bluuebunny/crossref_metadata_2025 huggingface dataset:
Die Kristallstruktur des Zinnsulfidiodids Sn4SI6 / The Crystal Structure of Sn4SI6
Authors: Fenner Jürgen
Published: February 2015

The new ternary tin(II) sulfide iodide Sn4SI6 was prepared by annealing of stoichiometric amounts of SnI2 and SnS at 280 °C. The structure of this compound was determined from three-dimensional X-ray data. The cell parameters for the monoclinic phase are a = 14.129, b = 4.425, c = 25.15 Å, and β = 93.42°; space group C2/m (No. 12), Z = 4. Parts of the structure are built up of the Snl2 structure.
K2PtS15, Synthese und Kristallstruktur / K2PtS15, Synthesis and Crystal Structure
Authors: Spangenberg Manfred , Bronger Weif
Published: February 2015

K2PtS15 can be synthesized from solutions of potassium polysulfide and hexachloro-platinic acid. X-ray investigations on single crystals revealed its structure. Similar to the ammonium salt (NH4)2PtS15 2 H2O, the Pt-atom of the PtS15
2-anion is found in an octahedral environment consisting of three bidentate five-membered sulfur chains.
Darstellung, Kristallstruktur und Eigenschaften von Au7P10I / Formation, Crystal Structure and Properties of Au7P10I
Authors: Binnewies Michael
Published: February 2015

Au7P10I can be prepared by chemical transport with iodine in a temperature gradient 900 °C→ 450 °C. The crystal structure has been determined. The compound shows metallic conductivity; its thermal stability has been studied.
Die Kristallstruktur von 2.2'-Bipyridin-bis(brenzkatechyl)phosphoniiimhexafluorophosphat / Crystal Structure of 2,2'-Bipyridine-bis(o-phenylenedioxy)phosphonium Hexafluorophosphate
Authors: Sheldrick William S. , Schmidpeter Alfred , Criegern Thomas von
Published: February 2015

2,2'-Bipyridine-bis(o-phenylenedioxy)phosphonium hexafluorophosphate crystallises in the monoclinic space group C2/c (Z = 8) with a = 18.654(4), b = 10.131(2), c = 24.344(4) Å, β = 99.53(4)°. The cationic phosphorus atom displays an octahedral coordination slightly distorted towards the tetrahedral one of an uncomplexed phosphonium center. The OPO bond angles are between 91.6 and 95.7(2)°, the NPN angle of the bipyridine chelate ring in contrast is only 81.7(2)°. The ring systems of the bipyridine ligand are inclined slightly to one another at an angle of 4.7°. The bond lengths to the cationic phosphorus are P - 0 1.668-1.672(3), P-N 1.896(4) and 1.898(4) Å. The hexafluorophosphate anion is disordered
The Crystal Structure of a Spirocyclic Cyclophosphazene N3P3(NMe2)4(NHCH2CH2NH) - Evidence for Intermolecular Hydrogen Bonding
Authors: Sudhakara Babu Y. , Manohar H. , Ramachandran K. , Krishnamurthy S. S.
Published: February 2015

An X-ray crystal structure analysis of tetrakis(dimethylamino)(ethylenediamino)cyclotriphosphazene reveals a novel spirocyclic structure with the spiro ring having an envelope conformation. There is evidence for an intermolecular N-H ··· N bond in the crystal which persists in solution
Chemie polyfunktioneller Liganden, XLIV [1] Darstellung und Eigenschaften von 1.1.1-Tris(diiodarsinomethyl)ethan / Chemistry of Polyfunctional Ligands, XLIV [1] Preparation and Characterization of 1,1,1-Tris(diiodarsinomethyl)ethane
Authors: Eilermann Jochen , Schössner Horst , Lindner Helmut A.
Published: February 2015

The phenylalkyl arsine CH3C[CH2As(C6H5)2]3 reacts with gaseous HI by selective cleavage of the arsenicphenyl bonds yielding CH3C(CH2AsI2)3. This compound is characterized using IR, FIR, Raman, 1H NMR and electron impact mass spectroscopy
Cis-2-telluro-1.3.2λ5.4λ3-diazadiphosphetidin - Kristallstruktur eines in Lösung fluktuierenden Redoxsystems / Cis-2-telhirium-1.3.2λ5.4λ3-diazadiphosphetidine - Crystal Structure of a Redox System Fluctuating in Solution
Authors: Pohl Siegfried
Published: February 2015

The crystal structure of the title compound was determined from single crystal X-ray data. The compound crystallises in the orthorhombic space group Pnma. In contrast to the solution where fluctuating P-Te bonds have been established by NMR analyses the crystals contain isolated molecules with fixed P-Te bonds (bond length: 235.4 pm). The four-membered phosphorus nitrogen ring exhibits significant deviations from planarity. The P-N bond lengths were found to be 168.3 and 175.0 pm, respectively
Production and Reaction of Singlet Oxygen in Aqueous Micellar Solutions Using Pyrene as Photosensitizer
Authors: Miyoshi Norio , Tomita Giiti
Published: February 2015

The reaction of singlet oxygen with 1,3-diphenylisobenzofuran was investigated in aqueous micellar solutions of sodium dodecyl sulfate and dodecyl trimethylammonium chloride using pyrene as photosensitizer. Singlet oxygen, produced by the photosensitization of pyrene bound to micelles, oxidized efficiently 1,3-diphenylisobenzofuran bound to micelles. The quantum yield for singlet oxygen production and the rate constant for furan oxidation were determined by the kinetic analysis for the oxidation reaction of furan. Quenching of singlet oxygen by sodium azide competed with the furan oxidation, and its rate constant was also determined.

Results obtained were compared with those in methanolic solutions. The quantum yield for singlet oxygen production and the rate constant for furan oxidation were much higher in micellar solutions than those in methanolic solutions. Empty micelles wxas found to act as a considerably strong scavenger for singlet oxygen. The penetration probability of singlet oxygen from aqueous phase into the interior of micelles which bound furan was also estimated
Elementorganische Amin/Imin-Verbindungen, XVIII [1] Amino-Imino-Thiophosphorane: σ3, λ5-Phosphazene / Elementorganic Amino/Imino Compounds, XVIII [1] Aminoiminothiophosphoranes: σ3, λ5-Phosphazenes
Authors: Scherer Otto J. , Külbach Ngoc-Tram , Glässel Walter
Published: February 2015

The reaction of the aminoiminothiophosphoranes (1) with methanol yields the bisamino-thiophosphoric acid derivatives (3). la and IVb → VTb element halides form the new P-N element four membered rings 4 →7, which partially exist as a mixture of eis and trans isomers. Different ylide group transfer is observed on the reaction of la with trimethyl -phosphine or trimethyl phosphite. With trimethylphosphine (CH3)3P(S) and a phos-pha(III)azene are formed, with trimethyl phosphite (CH3O)3P = NC(CH3)3 and the [2 + 2] cycloaddition product of la and (R3C)(R3Si)N-P = S (R = CH3) can be isolated.
Synthesis of 2-Methyl-l-phenylthiocarbamoylglyoxal Arylhydrazones and Diethyl(arylazo)(phenylthiocarbamoyl)malonate and their Reactions with Hydrazines
Authors: Amer Fathy. A. , Harhash Abdel Hamid , Awad Mary L.
Published: February 2015

Treatment of a-phenylthiocarbamoyl acetyl acetone (1) with aromatic diazonium salts effects acetyl cleavage with the formation of 2-methyl-I-phenylthiocarbamoylglyoxal arylhydrazones (2a-c), which afford the anilinopyrazoles (5a-c) and the phenylimino-2- pyrazolines (6a-c) on treatment with hydrazine or phenyl hydrazine respectively.

Treatment of diethyl a-phenylthiocarbamoyl malonate with aryl diazonium salts gave diethyl (arylazo)(phenylthiocarbamoyl) malonate which afford the 7-phenyl-5-(arylazo)- 2,3,7-triazabicyclo[3,2,0]hept-I-ene-4,6-dione (9a, b) and its 3-phenyl derivatives (9c, d) with hydrazines and phenyl hydrazine respectively
Notiz zur Absolutkonfiguration des Epoxipiperolids / Note on the Absulute Configuration of Epoxipiperolide
Authors: Hansel Rudolf , Schulz Jutta
Published: February 2015

The epoxide-ring of (+)-5-[trans-(Z)-2,3- epoxy-1-methoxy-propylidene]-4-methoxy- 2(5H)-furanone (1) was opened hydrogenolytically (palladium/charcoal) to (+)-(2S)-5-(2-hydroxy-1-methoxy-3-phenylpropylidene)- 4-methoxy-2(5H)-furanone (2) whose absolute configuration (2S) was determined applying Horeau's method. For the natural product (+)-1 itself follows (2S,3R) Reconfiguration
Darstellung und Kristallstruktur von Na2AgAs und KCuS / Preparation and Crystal Structure of Na2AgAs and KCuS
Authors: Savelsberg Gerhard , Schäfer Herbert
Published: February 2015

The title compounds have been prepared and their structures determined. Na2AgAs crystallizes in the Na2CuAs structure type, forming infinite Ag-As-zig-zag-chains. KCuS builds up a new structure type but with similar zig-zag-chains of Cu- and S-atoms. Crystallographic data:

Na2AgAs: C2221, a= 879 ± 2 pm, 6 = 736 ± 2 pm, c = 559 ± 2 pm;

KCuS: Pna21, a = 1066 ± 2 pm, 6 = 620 ± 2 pm, c = 532 ± 2 pm.
Ion Association and Solvation in Dichloromethane of Tetrachloro-and Tetrabromoferrates(III) Compared with Simple Halides
Authors: Bait S. , Chattel G. du , Kieviet W. de , Tieleman A.
Published: February 2015

Conductivity measurements are reported in dichloromethane for tetraethylammonium and tetraphenylarsonium salts of tetrachloro-and tetrabromoferrate(III) and halide ions (chiefly chloride and bromide). Analysis of the data in terms of the recent Fuoss equation has given the ion-pair association constants. The experimental values are close to the ones calculated from the electrostatic Fuoss-Eigen equation. The solvent acts as an acceptor by way of forming hydrogen-bonds to the simple halide ions and to a much less extent to the ferrates. Solvation of chloro-and bromoferrates(III) seems to be comparable, as deduced from the association constants and NMR paramagnetic line broadening. The phenyl groups of the tetraphenylarsonium ion seem to give π-interaction with the solvent.
Die Ultraviolettspektren der Halogenazide ClN3, BrN3 und IN3 / The Ultraviolet Spectra of the Halogen Azides ClN3, BrN3 and IN3
Authors: Dehnicke Kurt , Ruschke Peter
Published: February 2015

The ultraviolet spectra of the halogen azides ClN3, BrN3 and IN3 were recorded in hexane solution as well as in carbon tetrachloride solution. The spectra are in agreement with Cs-symmetry of the XN3 species and correspond well with other covalent azides.
Fragmentation of the α-Amino Acid Methionine in Field Desorption Mass Spectrometry
Authors: Greef J. van der , Nibbering N. M. M. , Schulten H.-R. , Lehmann W. D.
Published: February 2015

Field Desorption Mass Spectrometry, a-Amino Acid Methionine The fragmentation of methionine in field desorption mass spectrometry has been studied. Decomposition mechanisms are described which are based on stable isotope labelling, low and high resolution field desorption, and the application of field desorption kinetics. The combined use of these techniques for the study of some fundamental fragmentations in field desorption is demonstrated successfully. Further, a comparison with the fragmentation pattern of methionine under electron impact, chemical ionization and Curie point pyrolysis is given.
Darstellung und Struktur der Phase Li5Na2Sn4 / Preparation and Crystal Structure of Li5Na2Sn4
Authors: Volk Klaus , Müller Wiking
Published: February 2015

The new compound Li5Na2Sn4 crystallizes trigonally, a = 472.3 ± 1 pm, c = 7178 ± 8 pm, space group R3̅m-D5
3d. A quarter of the Sn atoms in the unit cell build up a puck­ered net of six-membered rings, another quarter is bound to the net-atoms forming a tetrahedral Sn coordination. The other half of the Sn atoms is ordered in layers of parallel Sn2 pairs. The nets and layers are separated by the alkali atoms. The structural relations to the variants of the W-structure type of compounds in the system Li-Sn and Na-Sn are shown.
CaAl2Se4 und SrAl2Se4 — Strukturvarianten des TlSe-Typs / CaAl2Se4 and SrAl2Se4 -Variants of the TlSe-Structure
Authors: Klee Wilfried , Schäfer Herbert
Published: February 2015

CaAl2Se4 and SrAl2Se4 have been prepared and their crystal structures determined. They crystallize orthorhombically, space group Cccm, with the lattice constants:

CaAl2Se4: a = 633 ± 1pm, b = 1048 ± 1pm, c = 1053 ± 1pm;

SrAl2Se4: a = 627 ± 1 pm, b = 1082 ± 1 pm, c = 1085 ± 1 pm.

The structures of these compounds are closely related both to each other and to the TlSe-structure.
Kristall- und Molekülstruktur von 5.10-Dihydro-5.10-diniethylphenaziniiimtniodid und 5.10-Dihydro-5.10-diethylphenaziniumtriiodid / Molecular and Crystal Structure of 5,10-Dihydro-5.10-dimethylphenaziniumtriiodide and 5.10-Dihydro-5.10-diethylphenazinium triiodide
Authors: Keller H. J. , Moroni W. , Nöthe D. , Scherz M. , Weiss J.
Published: February 2015

Oxidation of 5,10-dihydro-5,10-dimethylphenazine and 5,10-dihydro-5,10-diethyl-phenazine under different reaction conditions leads to several iodine containing solids. The preparation and X-ray structure of two of them, 5,10-dihydro-5,10-dimethyl-phcnaziniumtriiodide (3) and 5,10-dihydro-5,10-diethylphenaziniumtriiodido (4) are reported here.

Compound 3 crystallizes in space group P21/n with lattice parameters a = 8.552(6) Å, b= 16.953(2) Å, c- 12.157(9) Å and β= 103.46(2)° with four formula units in the unit cell. The structure was refined to an R-value of 0.046 using 2387 independent reflections. The lattice constains distinct, slightly distorted triiodide ions and bent 5,10-dihydro-5,10-dimethylphenazinium radical cations. Compound 4 crystallizes in the same space group P21/n with lattice parameters a = 8.531(6) Å, b = 8.332(21) Å, c = 13.320(15) Å and β= 94.44(19)° with two formula units in the unit cell. The structure was refined to an R-value of 0.076 using 1195 independent reflections. The lattice contains strictly linear symmetrical triiodide ions and planar centrosymmetrical 5,10-dihydro-5,10-diethyl- phenazinium radical cations.
Beiträge zur Untersuchung anorganischer nichtstöchiometrischer Verbindungen, VIIa Ein neuer einfacher Weg zur Berechnung von [(O,F)/Me]-Werten bei Blockstrukturen / Contributions to the Study of Inorganic Non-Stoichiometric Compounds, VIIa A New Simple Method to Calculate Values of [(O,F)/Me] for Block Structures
Authors: Hibst Hartmut , Gruehn Reginald
Published: February 2015

A simple, quick and reliable method is derived to calculate values of [(O,F)/Me] for block structures. The method of calculation is exemplified using ideal and real (defect) block structures and inconsistent published data. The method represents a simple means to systematically classify block structures.
Spektroskopische Untersuchungen in der Festkörperchemie, XII* Re-NQR-und 1H-Breitlinien-NMR -Studien an Rhenium(YII)- Sauerstoffverbindungen / Spectroscopic Investigations in Solid State Chemistry, XII* Re NQR and 1H Wideline NMR Studies on Rhenium(VII) Oxygen Compounds
Authors: Burkert Paul K. , Hutter Frank M.
Published: February 2015

The first Re NQR spectra of rhenium oxygen compounds with rhenium atoms in the pseudo-octahedral environment of Re2O7(H2O)2 and Re2O7(H2O)2 · 2(1,4)-dioxane were found. The values of the Re NQR coupling constants of these rhenium atoms are the highest measured until now. They show, that the gradient of the electrical field is much more sensitive to distortions of an octahedral crystal field than to distortions of a tetrahedral field.
Derivatives of cis-NPCl2(NSOCl)2 and (NPCl2)2NSOCl, Part X [1] Aminolysis of cis-NPCl2(NSOF)2 and (NPCl2)2NSOF
Authors: Baalmann H. H. , Grampel J. C. van de
Published: February 2015

The aminolysis of the ring systems cis-NPCl2(NSOF)2 and (NPCl2) 2NSOF by cyclic amines in acetonitrile at room temperature shows the S-F bond to be stable towards a nucleophilic attack. The amino derivatives are characterized by their spectral data. Structure assignments are based on 31P NMR spectroscopy.
Di-t-butyl(trimethylstannyl)stibin und Tetrakis(trimethylstannyl)distiban / Di-t-butyl(trimethylstannyl)stibine and Tetrakis(trimethylstannyl)distibane
Authors: Breunig Hans Joachim
Published: February 2015

By reaction of t-butyliodide with tris(trimethylstannyl)stibine di-t-butyl (trimethy 1 - stannyl)stibine as well as tetrakis(trimethylstannyl)distibane are formed.
Complexes of Some Platinum Metals with p-Diethylamino Anil of Phenyl Glyoxal
Authors: Verma H. S. , Saxena R. C.
Published: February 2015

Complex compounds of platinum metals Ru(III), Rh(III), Os(IV), Ir(IlI) and Pt(IV) with the bidentate Schiff base ligand derived by the condensation of phenyl glyoxal with p-diethylamino aniline have been prepared and characterized. All the complexes are stable at room temperature. The complexes of Ru(III) and Os(IV) are Paramagnetic and the other complexes of Rh(III), Ir(III) and Pt(IV) are diamagnetic. The spectral studies and the calculation of ligand field parameters clearly indicate the octahedral structure of these complexes.
Synthesis and Biological Activity of Some New Benzthiazoloazetidin-2-ones and Benzthiazolothizoiidin-4-ones, IV
Authors: Hassan Kh. M. , Mahmoud A. M. , Sherief H. A. El-
Published: February 2015

Arylidene-2-aminobenzthiazoles (1) were prepared by the condensation of 2-aminobenzthiazole with aromatic aldehydes. Cyclocondensation of mercaptoacetic acid and/or chloroacetyl chloride on 1 giving the corresponding 4-thiazolidinones (2) and/or azetidinones (3) respectively, in good yields. The biological activity of the prepared compounds were screened against some strains of bacteria.
Die ungewöhnliche Reaktion von 1.2—5.6-Di-O-isopropyliden-α-D-glucofuranose (Diacetonglucose) mit dem System Triphenylphosphin/Azodicarbonsäureester / The Unusual Reaction of 1,2-5,6-Di-O-isopropylidene Glucofuranose (Diacetoneglucose) with the System Triphenylphosphine/Azodicarboxylate
Authors: Kunz Horst , Schmidt Peter
Published: February 2015

The 1,2-5,6-Di-O-isopropylidene glucofuranose (7) reacts with triphenylphosphine/azodicarboxylate and methyliodide with formation of the relatively stable alkoxyphosphonium salt (8a). With water and alcohols 8 forms triphenylphosphine oxide and diacetone glucose 7. The reaction of 8 with sodium benzoate gives the glucofuranose-3-benzoat (10), the formal product of substitution under retention of configuration.
Zur Reaktivität von C=N-Doppelbindungssystemen, XV [1] Die Reaktion von Anilinomethylen-barbitursäuren mit methylenaktiven Nitrilen / The Reactivity of the C=N-Double Bond System, XV [1] The Reaction of Anilinomethylene-barbituric Acids with Methylenactive Nitriles
Authors: Wipfler Helmut , Ziegler Erich , Wolfbeis Otto S.
Published: February 2015

N,N′-Dimethyl-5-anilinomethylene-barbituric acids and its thio analogues react with alkyl cyanoacetates or malodinitrile in DMF in the presence of KOH to give 1,2,3,4- Tetrahydro-7 H-pyrano[2,3-d]pyrimidines, whereas N-unsubstituted anilinomethylenebarbituric acids under the same conditiones afford 1,2,3,4-tetrahydro-pyrimidine-5-propenoic acid derivatives.
Utilization of Various Phosphoryl Halides and Imidazolides for the Conversion of Aldoximes to Nitriles
Authors: Konieczny Maria , Sosnovsky George
Published: February 2015

Imidazolides of phosphorus 7, 9, and 13 are, in most cases, superior

to the chloridates 4, 5 (Ṙ = 2,2,6,6-tetramethyl-1-oxyl-4-piperidyl), 6, 8, and 12 for the transformation of aliphatic and aromatic aldoximes to nitriles

in yields generally exceeding 80%. The transformation is thought to occur via a phosphorylated intermediate, which was isolated in the case of the reaction bfn-butyraldoxime with the nitroxyl radical-labeled chloridate 4.
NOTIZEN: Al(H2PO4)(HPO4)(H2O), ein saures Phosphat mit zweidimensionaler Al-O-P - Vernetzung / Al(H2PO4)(HPO4)(H2O), an Acid Phosphate with Two-Dimensional Al-O-P Linking
Authors: Kniep Rüdiger , Mootz Dietrich , Wilms Axel
Published: February 2015

The crystal structure of aluminium-dihydrogenphosphate- monohydrogenphosphate-monohydrate contains macromolecular units

2
∞[Al(H2PO4)(HPO4)(H2O)]

consisting of Al(O)5(H2O) octahedra which share vertices with P(O)2(OH)2 and P(O)3(OH) tetrahedra. Neighbouring layers are linked by hydrogen bonds.
Neue Synthesen für ReNCl3 / New Syntheses of ReNCl3
Authors: Liese Werner , Dehnicke Kurt
Published: February 2015

ReNCl3 is prepared by the reactions of ReCl5 with NCl3 and Cl3VNCl, respectively.
Beiträge zur Chemie des Phosphors, 85 Synthese und Eigenschaften der Diphosphirane (t-BuP)2CMe2 und (t-BuP)2CH2 Contributions to the Chemistry of Phosphorus, 85 Synthesis and Properties of the Diphosphiranes (t-BuP)2CMe2 and (t-BuP)2CH2
Authors: Baudler Marianne , Saykowski Franz
Published: February 2015

The first three-membered P2C heterocycles, 1,2-di-tert-butyl-3,3-dimethyl-diphosphirane, (t-BuP)2CMe2 (1), and 1,2-di-tert-butyl-diphosphirane, (t-BuP)2CH2 (2), were synthesized by [2 + 1] cyclocondensation reactions of K(t-Bu)P-P(t-Bu)K with 2,2-dichloropropane and dichloromethane, respectively. Both compounds could be isolated in a pure state by vacuum distillation. Whereas 1 is surprisingly stable under inert condi­tions, 2 dimerizes already at room temperature to form the six-membered cyclocarbaphosphane 1,2,4,5-tetra-tert-butyl-cyclo-3,6-dicarba-1,2,4,5-tetraphosphane, (t-BuP)4(CH2)2 (3).The diphosphiranes 1 and 2 were characterized by elemental analysis, osmometric molecular mass determination, mass, NMR, and IR spectra. The t-butyl groups are situated on opposite sides of the P2C ring, whereas the dimeric compound 3 possesses an “all-trans” configuration of the organyl substituents.
Stabile Quecksilber(I)-Selen-Verbindungen, 2. Mitteilung Die Struktur der roten Modifikation des Tetrakis(diphenylseleno)- diquecksilber(I)-bis(chlorat(VII))/ Stable Mercury(I)-Selenium Compounds, 2nd Communication The Structure of the Red Modification of Tetrakis(diphenyl-seleno)-dimercury(I)-bis(chlorate(VII))
Authors: Brodersen Klaus , Liehr Günter , Rosenthal Michael , Thiele Gerhard
Published: February 2015

As shown by X-ray analysis the structure of the red modification of tetrakis(diphenyl-seleno)-dimercury(I)-bis(chlorate(VII)) contains cations [(C6H5)2Se]2Hg-Hg[Se(C6H5)2]2
⊕⊕ and ClO4
--anions. The twofold coordination of each mercury atom by 2 selenium atoms is remarkable for a mercury(I) compound. The relations between red and yellow modifications are discussed.
Molybdännitridbromid, MoNBr3/Molybdenumnitridobromide, MoNBr3
Authors: Dehnicke Kurt , Krüger Norbert
Published: February 2015

Molybdenumnitridobromide, MoNBr3, is prepared by the reaction of MoBr4 with iodine azide in CCl4 suspension. Some properties are given. The IR spectrum is discussed, which is in agreement with a M ≡ N triple bond.
Molekülstruktur des 7-Methyl-1.3.5-triaza-7-phosphaadamantan-7-ium-tetrafluoroborats. Darstellung und Charakterisierung des 7-Methyl-1.3.5-triaza-7-phospha-tricyclo[3.3.2.13,7]-undecan-7-ium-iodids/Molecular Structure of 7-Methyl-1 ,3,5-triaza-7-phosphaadamantane-7-ium-tetrafluoroborate. Preparation and Characterization of 7-Methyl-1,3,5-triaza-7-phospha-tricyclo[3,3,2,1 3,7]-undecan-7-ium-iodide
Authors: Jogun Kurt H. , Stezowski John J. , Fluck Ekkehard , Weißgraeber Hans-Jürgen
Published: February 2015

7-Methyl-1,3,5-triaza-7-phosphaadamantane-7-ium-tetrafluoroborate (2b) has been synthesized and characterized by crystal structure analysis. The crystal structure is interpreted in comparison with the parent compound 1,3,5-triaza-7-phosphaadamantane, and its 7-oxide and 7-sulfide. 7-Methyl-1,3,5-triaza-7-phospha-tricyclo[3,3,2,1 3,7]-undecan-7-ium-iodide (6) has been prepared and characterized by 31P, 13C, and 1H NMR spectroscopy and by its IR spectrum.
Oberflächenverbindungen von Übergangsmetallen, XX Komplexe von Oberflächen-Chrom(II) mit Olefinen /Surface Compounds of Transition Metals, XX Complexes of Surface Chromium(II) with Olefines
Authors: Krauss Hans-Ludwig , Westphal Ulrich
Published: February 2015

Surface chromium(II) supported on silica forms 1:1 and 1:2 complexes with defines; polyenes prefer chelate structures. For the ligand-to-metal bond a “Zeise-Salt” type is postulated. Secondary reactions include cis-trans isomerisation, shift of double bond, rearrangement of C-framework and polymerization/oligomerization. Cyclopentadiene obviously gives a h5 -cyclopentadienyl/hydrogen complex by oxidative addition followed by H2 emission and formation of a h5 -cp-CrIII complex; in this case the metal can be split off from the support by H+ without cleavage of the cp-Cr-bond.
Photochemische Reaktionen von Übergangsmetall-Olefin-Komplexen, II Die Umsetzung von Tricarbonyl-η-1.3.5-cycloheptatrien-chrom(O) mit substituierten Fulvenen /Photochemical Reactions of Transition Metal Olefin Complexes, II The Reaction of Tricarbonyl-η-1,3,5-cycloheptatriene-chromium(O) with Substituted Fulvenes
Authors: Kreiter Cornelius G. , Kurz Hans
Published: February 2015

When tricarbonyl-η-1,3,5-cycloheptatriene-chromium(O) (1) and 6,6-dimethylfulvene or tricarbonyl-η-6,6-dimethylfulvene-chromium(O) and 1,3,5-cyeloheptatriene are irradiated with UV light, a red crystalline dicarbonyl-chromium complex with an η3 -1′,2′,3′-(2-cyclohepta-2′, 4′ -dien 1′ ,6′-ylene)-η5 (2-cyclopentadienylidene)propane chelate ligand, Cr(CO)2C15H18 (2), is formed in high yields. Under the same conditions, 1 with 6,6-diphenylfulvene yields two isomeric complexes. One of them, Cr(CO)3C25H22 (3), is analoguous to 2 and contains the η3 -1′,2′,3′-cyclohepta-2′,4′-dien-1′ ,6′ / -ylene-η5 -cyclopentadienylidene-diphenyl-methane chelate ligand. The other one is the dicarbonyl η3 -1′,2′,3′-cyclohep-tatrienyl- η5 diphenylmethylcyclopentadienyl-chromium(O), Cr(CO)2(C7H7)(Ci8H15) (4). The complexes were characterized by analysis and mass spectra. The structures are based on IR, and 1H and 13C NMR spectra. Einführung
Elementorganische Amin/Imin-Verbindungen, XIX Phospha(III)azen-Komplexe des Platins /Elementorganic Amino/Imino Compounds, XIX Phospha(III)azene Complexes of Platinum
Authors: Scherer Otto J. , Kuhn Norbert , Jungmann Heribert
Published: February 2015

Reacting Zeise's salt with the phospha(III)azene (R3C)(R3Si)N-P = N-CR3 (R = CH3) (1) one gets the platinum phospha(III)azene complex (2), Cl2PtIL2 (L = 1). 2 adds water and methanol to the P = N bond of the phospha(III)azene ligand with formation of 3, Cl2Pt(PRR2
1)2 (R = (CH3)3SiO, R1 = (CH3)3CNH) and 4, Cl2Pt(PRR1R2)2 (R = CH3O, R1 = (CH3)3CNH, R2 = (CH3)3SiNC(CH3)3). 2, 3 and 4 have trans configuration, 4 also forms a mixture of the meso and d, 1 isomers. For 2 a P-σ coordination of the phospha(III)- azene ligand is proposed.
Metallkomplexe mit Tetrapyrrol-Liganden, XIX [1]. Synthese und elektrochemische Charakterisierung der Kohlenmonosulfid-Metalloctaethylporphyrine mit Eisen(II) oder Osmium(II) im Zentrum. Ein Beitrag zur "Bathochromie-Regel" / Metal Complexes with Tetrapyrrole Ligands, XIX [1]. Synthesis and Electrochemical Characterization of Thiocarbonyl Metallooctaethylporphyrins with Iron(II) or Osmium(II) in the Center. A Contribution to the "Rule of Bathochromism"
Authors: Buchler Johann W. , Kokisch Wolfgang , Smith Paul D. , Tonn Bernhard
Published: February 2015

The preparation and spectroscopic characterization of thiocarbonyl metalloporphyrins M(OEP)CS(L') (e.g. 2e: M = Fe, L' = Py, 1e: M = Os, L' = Py** are described. Especially noteworthy is the existence of a pentacoordinate, diamagnetic, air-stable heme Fe(OEP)CS (2f: M = Fe, no L′). A linear correlation of the α-band frequencies (expressed as ϋa) in the optical spectrum and the metal(II/III) redox potentials (E1/2) taken from cyclic voltam­metry experiments suggests (Abb. 3) that in complexes of the type M(OEP)LL' (1,2) λa is bathochromically shifted as the π-acceptor capacity of L increases (“Rule of Bathochromism”). The strong π-acceptor capacity of carbon monosulphide renders the attack of dioxygen to the thiocarbonyl heme unfavourable; O2 and CS seem to be comparable in their π-acceptor strength.
Diazadien-Nickel-Komplexe, I: Bis(diazadien)-nickel(O) und Bromo-diazadien-nickel(I) / Diazadiene Nickel Complexes, I: Bis(diazadiene) Nickel(O) and Bromo-diazadiene Nickel(I)
Authors: Dieck Heindirk tom , Svoboda Michael , Kopf Jürgen
Published: February 2015

Reduction of anhydrous nickel(II) compounds in the presence of diazadienes RN=CR'-CR' = NR, |(DAD), yields (DAD)2Ni(0). This complex 1 with R = CH(i-C3H7)2 is especially reactive and comproportionates with DADNiBr2 (2) to yield the bromobridged dimeric nickel(I) species (DADNiBr)2 (3). The crystal and molecular structure of 3 has been determined by single crystal X-ray diffraction: Space group Pbca with a = 1225.8(12), b = 1474.8(14) and c = 2167.4(22) pm; Ra = 0.076, 1034 reflections. Catalytic tetramerisation of substituted alkynes with 1 is discussed in view of the very easy formation of dimers 3.
Darstellung, Eigenschaften und Struktur des Cyclopentadienyl(1.3-diborolenyl)nickel-Sandwiehs [1] / Synthesis, Properties and Structure of the Cyclopentadienyl(1,3-diborolenyl)nickel Sandwich [1]
Authors: Siebert Walter , Bochmann Manfred , Edwin Joseph , Krüger Carl , Tsay Yi-Hung
Published: February 2015

1,3,4,5-Tetraethyl-2-methyl-1,3-diborolene (5) reacts with nickelocene and dimeric cyclopentadienylcarbonylnickel, yielding orange red 4 a, a diamagnetic nickelocene analogue. 1H and 11B NMR data indicate a sandwich structure, which is confirmed by X-ray structure analysis. The title compound crystallizes in the space group Pnma with a = 9.265(I), b = 15.1343(9), c = 12.777(2) Å and four molecules in the unit cell. All metal carbon distances are similar to those of the isoelectronic ferrocene.
Über die Darstellung und Reaktionen von S -Trifluormethyl-Schwefelmonofluoridimiden / Preparation and Reactions of S-Trifluoromethyl Sulfurmonofluoride Imides
Authors: Stahl Ingo , Mews Rüdiger , Glemser Oskar
Published: February 2015

S-Trifluoromethyl sulfurmonofluoride imides

(R = CF3CO (1), NC (2), (CF3)2CF (3), C2F5 (4)) are prepared by the reaction of CF3SF3 with appropriate nitrogen derivatives; from cyanuric fluoride and CF3SF3 the S(+2) derivative (CF3)2N-SCF3 (5b) is formed. In (3) and (4) fluorine is substituted by N-silylated amines and PCl5 to give

(7) respectively. Silver pseudohalides AgX (X = NCO, NCS) will exchange the chlorine in 7.
Darstellung und Kristallstruktur von CaRh2B2 und CaIr2B2 / Preparation and Crystal Structure of CaRh2B2 und CaIr2B2
Authors: Schmidt Bernd , Jung Walter
Published: February 2015

The isotypic compounds CaRh2B2 and CaIr2B2 were prepared and investigated by X-ray methods. They crystallize orthorhombic in space group Fddd-D2h
24 with lattice constants

CaRh2B2: a = 1060.6 ± 0.4 pm,

b = 924.0 ± 0.4 pm,

c = 583.2 ± 0.2 pm.

CaIr2B2: a = 1072.7 ± 0.4 pm,

b = 925.7 ± 0.4 pm,

c = 587.7 ± 0.2 pm.

The structure contains isolated boron-atoms and can be derived from the CeCo3B2- or CaCu5-type of structure, respectively.
Darstellung und Kristallstruktur von Li2In und Li13In3 / Preparation and Crystal Structure of Li2ln and Li13ln3
Authors: Stöhr Joachim , Müller Wiking , Schäfer Herbert
Published: February 2015

Li2In crystallizes isotypic with Li2Ga, space group Cmcm-D2a
17, a = 476.3(1), b = 1001.7(3) and c = 473.5(1) pm, the In-atoms build up zig-zag-chains. Li13In3 forms a new structure type, f.c.c., space group Fd 3m-Oh
7, a = 1355.6(2) pm; it can be described as an ordered variant of the b.c.c. package with isolated In-atoms.
Synthese und Eigenschaften von Eisen-und Molybdän-Komplexen mit Schwefelliganden [1] / Synthesis and Properties of Iron and Molybdenum Complexes with Sulfur Ligands [1]
Authors: Sellmann Dieter , Unger Eugen
Published: February 2015

Lithium-2-methylmercaptobenzol-1-thiolat reacts with C5H5Fe(CO)2Cl to give [C5H5Fe(CO)2(S-C6H4-SCH3]); with C5H5Mo(CO)3Cl cleavage of metal chlorine and metal carbonyl bonds occurs yielding [C5H5Mo(CO)2(S-C6H4-SCH3)]. Reaction of dilithium- benzene-1,2-dithiolate with C5H5Fe(CO)2Cl leads to the binuclear [{C5H5Fe(CO)2}2S2C6H4]. CO substitution and rearrangement are observed on irradiation of the complexes yielding [μ-S2C6H4{C5H5Fe(CO)}2], [C5H5Fe(CO)(S-C6H4-SCH3)] and [C5H5Fe(μ-S2C6H4)]2. Syn­theses, properties and spectra of the complexes are reported and discussed.
Siliciumverbindungen mit starken intramolekularen sterischen Wechselwirkungen, VII [1]. Tri-tert-butylsiliciumpseudohalogenide / Silicon Compounds with Strong Intramolecular Steric Interactions, VII [1]. Tri-tert-butylsilicon Pseudohalides
Authors: Weidenbruch Manfred , Pesel Helge
Published: February 2015

Tri-tert-butylchlorosilane reacts with potassium pseudohalides in the presence of catalytic amounts of the crown ether 18-crown-6 to give the tri-tert-butylsilicon pseudo-halides (t-C4H9)3SiX (X = CN, NCO, NCS, N3) in good yields. These new compounds are characterized by IR, 1H NMR, and mass spectra. In the absence of the crown ether no reaction occurs. Treating tri-tert-butylsilane with AgX (X = CN, SCN) gives the silicon pseudohalides in low yields.
Fluorierung von Platin(IV)amminkomplexen in wäßriger Lösung / Fluorination of Ammine Complexes of Platinum(IV) in Aqueous Solution
Authors: Jander Jochen , Mayer Hans Otto
Published: February 2015

Unlike chlorination fluorination of ammine complexes of platinum(IV) in aqueous solution does not lead to haloamido complexes. Instead, the triammine complexes [Pt(NH3)3Cl3]Cl and [Pt(NH3)3(NCl2)2Cl]Cl yield no definite main product, and the tetrammine and pentammine complexes trans-[Pt(NH3)4Cl2]Cl2, [Pt(NH3)4(NCl2)Cl]Cl2, [Pt(NH3)5Cl]Cl3, and [Pt(NH3)5(OH)]Cl3 form the sparingly soluble complex trans -[Pt (NH3)4Cl2](H2F3)2 · 2H2O as the main product.
tert-Butylphosphin-Komplexe von Gold(I)-und Silber(I)-halogeniden/tert-Butylphosphine Complexes of Gold(I) and Silver(I) Halides
Authors: Schmidbaur Hubert , Aly Aref A. M.
Published: February 2015

From HAuCl4 and tri-tert-butyl phosphine in methanol the gold(I) complex [(CH3)3C]3P-Au-Cl (1) has been synthesized and converted into the bromide 2 and iodide 3, using KBr and KI, respectively, in acetone solvent. The corresponding P-Cl functional complexes [(CH3)3C]2PCl-AuCl (4) and (CH3)3CPCl2 - AuCl (5) could be obtained from (carbonyl)gold chloride ClAu(CO) and the chlorophosphine in benzene, with evolution of CO.

The di-tert-butyl-phosphine analog, [(CH3)3C]2PH - AuCl (7) results from a lowtemperature reduction of HAuCl4 with this phosphine. All these gold(I) complexes are soluble in many solvents as monomers. The corresponding silver compounds, prepared from [(CH3)3C]3P and AgCl, Br, I in an inert solvent, appear to be oligomers, however, and showed dimer or tetramer association in halocarbon or benzene solvent. Infrared and 1H, 13C, 31P NMR spectra have been used for further characterization of the compounds.
Solvent Extraction Study of Nickel(II) and Cobalt(II) with I-Phenyl-3-methyl-4-benzoylpyrazol-5-one (PMBP-OH)
Authors: Patel A. N. , Qureshi A. M.
Published: February 2015

The extraction of nickel(II) from aqueous hydrochloric acid solution by I-phenyl -3-methyl-4-benzoylpyrazol-5-one (PMBP·OH) dissolved in carbon tetrachloride has been studied. The extraction of nickel(II) from the aqueous solution in the range of 1.0-5.0 M hydrogen ion concentration has been found to be much higher compared to that of cobalt(II). The extraction of nickel with PMBPOH is simple, fast and selective. The composition of the extracted species in solution as well as in solid form have been studied. The IR bands for the reagent and the metal complexes are reported.
Cyclopentadienyl Titanium(IV) Complexes with Phenylisocyanate
Authors: Parashar G. K. , Bharara P. C. , Mehrotra R. C.
Published: February 2015

Complexes of the type

CpTi(OR)3-n[N(Ph)COOR]n where R = Et, Pri and But, n = 1, 2 or 3, have been synthesized by the reactions of cyclopentadienyl titanium trialkoxides with phenylisocyanate. All these complexes have been characterized by the elemental analysis and infrared spectra.
Beiträge zur Chemie des Bors, XCVII Eine Untersuchung des Substituentenaustausches zwischen Trithiadiborolanen / Contributions to the Chemistry of Boron, XCVII An Investigation of the Substituent Exchange between Trithiadiborolanes
Authors: Nöth Heinrich , Taeger Tilman
Published: February 2015

The substituent exchange between trithiadiborolanes has been studied by the 10B isotope technique. A simultaneous exchange of the substituent and the boron atom to which the substituent is bound was observed. This result is explained by a mechanism comprising a conformationally flexible ten membered ring as an intermediate. The exchange occurs not only between differently substituted trithiadiborolanes but also between trithiadiborolanes of one sort.
Reaktion des Orthovanadinsäure-tri-tert-butylesters mit Monocarbonsäuren / Reaction of Tris-tert-butylorthovanadate with Monocarboxylic Acids
Authors: Preuss Fritz , Woitschach Joachim
Published: February 2015

Tris-tert-butylorthovanadate VO(OC4H9)3 undergoes reaction with monocarboxylic acids to yield monomeric VO(OC4H9)(RCOO)2; no VO(OC4H9)2(RCOO) or VO(RCOO)3 could be isolated from the reaction mixture. Polymeric dioxovanadium(V)-monocarbox-ylates(VO2RCOO)n are formed by thermolysis or partial hydrolysis of VO(OC4H9)(RCOO)2; the reaction mechanism is studied and discussed. Syntheses of Ba[VO2(CH3COO)3], Ba[VO2(C2H5COO)3] and N(C4H9)4[V4O8Br(CH3COO)4] are described. All compounds obtained are characterized by IR and 1H NMR spectroscopy as well as by chemical reactions. The carboxyl groups are mostly acting as bidentate ligands.
RbSb3S5 · H2O, ein neuer Formel-und Strukturtyp bei Thioantimoniten / RbSb3S5 · H2O -a New Formula and Structure Type in the Group of Thioantimonites
Authors: Volk Klaus , Schäfer Herbert
Published: February 2015

RbSb3S5 · H2O has been prepared and its structure determined. The compound crystallizes triclinic, P1̄ with a = 1053.6(5) pm, b = 893.8(5) pm, c = 599.0(5) pm, α = 87.09(5)°, β = 100.33(5)° and γ = 102.39(5)°. SbS4-ψ-trigonal bipyramids and SbS3-ψ-tetrahedra are connected together to sheets separated by Rb-ions and water molecules.
Na3(AlSi)Te4 -das erste Hypotelluroalumosilikat / Na3(AlSi)Te4 -the First Hypotelluroalumosilicate
Authors: Weis Jürgen , Schäfer Herbert
Published: February 2015

Na3(AlSi)Te4 has been prepared and analytically characterized. The compound is monoclinic, C2/m, with a = 747 ± 1 pm, b = 434 ± 1 pm, c = 852 ± 1 pm, β = 107.4° ±0.1. The structure can be described as a variant of the a-NaFeO2-type. One half of the octahedral sites is occupied by Na ions while in the other half of these holes Na ions and Al-Si-dumbbells in the ratio 1:1 are randomly distributed.
Kohlenstoffe als Katalysatoren für die Oxydation von schwefliger Säure / Carbons as Catalysts for the Oxidation of Sulfurous Acid
Authors: Zuckmantel Michaela , Kurth R. , Boehm H. P.
Published: February 2015

Conductometric measurements of the catalytic oxydation of dilute aqueous sulfurous acid were used in the comparison of various carbon catalysts, e.g. active charcoals and carbon blacks. The oxidation rate is proportional to (Po2) 1/2 and to the amount of adsorbed HSO3- ions. Basic surface oxides are responsible for the HSO3 -adsorption. The catalytic activity of a carbon is influenced also by other factors than the concentration of basic surface oxides. It is changed by heat treatment of the carbon as well as by chemical treatment of its surface. Treatment with ammonia at 600 °C increases its activity dramatically, absolutely inactive carbon blacks were rendered highly active.
Azido-chelatkobalt(III)-Komplexe / Azido Chelate Cobalt(III) Complexes
Authors: Beck Wolfgang , Kemmerich Timm , Böhme Heiko
Published: February 2015

The preparation and characterization of a series of azido chelate complexes of cobalt(III), N3Co(chel)2B (chel = anionic bidentate ligand, B = base e.g. PPh3, P(OEt)3) and N3Co(chel′)B (chel′ = anionic tetradentate ligand) is reported. In addition, analogous chelate cobalt(III) complexes containing the pesudo halides NCO-, NCS -, CN -, C ≡ CR-, C(CN)3-, CH2NO2- have been prepared.
Ternary Complexes in Solution, XXX Increased Stability Through Intramolecular Stacking in Mixed-Ligand Cu 2+ and Zn 2+ Complexes of 2,2′ -Bipyridyl and Carboxymethyl Aryl Derivatives
Authors: Farkas Etelka , Fischer Beda E. , Griesser Rolf , Rheinberger Volker M. , Sigel Helmut
Published: February 2015

The stability constants of ternary Cu 2+ and Zn 2+ complexes, each of which contains 2,2′-bipyridyl and a carboxymethyl aryl sulfide, were determined in 50% aqueous dioxane. A comparison of the stability of these ternary complexes with those formed with simple carboxylates demonstrates an enhanced stability of the carboxymethyl aryl sulfide containing mixed ligand complexes. This enhanced stability is not due to a thioether-metal ion interaction, but due to an intramolecular aromatic stacking interaction between the aryl moiety of the carboxymethyl aryl sulfide and 2,2′-bipyridyl. Indeed, by UV difference spectra and by PMR measurements it is possible to show that a binary (metal ion-free) stacked adduct between the aromatic moieties of the two mentioned ligands is formed. Furthermore, by studying the binary and ternary systems of Zn 2+ or Cu 2+ , 2,2′-bipyridyl and hydrocinnamate, i.e. 3-phenylpropionate (-S-of carboxymethyl phenyl sulfide is replaced by -CH2-), it becomes obvious that the thioether moiety is not essential for the observation of an enhanced stability of the ternary complexes. PMR shift studies of 2,2′-bipyridyl/Zn 2+ /carboxymethyl aryl sulfide systems confirm the presence of stacking in the corresponding ternary complexes. Depending on the kind of the ternary metal ion complex the stability enhancement, due to the intramolecular stacking between the aromatic parts of the coordinated ligands, is between about 0.2 to 0.5 log unit.
Oxidation von Mercapto-Carbonyl-Mangankomplexen / Oxidation of Mercapto Carbonyl Manganese Complexes
Authors: Küllmer Volker , Röttinger Erika , Vahrenkamp Heinrich
Published: February 2015

Chemical oxidation of the mercapto carbonyl manganese complexes (Me3P)2(CO)3Mn-SX (1), (Me3P)2(CO)5Mn2(SX)2 (2), and (CO)8Mn2(SX)2 (3) (X = H, SnMe3) were investigated. From the SH complexes no identifiable products could be obtained. For X = SnMe3, the iodine oxidation of 2 yielded (Me3P)2(CO)5Mn2S2 (5), that of 3 gave (CO)15Mn4S4 (7), both containing bridging disulfide ligands. The crystal structure of 7 was determined.
Zur Darstellung und Kristallstruktur des SrZnSb2 / On the Preparation and Crystal Structure of SrZnSb2
Authors: Brechtel Erwin , Cordier Gerhard , Schäfer Herbert
Published: February 2015

SrZnSb2 has been prepared and characterized analytically and structurally. The compound crystallizes in the orthorhombic system with a = 2305 ± 5 pm, b = 437 ± 1 pm, c = 446 ± 1 pm, Pnma-D2h
16. Zn- and Sb-atoms form distorted fourfold pyramids, connected by common edges in the basis to two-dimensional sheets. These sheets are separated by double layers of Sr-atoms in which further Sb-atoms are located building four-cornered networks.
Ligandenfeldspektroskopische Untersuchungen an Übergangsmetall -Aluminium -Tetraalkoxiden / Ligand Field Spectroscopic Studies of Transition Metal Aluminium-Tetraalkoxides
Authors: Stumpp Eberhard , Hillebrand Uwe
Published: February 2015

The preparation and the electronic spectral properties of compounds M[Al(OR)4]2 (M = Co, Ni, Cu and R = CH3, C2H5, n-C3H7, n-C4H9) are described. The spectral data are used in conjunction with ligand field theory in deducing the structures of the compounds. The spectrum of green Ni[Al(OR)4]2 is interpreted as a Ni(OR)6 octahedron sharing faces with two Al(OR)4 tetrahedrons. It is proposed that Co 2+ and Cu 2+ are in a distorted octahedral coordination. The alkoxide ligands have been fitted into the spectrochemical and the nephelauxetic series. They are close to H2O in this series.
Semiempirische SCF-Rechnungen zur Hydroxypyridin-Pyridon-Tautomerie / Semiempirical SCF-Calculations on the Hydroxypyridine-Pyridone-Tautomerism
Authors: Fabian Walter
Published: February 2015

The electronic spectra of a series of substituted 4-hydroxypyridones are calculated by the CNDO/CI-method. Best agreement between observed and calculated transition energies is obtained when the geometry of the pyridone-form is assumed. In addition, MINDO/2-calculations predict the pyridone tautomer to be the more stable one in most cases.
The Delayed Luminescence of Tryptophan in Aqueous LiCl Solutions at 77 K
Authors: Yamashita Shozi , Tomita Giiti
Published: February 2015

The effect of LiCl on the delayed luminescence caused by the recombination of photo -ejected electrons with tryptophan cations in aqueous solutions was investigated at 77 K. The luminescence intensity strongly depended on LiCl concentration. At high LiCl concentrations, the intensity of the fast decay component of the recombination fluorescence decreased to a constant value, whereas that of the slow decay component inversely increased. The intensity of the recombination phosphorescence was weak and unchanged in low LiCl concentration range but increased steeply above 7 M LiCl. NO3̄, electron scavenger, quenched both the recombination fluorescence and phosphorescence, but the degree of the quenching decreased rapidly in the order of the fast decay component of the recombination fluorescence, the slow decay component of the recombination fluorescence, the recombination phosphorescence. Furthermore, the quenching efficiency of NO3̄ for each recombination luminescence was found to diminish with increasing LiCl concentration. The distribution of photo-ejected electrons to shallow-and deep-traps, dependent on LiCl concentration, was discussed from results obtained.
Über eine neue Präparationstechnik in der Feststoffchemie, I Hochtemperatursynthesen mit CO2-Laser / A New Preparation Technique in Solid State Chemistry, I High Temperature Reactions with CO2-Laser
Authors: Müller-Buschbaum Hk. , Pausch H.
Published: February 2015

A new high temperature method using a CO2-Laser radiation is reported. Its application on solid state reactions in air or in defined gas atmospheres is described.
Über die Darstellung und röntgenographische Untersuchung von Cu2SrGeS4 und Cu2BaGeS4 / On the Preparation and X-ray Investigation of Cu2SrGeS4 and Cu2BaGeS4
Authors: Teske Chr. L.
Published: February 2015

Single crystals of Cu2SrGeS4 and Cu2BaGeS4 were prepared by using molten bromides as solvents. The compounds crystallize isotypically to their homologous thiostannates(IV) [1, 2]. (Cu2SrGeS4: Space group P32, a = 614,3, b = 614,3 and c = 1528,2 pm; Cu2BaGeS4: Space group P31, a = 621,5, b - 621,5 and c = 1553,4 pm). The atomic parameters and interatomic distances are reported.
Tetraquecksilbermethane, II [1]Tetrakis(halogenoquecksilber)-methane C(HgX)4 (X = F, Cl, Br und I): Synthesen und Schwingungsspektren / Tetramercurimethanes, II [1]Tetrakis(halomercuri)methanes C(HgX)4 (X = F, Cl, Br und I): Syntheses and Vibrational Spectra
Authors: Breitinger Dietrich , Morell Wilfred , Grabetz Knut
Published: February 2015

The complete series of tetrakis(halomercuri)methanes C(HgX)4 (X = F, Cl, Br and I) was prepared by metathesis of tetrakis(acetoxymercuri)methane and aqueous hydrofluoric acid and solutions of halides (Cl-, Br-, and I-), respectively. All compounds are insoluble in most common solvents, but partly soluble in dimethylsulfoxide. Complete vibrational spectra indicate more or less ideally tetrahedral molecules C(HgX)4 in all cases. The originally triply degenerate valence vibrations of the CHg4 entities and the force constants for the C-Hg bonds show distinct correlations with the electronegativities of the halides X. On the other hand the totally symmetrical valence vibrations of CHg4 were found to be highly sensitive to variations in X, mainly due to coupling with the valence vibrations of the Hg-X-groups of the same symmetry species. Some analogies in the vibrational behaviour of the CHg4 fragments and of the isosteric NHg4 core in tetramercurioammonium complexes were observed and discussed.
Na3Cu4S4-ein Thiocuprat mit unverknüpften 1
∞[Cu4S4] -Ketten / Na3Cu4S4-a Thiocuprate with Isolated 1
∞[Cu4S4]-Chains
Authors: Burschka Christian
Published: February 2015

Na3Cu4S4 can be prepared by fusion reaction of copper with Na2CO3 and sulfur at 600 °C. The structure (orthorhombic, Pbam, a= 14,624(6), 6 = 7,163(3), c = 3,771(1)Å; Z = 2) solved from x-ray diffractometer data (R = 0,024; 391 obs. reflections) shows unlinked copper-sulfur chains of the kind already observed in two-dimensional copper-sulfur networks.
Cyclotri(λ3-phospliazane) / Cyclotri(λ3-phosphazanes)
Authors: Zeiss Werner , Barlos Kleomenis
Published: February 2015

P-perhalogenated cyclotri(λ3 -phosphazanes) 3 a, b are obtained from the reaction of 1 or 2 with excess PX3 (X = Cl, Br). Under mild reaction conditions 4-7 are found to be intermediates. The existence of a six-membered ring trimer is proven by NMR and mass spectroscopy. No dimer (XPNMe)2 could be detected.