bluuebunny/crossref_metadata_2025_split huggingface dataset:
Einzelvorgänge der thermischen Umwandlung von Magnesiumhydroxid ins Oxid / Details of the Thermal Conversion of Magnesium Hydroxide into Oxide
Authors: Koubowetz Franz , Noller Heinrich 
Published: March 2015

The decomposition of Mg(OH)2 was studied by means of thermogravimetry, IR-spectroscopy, DTA, thermodesorption with GC and MS, and X-ray analysis.
Water was evolved in two steps, at 230 °C (a small amount only) and 380 °C. The band at 3700 cm-1, that is assigned to OH groups of Mg(OH)2, was not present above 270 °C. Assuming that only surface OH groups appear in the IR spectrum, but no bulk OH groups, the steps at 230 °C and 380 °C can be attributed to the decomposition of the surface and the bulk, resp.
Improvements in the Preparation of Spin-Labeled Phosphorus Compounds of Potential Cytotoxicity
Authors: Sosnovsky G. , Konieczny M. 
Published: March 2015

The syntheses of spin-labeled phosphorus compounds containing the ethyleneimine, —N, and nitrogen mustard, —N(CH2CH2Cl)2, moieties were reinvestigated. By a judicious choice of solvents, stoichiometry, and reaction conditions yields of these compounds have been optimised. Thus, monoradical diamidates (5) and (9) wore prepared in 95 and 82% yields, respectively, and diradical monoamidates (7) and (12) were prepared in 95 and 45% yields, respectively. The nitrogen mustard derivative (16) was obtained in 92% yield.
[xxx]
Yields of 2-Deoxy-D-gluconic, D-Gluconic and Other Sugar Acids in Gamma-Irradiated Aqueous Solutions of D-Glucose
Authors: Esterbauer Hermann , Schubert Jack , Sanders Edward B. , Sweeley Charles C. 
Published: March 2015

The yields of 2-deoxy-D-gluconic, D-gluconic and other sugar acids from 60Co-gamma irradiated (dose rate = 4 Krads/min) D-glucose solutions are reported. The acids produced upon radiolyses were separated from glucose and neutral products by anion exchange, assayed by gas chromatography of the trimethylsilyl derivatives, and definitive identification made by mass spectrometry. In He degassed, irradiated 0.055 M glucose G(2-deoxy-D-gluconic acid) = 0.62 and G(D-gluconic acid) = 0.20. The approximate G values for the other identified acids are: glyceric acid 0.03, 2-deoxy-tetronic acid 0.04, tetronic acid 0.03, 4-deoxypentonic acid 0.02, deoxyketogluconic acid 0.17.
In N2O saturated glucose solutions D-gluconic acid yields increased by a factor of ∼1.9 while that of 2-deoxy-D-gluconic acid increased by a factor of only ∼ 1.1.
Photochemistry of (Iso)Alloxazines, V Mechanism of the Photoreaction of Flavin with 1,4-Cyclohexadiene and Analogous Compounds
Authors: Knappe Wolfgang-R. 
Published: March 2015

On illumination flavin reacts from its triplet state with dihydroaromatic systems at room temperature yielding 1,5-dihydroflavin. Substrates which are substituted with methyl groups to hinder aromatisation (3,3-dimethyl-1-phenyl-1,4-cyclohexadiene, ergosterol, N-methylacridan, 1,3,10-trimethyl-1,5-dihydro-5-deazaisoalloxazine) yield at -40 °C 4a-substituted 4a,5-dihydroflavins (adducts), which on warming split homolytically, yielding a 1:1:1-mixture of 1,5-dihydroflavin/starting flavin/dimerized substrate after disproportionation and dimerisation, resp.
In the case of unblocked substrates these adducts are not UV-detectable even at -80 °C but split heterolytically, yielding 1,5-dihydroflavin and oxidized substrate in a 1:1-ratio.
Notizen: Preparation and Crystal Structure of NiHg
Authors: Pušelj M. , Ban Z. 
Published: March 2015

A single phase binary amalgam of the composition NiHg was found to form at room temperature after an extended period of time (approx. 2 years).
X-ray powder diffraction analysis enabled us to determine the crystal structure. The compound crystallizes tetragonally with a = 4.22 Å and c = 3.14 Å. It belongs to L 10 crystal structure type.
Complexes of Oxamic Acid with Cu(II), Ni(II), Co(II) and Cr(III)
Authors: Galinos A. G. , Tsangaris J. M. , Kouinis J. K. 
Published: March 2015

The preparation of the complexes of oxamic acid with Cu(II), Ni(II), Co(II) and Cr(III) is reported. From the study of IR, diffuse reflectance spectra and the magnetic moments it is concluded that in all complexes the metal is coordinated with the amidic nitrogen, after ionization of one amidic hydrogen, and with the carboxyl oxygen.
Octahedral structures are proposed for the complexes K2[Ni(oxamic)2] · 2 H2O and K3[Cr(oxamic)3] and planar configurations for K2[Cu(oxamic)2] and K2[Co(oxamic)2].
Funktionelle Trimethylphosphinderivate, VI1 Lithium-dimethylphosphinomethanid, (CH3)2PCH2Li, Tetraorganodiphosphinomethane, R2PCH2P(CH3)2 und Tris(dimethylphosphinomethyl)phosphin, P[CH2P(CH3)2]3 Functional Derivatives of Trimethylphosphine, VI1 / Lithium-dimethylphosphinomethanide, (CH3)2PCH2Li, Tetraorganodiphosphinomethanes, R2PCH2P(CH3)2, and Tris(dimethylphosphinomethyl)phosphine, P[CH2P(CH3)2]3
Authors: Karsch Hans H. , Schmidbaur Hubert 
Published: March 2015

Dialkylmethylphosphines R2PCH3 are metallated by tert-C4H9Li to give LiCH2PR2 (la: R = CH3, lb: R. = tert-C4H9). la introduces the eCH2P(CH3)2-ligand into L3CoCl to
give [xxx] (2). With diorganochlorophosphines R2PCl (R = CH3, tert-C4H9,
C6H5) and with triphenylphosphite P(O Ø)3 the new biphosphinomethane derivatives (CH3)2PCH2PR2 (4 a-c) and P[CH2P(CH3)2]3 (5) are formed, resp.. Tetramethyldiphosphinomethane (3 a) is also obtained from (CH3)2PCl and Li2CH2. Some properties and spectroscopic data of these new materials are described.
Darstellung und Untersuchung teilweise hydrolysierter Natriumtetrakis(methoxy)borate / Preparation and Investigation of Partially Hydrolyzed Sodium tetrakis(methoxy)borates
Authors: Heller Gert , Horbat Ferdinand 
Published: March 2015

Abstract
By careful hydrolysis of B(OCH3)3 in the presence of NaOCH3 in absolute methanol, crystallized Na[B(OCH3)4] · CH3OH · 1.5 H2O has been prepared. The properties, IR, NMR spectra and X-ray parameters (Pbca; a = 18.2; b = 13.7; c = 19.5 Å; D25
exp = 1.2 g/cm3) are described. The crystal structure was determined by single crystal diffractometer data and refined to a conventional R value of 4.5.
The Photochemically-Induced Degradation of (η5-C5H5)M(CO)3CH3 Complexes (M = Cr, Mo, W)
Authors: Rausch M. D. , Gismondi T. E. , Alt H. G. , Schwäbzle J. A. 
Published: March 2015

Abstract
The photolysis of (η5-C5H5)M(CO)3CH3 complexes (M = Cr, Mo, W) in solvents such as pentane, benzene or tetrahydrofuran results in cleavage of the methyl-metal sigma-bond and formation of the corresponding [(η5-C5H5)M(CO)3]2 analogs as well as methane. Deuterium labeling studies indicate that, for the molybdenum system, abstraction of a hydrogen atom from a cyclopentadienyl ring by the methyl group represents a major reaction pathway for the production of methane. Photolysis of (η5-C5H5)M(CO)3CH3 complexes in CHCl3 produces high yields of [(η5-C5H5)CrCl2]2 in the case of the chromium analog, or (η5-C5H5)M(CO)3Cl where M = Mo or W.
Synthese, Strukturfestlegung und Dissoziationsgleichgewicht eines 15N-markierten Diazadiphosphetidins / Synthesis, Structure Determination, and Dissociation Equilibrium of a 15N-Labeled Diazadiphosphetidine
Authors: Appel Rolf , Halstenberg Mechthild , Knoll Fritz 
Published: March 2015

Abstract
The 15N-labeled diazadiphosphetidine (3a) was prepared to confirm the proposed ring structure by 1H, 31P, 13C, and 15N NMR spectroscopy. The temperature dependence of the NMR spectra suggests a dissociation equilibrium which could be verified by an exchange reaction.
Neue Hochdrucksynthesen von bekannten und unbekannten Derivaten des Co2(CO)8 aus metallischem Kobalt / New High Pressure Syntheses of Known and Unknown Derivatives of Co2(CO)8 Starting from Cobalt Metal
Authors: Behrens Helmut , Hüller Rolf , Jungbauer Anton , Merbach Peter , Moll Matthias 
Published: March 2015

The following known and novel cobalt carbonyl complexes are formed by reactions of cobalt metal with bipy, phen, Ph2P-CH2-CH2-PPh2 (P͡P), PPh3, Ph2P-CH2-CH2-NEt2 (P͡N), InCl, SnX2 (X = Cl, Br, I), Cd and HgBr2 under CO pressure (200 bar):
[Co(bipy)3][Co(CO)4]2, [Co(phen)3][Co(CO)4]2, [Co2(P͡P)3(CO)4][Co(CO)4]2; Co2(CO)6 (PPh3)2, Co2(CO)6 (P͡N)2; [Co(CO)4]2SnCl2, {[Co(CO)4]2InCl}2; [Co(CO)3PPh3]2SnX2(X = Cl, Br, I), [Co(CO)3(P͡N)]2SnCl2, [Co(CO)3(P͡N)]2M (M = Cd, Hg).
Darstellung und Kristallstruktur von MgNi2,5B3 und Li1,2Ni2,5B2 / Preparation and Crystal Structure of MgNi2,5B2 and Li1,2Ni2,5B2
Authors: Jung Walter 
Published: March 2015

The ternary borides MgNi2,5B2 and Li1,2Ni2,5B2 have been prepared and investigated by X-ray methods. They are isotypic and crystallize hexagonal in the space group P6222—D4
6-with the following constants :
MgNi2.5B2 α = 4.887 ± 0.002 Å, c = 8.789 ± 0.004 Å;
Li1.2Ni2.5B2 a = 4.842 ± 0.002 Å, c = 8.664 ± 0.004 A.
The structure contains boron-pairs and can be derived from the CeCo3B2-type of structure.
Darstellung von Phthalocyaninen von Ib-Elementen in aprotischen Lösungsmitteln / Preparation of Phthalocyanines of lb-Elements in Aprotic Solvents
Authors: Homborg Heinrich , Kalz Winfried 
Published: March 2015

Abstract
The double decomposition of (TDBA)LiPc(2-) with halocomplexes of the lb-elements is investigated in nonpolar aprotic solvents. Phthalocyanines of the formula MLiPc(2-) are isolated only for the univalent cations Cu(I) and Ag(I), but not for Au(I). The impure AgLiPc(2-) is light sensitive. In contrast to earlier observations only oxidation products of the phthalocyanine anion are obtained in the presence of Cu(II) and Au(III). The preparation of Ag(II) and Au(II) phthalocyanines failed.
N-Sulfonylsulfimides / N-Sulfonylsulfimides
Authors: Roesky Herbert , Aramaki Minoru , Schönfelder Lothar 
Published: March 2015

Abstract
(CF3SO2NSO2)2 (1), a compound with a four-membered ring, was prepared from CF3SO2NSO and SO3. 1 as well as (FSO2NSO2)2 form 1:1 adducts with S4N4 , pyridine and pyridine carbonitrile-4 (2a-2f). By comparison with FSO2NCOS4N4 it was shown that a dipolar type of addition had occured. In contrast the reaction of 1 and (FSO2NSO2)2 with aromatic nitriles yields 1:2 cycloaddition products (3a-3g) which were characterized on the basis of mass spectra. The six-membered rings of 4a-4b which contain carbon, nitrogen and sulfur atoms were obtained from the reaction of isocyanates with (FSO2NSO2)2 or (CF3SO2NSO2)2. 4-BrC6H4NCO and SO3 react in a similar way to yield 5. The starting materials are extremely sensitive to moisture while most of the adducts can be handled in open air without decomposition.
NaMgAs(Sb) -Ternäre Verbindungen mit modifizierter Cu2Sb-Struktur / NaMgAs(Sb) -Ternary Compounds in a Modified Cu2Sb Structure
Authors: Krenkel Burkhard , Schuster Hans-Uwe 
Published: March 2015

Abstract
The compounds NaMgAs and NaMgSb were prepared and their structures determined by powder and single crystal data. NaMgAs and NaMgSb crystallize in a modified Cu2Sb-type-structure, space group P4/nmm-D7
4h. The cell parameters for the tetragonal com-pounds are:
Neue Intercalationskomplexe von Eisen(III)oxichlorid, FeOCl / New Intercalation Complexes of Iron(III) Oxichloride, FeOCl
Authors: Weiss Armin , Sick E. 
Published: March 2015

Abstract
Nonstoichiometric iron (III) oxichloride is capable of intercalating a large number of guest molecules with Lewis base character, e.g. dimethylsulfoxide, formamide, hexa-methylphosphortriamide, or alkylamines, while the reactions of stoichiometric FeOCl are restricted to pyridine and its derivatives only. The nonstoichiometric host lattice can be synthesized either by direct reaction form Fe2O3, FeCl3 and Fe or by reduction of the stoichiometric compound. In the latter case the basal spacings of the intercalation complexes depend upon the degree of reduction and the electrolyte concentration. The highly expanded lattice is rapidly hydrolyzed in the presence of water.
N-Organoquecksilber-triazene - Darstellung und Eigenschaften / N-Organomercury-triazenes - Preparation and Properties
Authors: Peringer Paul 
Published: March 2015

Abstract
The symmetric N-organomercury-triazenes C6H4X-N = N-N(HgC6H5)-C6H4X (X = H, 2-F, 2-Cl, 2-Me, 2-NO2, 3-Cl, 3-NO2, 4-Cl, 4-Me and 4-NO2) were prepared. IR and PMR measurements indicate monodentate structures associated with rapid C6H5Hg exchange in solution. MS and UV data are given.
Reaktionen von Übergangsmetall-Tyrosinkomplexen mit Kaliumnitrosodisulfonat / Reactions of Transition Metal-Tyrosine Complexes with Potassium Nitrosodisulfonate
Authors: Von Martius Konstantin , Schwarzhans Karl 
Published: March 2015

Abstract
Transition Metal-Tyrosine Complexes, Oxidation Tyrosine and the copper(II), cobalt(II) and nickel(II) complexes of this amino acid have been oxidized with potassium nitrosodisulfonate. The chemical oxidation follows the enzymatic pathway, i.e. the Raper-Mason mechanism through the intermediate of dopachrome. The complexes take a considerable shorter reaction time compared with uncomplexed tyrosine. Analytical and spectroscopic data of the resulting black oxidation products indicate a composition comparable with that of natural melanines.
Übergangsmetall-Methylen-Komplexe, VI [1] Zur irreversiblen µ-Methylen/Carbonyl-Isomerie zweikerniger Cobalt-Komplexe mit bifunktionellen Methylen-Liganden / Transition Metal Methylene Complexes, VI [1] On the Irreversible µ-Methylene/Carbonyl Isomerization of Binuclear Cobalt Complexes with Bifunctional Methylene Ligands
Authors: Herrmann Wolfgang , Schweizer Ilona 
Published: March 2015

Abstract
Ethyl diazoacetate (2 a) and tert-butyl diazoacetate (2 b) are converted into the metal stabilized, doubly bridging alkoxycarbonyl carbenes upon photolysis with (ƞ5-C5H5)Co(CO)2 (1) in tetrahydrofurane at -110°C. Although the yields of µ-dicarbonyl-µ-ethoxycarbonylmethylene- bis(ƞ5-cyclopentadienylcobalt) (3 a) and the corresponding ieri-butyl derivative (3b) are low, both compounds attract considerable attention due to an unexpected and hitherto unknown irreversible carbonyl bridge opening process with concomitant µ-methylene rearrangement. These isomerizations have been established by IR and 1H NMR methods to be first order intramolecular processes.
Cleavage Reactions of Oxazolin-5-ones Reactions with 4-Substituted-2-aryl-2-oxazolin-5-ones
Authors: Kassab Nazmi , Harhash Abdul , Elbahaii Said 
Published: March 2015

Abstract
The oxazoline ring in 4-arylazo-2-aryl-2-oxazolin-5-ones (1) is converted to triazolyl-carbonyl amino acids 2, 4 and 6 by the nucleophiles glycine, anthranilic and p-aminobenzoic acids, respectively. The arylidene derivatives 3 of 2-triazolyl-2-oxazolin-5-one were obtained. Triazolylbenzoxazinones 5, were obtained by the ring closure of the amino acid 4.
Grignard's reagent effected ring cleavage of the oxazolinone ring in 4-cinnamylidene-2-aryl-2-oxazolin-5-ones yielding the carbinols 8, the latter cyclizes either in acidic or alkaline medium to afford either benzotropilidenes or oxazolines, respectively.
Notizen: N-Salicyliden-D.L-valinato-thioharnstoffkupfer (II)-Komplex / N-Salicylidene-D,L-valinato-thioureacopper( II) Complex
Authors: Švajlenová O. , Krätsmár-Šmogrović J. 
Published: March 2015

Abstract
N - Salicylidene - D,L - valinato - thiourea - cop - per(U) complex reacts with thiourea to give magnetically diluted stable Cu(II) complex Cu(salal-D,L-val)(tu). This compound shows similar magnetic and spectral properties to those of N-salicyhdene-glycinato-thiourea-copper(II) complex [1].
Notizen: Unusual Formation of Carbamate Salts: an Experimental Proof for the Mechanism of the Removal of Carbobenzoxy Group by Catalytic Hydrogenolysis
Authors: Schőn István , Kisfaludy Lajos 
Published: March 2015

Abstract
Carbamate Salts, Catalytic Hydrogenolysis Catalytic hydrogenolysis of Z-Gly-NH2 and Z-Ala-NH2 resulted in the corresponding free amides and carbamate salts. This observation is a further experimental proof that carbamic acid derivatives are intermediates of hydrogen-olytic removal of carbobenzoxy group under neutral conditions. The ratio of the formation of the two compounds is dependent on the solvent, concentration and chemical structure. The carbamate salts can be acylated without difficulties under the conditions of peptide bond formation.
Ethylene Insertion with Soluble Ziegler Catalysts: Direct Insight into the Reaction Using Enriched 13C2 H4 and 13C NMR Spectroscopy II. The System Cp2TiMeCl/AlMeCl2/13C2H4
Authors: Fink Gerhard , Fenzl Wolfgang , Mynott Richard 
Published: March 2015

Abstract
The elementary processes involved in the polymerization of ethylene by soluble Ziegler catalysts of the type Cp2TiMeCl/AlMeCl2 have been studied by 13C NMR spectroscopy. Using 13C-enriched ethylene, detailed information was obtained directly on the system in the course of the polymerization. No spectroscopic evidence was found for precoordination of the monomer. The development of the oligomer distribution, which could be followed spectroscopically, proves that the mechanism proposed by Olivé cannot be correct. These experiments show conclusively that the ethylene is inserted into the titanium-carbon bond.
Metallkomplexe mit biologisch wichtigen Liganden XXVI : Reaktionen von Bis(α-aminoacidato)platin(II)-Komplexen mit Nitrosylsalzen: Nitrosylplatin-Komplexe[xxx] + X- (X = BF4 , PF6 , SbF6 )/Metal Complexes with Biologically Important Ligands XXXVI : Reaction of Bis(α-aminoacidato) Platinum(II) Complexes with Nitrosyl Salts: Nitrosyl Platinum Complexes[xxx]+X-(X = BF4 , PF6 , SbF 6)
Authors: Ambach Eberhard , Beck Wolfgang 
Published: March 2015

Abstract
The reactions of the glycinato, alaninato, or cyclo-leucinato chelate platinum complexes trans -[xxx] with nitrosyl salts NO+X- (X = BF4, PF6, SbF6) in acetonitrile at -20 °C give the blue nitrosyl compounds {(0N)Pt [xxx] X·nCH3CN. Nitrosation at the amino group is not observed. The spectroscopic data of the nitrosyl complexes (IR, XPE) are reported. [xxx] + PF6
- reacts with lithium halides or halogens in DMF to give the platinum (IV) complexes X2Pt(NH2CH2CO2)2 (X = CI, Br, I).
Oxidative Knüpfung einer Phosphor-Phosphor-Bindung unter Einwirkung von Ag(I)- bzw. Cu(II)-Ionen: Synthese und Struktur von [(C6H5)PH2Ag{μ-(C6H5PH)2}]2 (AsF6)2, einem sechsgliedrigen Silber-Phosphor-Ring / The Oxidative Formation of a Phosphorus-Phosphorus Bond in the Presence of Ag(I) and Cu(II) Ions: Synthesis and Structure of [(C6H5)PH2Ag{μ-(C6H5PH)2}]2 (AsF6)2, Containing a Six-Membered Silver-Phosphorus Ring
Authors: Jones Peter G. , Roesky Herbert W. , Grützmacher Hansjörg , Sheldrick George M. 
Published: March 2015

Abstract
The reaction between AgAsF6 and phenylphosphine proceeds with formation of a phosphorus-phosphorus bond. The main product 1, [(C6H5)PH2Ag{μ-(C6H5PH)2}]2 (AsF6)2, was characterized by an X-ray structure determination [P1̄, a = 919.0(4), b = 1109.8(4), c = 1316.4(5) pm, α = 97.48(3), β = 107.25(3), γ = 102.71(3)°, Z = 1, R = 0.057 for 2806 observed reflections], 1 contains Ag2P4 rings; the silver atoms are further coordinated by phenylphosphine ligands, thus acquiring trigonal coordination geometry. A similar reaction is observed with Cu(AsF6)2, forming the analogous Cu(I) complex 2.
Rearrangement of 14β-Hydroxy-12β-sulfoxy-steroids to 13,17-Seco-12,17-cyclo-steroids; a 2D-NMR Analysis
Authors: Habermehl Gerhard G. , Hammann Peter E. 
Published: March 2015

Abstract
The rearrangement of 3-oxo-14β-hydroxy-12β-methanesulfoxy-card-20(22)-enolide and 14β-hydroxy-12β-methanesulfoxy-pregnane-3,20-dione during elimination of the sulfoxygroups was studied. By means of 2D-NMR analysis the structures were determined as 13,17-seco-12,17-cyclo-steroids.
2,5-Dihydro-1,2,5-azoniastannaboratole: Nützliche Vorstufen für die Heterocyclensynthese / 2,5-Dihydro-1,2,5-azoniastannaboratole: Useful Steps for the Synthesis of Heterocycles
Authors: Kerschl Susanna , Wrackmeyer Bernd 
Published: March 2015

Abstract
Organoboration, Heterocycles, Multinuclear NMR 1,1-Organoboration of diethylamino-dimethyl-(1-propynyl)stannane (6), formed by an exchange reaction between the bis(propynyl)-(4) and bis-(diethylamino)dimethylstannane (5), with trimethyl-(2a) or triethylborane (2b) leads to highly reactive new heterocyclic compounds (7). Both, the coordinative N→B and the weak Sn-N bond are readily attacked by H-acidic compounds. Ammonia or primary amines are used as examples. Multinuclear NMR (1H, 11B, 13C, 15 N, 119Sn) data serve for the characterization.
Ba2Sb3, eine neue Zintlphase mit Sb6-Ketten / On Ba2Sb3, a New Zintl Phase with Sb6-Chains
Authors: Eisenmann Brigitte , Jordan Hanna , Schäfer Herbert 
Published: March 2015

Abstract
The new compound Ba2Sb3 crystallizes in the monoclinic system, space group P21/c (No. 14) with the lattice constants a = 693.4(3) pm, b = 1345.3(6) pm, c = 1581.7(6) pm, β = 90.25(15)°.
The compound is isotypic to the Sr2Sb3 structure with discrete Sb6
8- chain anions
Chloronitrosylkomplexe von Ruthenium(II) Die Kristallstruktur von (PPh3Me)2[Ru(NO)Cl4]2-2 CH2Cl2 / Chloro Nitrosyl Complexes of Ruthenium (II) The Crystal Structure of (PPh3Me)2 [Ru(NO)Cl4]2 • 2 CH2Cl2
Authors: Fenske Dieter , Demant Udo , Dehnicke Kurt 
Published: March 2015

Abstract
Ruthenium trichloride, obtained from its hydrate with thionyl chloride, reacts with excess trichloronitrom ethane yielding polymer [Ru(NO)Cl3]; by addition of triphenylmethylphosphonium chloride in dichlorom ethane (PPh3Me)2[Ru(NO)Cl4]2 · 2 CH2Cl2 is obtained, the IR spectrum of which is reported and assigned. Its crystal structure was determined with X-ray diffraction data (6404 independent observed reflexions, R = 0.068). Crystal data at -90 °C: a = 1145, b = 1591, c = 1406 pm, β = 96,0°, Z = 2, space group P21/C. The structure consists of PPh3Me⊕ cations, centrosymmetric anions [Ru(NO)Cl4]2
2⊖ nearly fulfilling C2h symmetry, and CH2Cl2 molecules. In the anions the Ru atoms are linked via chloro bridges; the nitrosyl groups occupy axial positions with bond distances RuN of 175 and NO of 113 pm, bond angle RuNO 172.7°.
Zur Stereochemie des freien Elektronenpaares in Verbindungen des vierwertigen Tellurs: Verzerrtes TeCI6
2-Oktaeder in [H3N(CH2)3NH3TeCI6 regulär oktaedrisches Anion in H3N(CH2)3NH3SnCI6 / On the Stereochemistry of Lone Pair Electrons in Compounds with Tetravalent Tellurium: Distorted TeCl6
2-Octahedron in [H3N(CH2)3NH3]TeCl6, Regular Octahedral Anion in [H3N(CH2)3NH3]SnCl6
Authors: Abriel Walter , Friedrich Claudia 
Published: March 2015

Abstract
Using 293 K diffractometer intensity data, the structures of [H3N(CH2)3NH3]TeCl6 and [H3N(CH2)3NH3]SnCl6 have been determined by single crystal X-ray technique and refined to a final of 0.027 and 0,029, respectively. The yellow crystals of the tellurate are orthorhombic (space group Pnma) with a = 22.952(2), b = 7.5414(4), c - 7.801(1) Å and Z = 4. This structure contains distorted TeCl6
2- octahedra (distances Te - Cl min. 2.426(1), max. 2.672(1) Å ) with approximate 2mm point symmetry. In contrast, the SnCl6
2- ion in the second title com pound is octahedral with only small deviations from m 3m symmetry (distances Sn -Cl mean: 2.438(3) Ä ). The colourless crystals of this tin com pound are orthorhombic (space group Pnma) with a - 17.6082(9), b = 7.1809(3), c = 10.190(1) Å and Z = 4. Considering the TeX6
2- (X = Cl, Br, I) salts known to date, a distorted species is an exception, although a distortion is predicted by the VSEPR theory. The results agree with the rules for the appearance of a static stereochemical effect of the lone pair electrons in the TeX6
2- species
NaLiS: Ein weiteres Interalkalimetallsulfid / NaLiS: A nother Inter Alkaline Metal Sulphide
Authors: Sabrowsky Horst , Thimm Alfred , Vogt-Mertens Petra 
Published: March 2015

Abstract
The colourless com pound NaLiS has been prepared and its structure determined by single crystal X-ray diffraction techniques. The very hygroscopic NaLiS crystallizes in the tetragonal space group P4/nmm (Z = 2) with the cell parameters a = 402.6(1), c = 649.5(2) pm. The structure was solved from 720 counter reflections (216 symmetry independent reflections) by differential Fourier syntheses. Refining gives a least squares residue of 0.024.
The anti-PbFCl-type structure is characterized by layers of LiS4/4-tetrahedra connected by their edges in two dimensions and 2 interspersed layers of sodium