SiMe3)PR2].

The structures of these complexes are discussed on the basis of their IR and NMR spectra.
Notizen: Beiträge zur Chemie des Phosphors, 771 Spektroskopischer Nachweis eines Diphosphirans (Diphosphacyclopropans) / Contributions to the Chemistry of Phosphorus, 771 Spectroscopic Detection of a Diphosphirane (Diphosphacyclopropane)
Authors: Baudler Marianne , Carlsohn Burkhard
Published: March 2015

1,2 - Diphenyl - 3,3 - dimethyl - diphosphirane (1,2- Diphenyl- 3,3- dimethyl-diphosphacyclopropane) (1) is formed by the reaction of K(C6H5)P–P(C6H5)K with 2,2-dichloropropane in n-pentane at —30 °C. It could be detected and identified by its 31P NMR singlet at —122 ppm, which lies in the high field region characteristic for phosphorus three-membered ring compounds, as well as by its mass spectrum. Besides, (PC6H5)5 and several cyclocarbaphosphanes of ring sizes five and six are formed. After the reaction of (CH3)3Si(C6H5)P–P(C6H5)Si(CH3)3 with methylene iodide a weak 31P NMR signal at —147 ppm could be observed, which probably corresponds to the 1,2-diphenyl-diphosphirane.
The Influence of the Exchangeable Monovalent Cations on Vibrations of Y Zeolite Framework
Authors: Radak V. M. , Ćeranić T. S. , Živadinović I. M.
Published: March 2015

The influence of the exchangeable monovalent cations on the vibrations of the frame-work of Y zeolite has been studied. A regular shift of the frequencies of some absorption bands is observed and described as a function of interaction between the exchangeable cation and the oxygen from the zeolite framework. The linear dependence of the fre-quencies of some absorption bands and the reciprocal of the sum of ionic radii of the cation and the framework oxygen suggests that the exchanged cations: Na+ , Ag+, K+ and Tl+ are occupying similar positions in the zeolite lattice. Li+ and Cs+ ions do not obey this regularity. The present IR studies agree with the results of chemical analysis of the studied zeolites.
Notizen: Über Thiotitanate(IV): Synthese und Struktur von Cs2[TiS3] [1] On Thiotitanates(IV): Synthesis and Structure of Cs2[TiS3]
Authors: Rad H. , Hoppe R.
Published: March 2015

Cs2TiS3, black single crystals, dark red transparent, a = 12.518, b = 9.036, c = 6.550 Å, Z = 4.

[Cmc 21, 4-circle-diffractometer 4° ≤ ω ≤ 30°, Moka, R = 5.68, Rw = 5,12%] is isotypic with Cs2PbO3, exhibiting Coord. Number 5 of Ti4+.