bluuebunny/crossref_metadata_2025 huggingface dataset:
Reaktionen von 1-Alkoxy-isoindoleninen / Reactions of 1-Alkoxy-isoindolenines
Authors: Kreher Richard , Hennige Hans
Published: February 2015

Reactions of 1-alkoxy-isoindolenines with electrophilic, nucleophilic and dienophilic reagents have been investigated as a general route for the synthesis of substituted isoindoles and isoindolenines.
Polarographic Reduction of Zinc and Thorium in Furfuryl Mercaptan Media
Authors: Sαxena R. S. , Sheelwant S. S.
Published: February 2015

The reduction of Zn and Th in furfuryl mercaptan has been found to be irreversible and diffusion-controlled in 50% ethanolic media and 0.1 M NaClO4. The values of kinetic parameters - transfer coefficient (α), formal rate constant (K°f,h) - for the electrode reactions were determined by KOUTECKY’S method as extended by MEITES and ISRAEL. The values of ΔH, ΔG and ΔS have also been reported.
Infra Red and Ultra Violet Spectra of Some Divalent Transition Cupferrone Complexes
Authors: Abou El Ela A. H. , Abdel Kerim F. M. , Afifi H. H. , Aly H. F.
Published: February 2015

The IR and UV absorption spectra of the ammonium salt of cupferrone and manganese, cobalt, nickel, copper and zinc divalent cupferrate complexes are investigated. The IR absorption bands identified in the region 400-4000 cm-1 are given and assigned, especially those three related to M-O vibrations.

In the UV absorption spectrum of the cupferrone metal complexes a characteristic shift in the maxima and minima appears.
Über die Reaktionen von Phosphanen MenP[OCH(CF3)2]3-n mit Hexafluoraceton / Reactions of Phosphanes MenP[OCH(CF3)2]3-n with Hexafluoroacetone
Authors: Röschenthaler Gerd-Volker
Published: February 2015

The stable phosphanes Me2POCH(CF3)2 and MeP[OCH(CF3)2]2 have been prepared and reacted with hexafluoroacetone yielding 1,2-oxaphosphetanes. The analogous reaction with Me2PF was carried out giving a 1 : 1 : 1 mixture of a 1,3,2-, a 1,3,4-dioxaphospholane, and a 1,2-oxaphosphetane. P[OCH(CF3)2]3 did not react with hexafluoroacetone. The new compounds were characterized by NMR, mass spectrometry and elemental analysis
Zur Bildung makrocyclischer B-N-Verbindungen / About the Formation of Macrocyclic B-N-Compounds
Authors: Meller A. , Füllgrabe H. J.
Published: February 2015

By the reaction of 2-alkyl-4,6-dichloro-1,3,5-trimethylborazines with bis(trimethylsilyl)amine and pyrolysis of the products in vacuo, macrocyclic polyborazines consisting of NH-bridged borazine rings are obtained. Besides pentacyclic systems (of four borazine rings) which have been isolated, a hexacyclic compound formed by five borazines was detected in a mass spectrum
Experimentelle Prüfung von Näherungsansätzen für Chiralitätsfunktionen am Beispiel der optischen Aktivität von Methan-Derivaten im Transparenzgebiet II / Semiempirical Use of Chirality Functions for the Description of the Optical Activity of Methan Derivatives in the Transparent Region II
Authors: Richter Wolf Jürgen
Published: February 2015

Simple alcohol derivatives are used to test approximative chirality functions experimentally. The approximations of the type 1 b yield a competent description of the optical rotatory power of methan-derivatives. Provided that certain restrictions of ligand inter-actions are taken into account, a set of ligand-specific parameters is obtained; however, no common set of parameters is suitable for both the alcohol and the amino-alcohol derivatives, which have been published before
Ternäre Pnictide und Chalkogenide von Alkalimetallen und IB-bzw. IIB-Elementen / On Ternary Pnictides and Chalkogenides of Alkaline Metals and IB-resp. II B-Elements
Authors: Savelsberg Gerhard
Published: February 2015

The new compounds NaCuSe, NaCuTe, KCuSe, KCuTe and KZnP were prepared and their structures − together with those of KZnSb, NaCdSb and NaZnSb − determined. NaCuSe, NaCuTe and NaZnSb crystallize in a PbFCl type, while NaCdSb forms the anti-PbCl2-structure. KCuSe, KCuTe, KZnP and KZnSb build up the Ni2ln-structure.

The lattice constants are:

NaZnSb P4/nmm a = 444(2) pm c = 749(2) pm c/a = 1.69

NaCuSe P 4/nmm a = 410(2) pm c = 682(2) pm c/a = 1.66

NaCuTe P4/nmm a = 438(2) pm c = 711(2) pm c/a = 1.62

NaCdSb Pnma a = 795(2) pm b = 471(2) pm c = 842(2) pm

KZnP P 63/mmc a = 409(2) pm c = 1014(2) pm c/a = 2.48

KZnSb P 63/mmc a = 454(2) pm c = 1050(2) pm c/a = 2.31

KCuSe P 63/mmc a = 418(2) pm c = 954(2) pm c/a = 2.28

KCuTe P 63/mmc a = 446(2) pm c = 995(2) pm c/a = 2.23
Darstellung und thermische Zersetzung von Erdalkalimetall-Carbamoylphospliaten / Preparation and Thermal Decomposition of Carbamoylphosphates of Alkaline-earth Metals
Authors: Seel Fritz , Schinnerling Fritz
Published: February 2015

After the formation of carbamoylphosphate through the reaction of KH2PO4 with KNCO in aqueous solution, unreacted phosphate and carbamoylphosphate can be separated by fractional precipitation with barium (first step) and calcium or strontium or barium salt solutions (second step) at low temperatures. The carbamoylphosphates of the alkaline earth metals are decomposed above 100 °C to yield predominantly diphosphates and urea. In aqueous suspensions the decomposition proceeds even at room temperature. - The chemical shifts of the phosphorus atom of the carbamoylphosphate ion between pH 6.5 and 8.2 are given.
Kristall-und Molekülstruktur von N-(TricHorgermyl)-trimethylphosphinimin [Cl3Ge-N=PMe3]n, n = 1 und 2 / Crystal and Molecular Structure of N-(Trichlorogermyl)-trimethylphosphinimine [Cl3Ge-N=PMe3]n, n= 1 and 2
Authors: Sheldrick W. S. , Schomburg D. , Wolfsberger W.
Published: February 2015

N-(Trichlorogermyl)trimethylphosphinimine crystallizes in the triclinic space group P1̅ with a = 12.49(2), b = 12.54(3), c = 6.66(1) Å,a = 100.96(10),β = 91.45(14), γ = 102.77(15)°. The structure was solved by Patterson and difference syntheses and refined to R = 0.063 for 2867 independent reflections. In the unit cell there are two symmetry related monomers containing tetracoordinated Ge and one crystallographically centrosymmetric dimer with a planar four-membered [GeN]2 ring exhibiting trigonal-bipyramidal pentacoordinated Ge and trigonal N. Significant differences are observed in the bond lengths from pentacoordinated Ge to its equatorial and axial ligands: Ge-Neq 1.837(7), Ge-Nax 1.972(7), Ge-Cleq 2.176(2) and 2.170(2), Ge-Clax 2.345(3) Å. The Ge-Neq distance is similar to that observed in tetracoordinated derivatives [1.81-1.87 Å], whereas the Ge-Nax distance is 0.22 Å shorter than that observed for the axial N→Ge coordinate bond in hitherto known pentacoordinated derivatives [2.19-2.24 Å]. The very short Ge-N bond length of 1.737(8) Å in the monomer which is 0.07 Å shorter than in other tetracoordinated derivatives may be indicative of the involvement of a (p→d)π component.
Elektrochemische Synthesen, XIV [1] Radikalkation-Salze des Naphthalins / Electrochemical Syntheses, XIV [1]. Radical Cation Salts of Naphthalene
Authors: Fritz Heinz P. , Gebauer Helmut , Friedrich Peter , Ecker Peter , Artes Reinhold , Schubert Ulrich
Published: February 2015

By anodic oxidation of naphthalene in H2CCl2/O.O2m Bu4NPF6 at -45 °C dark red-violet crystals of (C10H8)2PF6 can be obtained by electrocrystallisation. They are stable at low temperatures, however, decompose on warming. In solution and in the polycrystalline state these radical cation salts show only narrow e.p.r. signals without h.f.s. The specific conductivity of a polycrystalline pellet at room temperature was determined to be 0.12 ±0.046 Ohm-1 cm-1 . The structure determination of (C10H8)2PF6 yielded the tetragonal space group P42/n, Z = 2, a = b = 1156(2), c = 640(1) pm. Patterson synthesis and difference Fourier analyses showed the compound to have a columnar stacking of C10H8 units the long molecular axes of which are twisted alternately by 90° around a screw axis in c-direction, and the molecular planes of which are 320 pm apart. The PF6
-ions have four nearest C10H8 neighbours lying in pairs in parallel planes 63 pm above and below that plane of PF6
- perpendicular to the c-axis and containing a PF4 group. This is the first established case for a columnar structure of a pure hydrocarbon radical cation. (C10H8)2AsF6 is isomorphous.
Reaktionen von Lithio-aminofluorsilanen mit Halogensilanen und Trimethylzinnchlorid / Reactions of Lithio-aminofluorosilanes with Halogensilanes and Trimethyltinchloride
Authors: Klingebiel Uwe
Published: February 2015

Fluorosilanes react with lithium amides and organolithium compounds to give aminofluorosilanes. (Lithioamino)fluorosilanes are formed by the reaction of aminofluorosilanes with butyllithium depending on the steric influence and molecular stabilization of the ligands. These lithium salts react with halogensilanes and trimethyltin chloride with substitution. By LiF elimination the lithioaminofluorosilane

C6H5-SiF-NLiC(CH3)3-N(p-C6H4CH3Si(CH3)3)

cyclisizes through a (2+2)cycloaddition and SiC-H-cleavage.
BaSb3, ein Antimonid mit einem zweidimensional unendlichen [Sb3
2-]n-Polyanion / BaSb3, an Antimonide with an Infinite Twodimensional [Sb3
2-]n - Anion
Authors: Deller Klaus , Eisenmann Brigitte
Published: February 2015

The new compound BaSb3 has been prepared and its structure determined. It crystallizes monoclinic (C 2/m, a = 1080.7(5) pm, b = 851.9(5) pm, c = 647.1(5) pm, β = 112.66(4)°). The Sb-atoms build up 14-rings of two-and threebonded Sb, which are connected to puckered nets.
Arsenhaltige Heterocyclen / Heterocycles Containing Arsenic
Authors: Roesky Herbert W. , Sidiropoulos Georg
Published: February 2015

In the reaction of N,N'-bis-trimethylsilyl-dimethylurea with As[N(CH3)2]3 a four membered ring O = C(NCH3)2AsN(CH3)2 1 could be isolated. 1 was not obtained by cleavage of the Si-N-bonds with the corresponding chloride. In contrast

CH3N[CONCH3Si(CH3)3]2

reacts with AsCb to yield the six-membered ring CH3N(CON-CH3)2ASCl 2. The four-membered ring which contains an arsenic-halogen bond seems to be unstable. In the adamantane-type compound, AS4(NCH3)6, one methylamine could be eliminated by CF3SO3H to give AS4(NCH3)5(OSO2CF3)2 3. 1H, 19F NMR as well as mass spectroscopy have been used in the characterization of the products obtained.
Über Reaktionen von 3-trifluormethylphenylsubstituierten silicium-und zinnorganischen Verbindungen / Reactions of 3-Trifluoromethylphenyl Substituted Silicon and Tin Organic Compounds
Authors: Roesky Herbert W. , Ambrosius Klaus
Published: February 2015

Several routes were investigated for the preparation of 3-CF3C6H4N[Si(CH3)3]2 2 and 3-CF3C6H4N[Sn(CH3)3]2 3. The latter compound reacts with 3-CF3C6H4NCO to yield [3-CF3C6H4(CH3)3SnN]2CO 4. A substituted urea 5 is also formed from [(CH3)3Si]2NCH3 and 3-CF3C6H4NCO. 5 is used for the preparation of cyclic compounds, with S2Cl2 the ten-membered ring (3-CF3C6H4NCONCH3S2)2 6 is formed. 5 and HN(SO2Cl)2 yield the six-membered ring 3-CF3C6H4NCONCH3(SO2)2NH 7. SeOCl2 and 5 react under formation of a spiro compound (S-CF3C6H4NCONCH3)2Se 8. The compounds were characterized on the basis of mass and 19F NMR spectra.
Neue ternäre Erdalkaliverbindungen des Arsens mit Mangan / New Ternary Alkaline Earth Compounds of Arsenic with Manganese
Authors: Brechtel Erwin , Cordier Gerhard , Schäfer Herbert
Published: February 2015

The new compounds CaMn2As2, SrMn2As2 and BaMn2As2 have been prepared and their structures determined. The crystallographic data are (pm):

CaMn2As2:

P3̄m 1, a = 423 ± 1, c = 703 ± 1, c/a = 1.66

SrMri2As2:

P3̄m 1, a = 429±1, c = 732 ± 1, c/a = 1.70

BaMn2As2:

I4/mmm, a = 415 ± 2, c = 1347 ± 2, c/a = 3.24
Das Verhalten von (Halogen)Acyldiphenylphosphinen gegenüber molekularem Sauerstoff in Abhängigkeit vom Acylrest / Behavior of (Halogeno) Acylphosphines Towards Molecular Oxygen in Dependence of the Acyl Residue
Authors: Lindner Ekkehard , Lesiecki Hans
Published: February 2015

The halogenated acylphosphines RC(O)PPh2 (1a-f) [R = ClCH2 (a), FCH2 (b), F2CH (c), C2F5 (d), C3F7 (e), C6F5 (f)], which can be oxidized by rigorously dried oxygen to the phos­phine oxides RC(O)P(O)Ph2 (2a-f), are obtained by reaction of NaPPh2 with the acyl chlorides RC(O)Cl. From 2a-f and stoichiometric amounts of water the alcohols RC[Ph2P(O)]2OH (3a-f) are formed. While 3c-f are isomerized into the phosphinates RC[Ph2P(O)][OP(O)Ph2]H (4c-f), the alcohols 3a, b are stable. The hydrolytic and thermal behavior of the phosphine oxides 2 and the alcohols 3 are discussed regarding the nature of the acyl residue.
Die Verbindungen MgFe6Ge6 und LiCo6Ge6 / The Compounds MgFe6Ge6 and LiCo6Ge6
Authors: Buchholz Werner , Schuster Hans-Uwe
Published: February 2015

The hexagonally crystallizing compounds MgFe6Ge6 and LiCo6Ge6 were prepared and structurally characterized by single crystal investigations. The lattice constants are a = 506.7 pm, c = 804.5 pm, c/a= 1.58s for MgFe6Ge6 and a = 504.8 pm, c = 772.9 pm, c/a = 1.531 for LiCo6Ge6. The structures (space group P6/mmm) are closely related to the structure of LiFe6Ge6 and the B 35-type structure of FeGe.
Starke metallorganische Lewissäuren: Tricarbonyl-π-cyclopentadienylkationen von Molybdän und Wolfram [(π-C5H5 )(OC)3M]+⊕(M = Mo, W)/Strong Organometallic Lewis Acids: Tricarbonyl-π-cyclopentadienyl Cations of Molybdenum and Tungsten [(π-C5H5)(OC)3M]+ (M = Mo, W)
Authors: Beck Wolfgang , Schloter Klaus
Published: February 2015

Hydride abstraction from the hydrides (π-C5H5)(OC)3MH (M = Mo, W) using Ph3C+X_ (X = BF4, PF6) affords the compounds (π-C5H5)(OC)3MX in high yields. IR data indicate that in these complexes tetrafluoroborate and hexafluorophosphate are coordinated to the metal. The complexes behave as strong Lewis acids; they react with σ- and π-donors L to give [(π-C5H5)(OC)3ML]+X- [L = CO, PPh3, PCl3, C2H4, CH3CN, H2O, (CH3)2CO, C4H8O(THF)]. The hexafluorophosphate compounds add methylene chloride to give [(π-C5H5)(OC)3M(CH2Cl2)]+PF6
-. Reaction with diphenylacetylene yields [(π-C5H5)(OC)M(PhC ≡CPh)2]+BF4- (M = Mo, W). The hydride-bridged complexes {[(π-C5H5)M(CO)3]2H}+X- have been obtained by reaction of (π-C5H5)(OC)3MX with (π-C5H5)(OC)3MH.
Substituenteneffekte und Störung von π-Systemen, XXXV Radikalanionen Zinn-substituierter Naphthaline/ Substituent Effects and Perturbation of n Systems, XXXV Radical Anions of Tin-Substituted Naphthalenes
Authors: Bock Hans , Kaim Wolfgang , Tesmann Holger
Published: February 2015

Novel radical anions of trimethylstannyl substituted naphthalenes and their ESR spectra are reported. Both 119 Sn and 117 Sn coupling can be assigned unequivocally. The perturbation of π systems by R3X substituents of group IV b elements X = C, Si, Ge, Sn and Pb is discussed with respect to photoelectron ionization potentials, charge transfer excitations, half-wave reduction potentials and ESR spin distribution.
Optisch aktive Übergangsmetall-Komplexe, LIX (+)436- und (—)436-C5H5Fe(CO)(COCH3)Pø2R*. Das Gleichgewicht C5H5Fe(CO)2CH3 + PR3 ⇄ C5H5Fe(CO)(COCH3)PR3
Authors: Brunner Henri , Vogt Heinz
Published: February 2015

The pair of diastereoisomers (+)436-and (-)436-C5H5Fe(CO)(COCH3)PØ2R*, with PØ2R* = (S)-(+)-(C6H5)2PN(CH3)CH(CH3)(C6H5), can be separated into its components by preparative liquid chromatography under pressure. On heating (+)436-C5H5Fe(CO)-(COCH3)PØ2R* equilibrates with C5H5Fe(CO)2CH3 and PØ2R* before epimerization at the Fe atom takes place. In the same way, the equilibrium C5H5Fe(CO)(COCH3)P(C6H5)3 ⇄ C5H5Fe(CO)2CH3 + P(C6H5)3 can be obtained starting from either side. It is shown that the decarbonylation C5H5Fe(CO)(COCH3)P(C6H5)3 → C5H5Fe(CO)(CH3)P(C6H5)3 + CO is not a thermal but a photochemical reaction.
Das Radikal Cp(CO)3Cr in Lösung/The Radical Cp(CO)3Cr in Solution
Authors: Madach Thomas , Vahrenkamp Heinrich
Published: February 2015

The monomeric complex Cp(CO)3Cr (2) is formed in benzonitrile solution by electrochemical oxidation of the anion Cp(CO)3Cr- (3) or by dissolution of the parent dimer Cp(CO)3Cr-Cr(CO)3Cp (1). Its existence is obvious from electrochemical and ESR data which together with the IR and NMR spectra indicate that in this solution the dimer 1 is in a rapid equilibrium with about 1% of the monomer 2.
Beiträge zur Chemie des Bors, XCIX Borylphosphin-Metallcarbonyle der VI. Nebengruppe /Contributions to the Chemistry of Boron, XCIX Borylphosphine Metal Carbonyls of Group VI Transition Metals
Authors: Nöth Heinrich , Sze Siu Ning
Published: February 2015

The following new types of coordination compounds were prepared by direct and indirect methods: (CO)5M · PR2-B(NR2), cis(CO)4M · (PR2)2BNR2′, cis-(CO)4M · (PR2BNR2′) and (CO)4MO · (R2P)2B(R2P)2B(PR2)2 · Mo(CO)4 (M = Cr, Mo, W). It was assumed that an increased metal-boron interaction would result in the series (CO5M · R2PBR2
′, (CO)4M(R2P)2BR′, (CO)3M(R2P)3B. However, no firm conclusion on this point is possible from the spectroscopic data obtained.
Darstellung und Eigenschaften von Dihydrogensulfido-, Dihydrogenselenido-und Dinatriumsulfido-Komplexen von Palladium(II) und Platin(II) /Synthesis and Properties of Di-hydrogensulfido, Di-hydrogenselenido and Di-sodiumsulfido Complexes of Palladium(II) and Platinum(II)
Authors: Schmidt Max , Hoffmann Gerhard G.
Published: February 2015

Dichloro-bis(triphenylphosphine)platinum(II) (2) and Dichloro-1,2-bis(diphenylphosphine)ethane-palladium(II) (3) do react with hydrogensulfide and sodiumsulfide under formation of the corresponding compounds Di-hydrogensulfido-1,2-bis(diphenylphos-phine)ethane-palladium(II) (4), Disodiumsulfido-1,2-bis(diphenylphosphine)ethane-palladium(II) (7), Di-hydrogensulfido-bis(triphenylphosphine)platinum(II) (1) and Di-sodium-sulfido-bis(triphenylphosphine)platinum(II) (8). 2 and 3 react with sodiumhydrogen-selenide under formation of Di-hydrogenselenido-1,2-bis(diphenylphosphine)ethane-palladium(II) (5) and Di-hydrogenselenido-bis(triphenylphosphine)platinum(II) (6). IR and 1H NMR spectra are reported.
N2H4-Koordination an Eisen-Schwefel-Zentren: Synthese und Struktur von [N(C4H9)4]2[μ-N2H4{Fe(S2C6H4)2}2]/N2H4Coordination on Iron Sulfur Centres: Synthesis and Structure of [N(C4H9)4]2[μ-N2H4{Fe(S2C6H4)2}2]
Authors: Sellmann  , Kreutzer Peter , Huttner Gottfried , Frank Albin
Published: February 2015

The reactions of N2H4 and N2H4 · H2O respectively, with [N(C4H9)4][Fe(S2C6H4)2] are investigated. With N2H4 · H2O the complex salt [N(C4H9)4]2[μ-N2H4{Fe(S2C6H4)2}2] is obtained, the first hydrazine complex of a dithiolato transition metal system, which can be fully characterized. The structure shows, that the compound consists of discrete cations and anions; in the centrosymmetrical anions two [FeS4] centres are bridged by a hydrazine ligand with Fe-N distances of 224 pm, N-N distances of 142 pm and Fe-N-N angles of 116.1°. The iron atoms are square pyramidally configurated and located 35 pm above the plane determined by the S atoms.
Azido- und Isocyanato-trichloro-borat und -aluminat / Azido and Isocyanato Trichloro Borate and Aluminate
Authors: Chow Lyonel , Schmock Fritjof , Müller Ulrich
Published: February 2015

N(CH3)4[BCl3N3], N(CH3)4[AlCl3N3], K[BCl3NCO] and K[AlCl3NCO] were prepared from N(CH3)4N3 and KNCO with BCl3 and AlCl3 using liquid SO2 as solvent. It is essential to avoid any excess of the halide in order to supress secondary reactions. The IR spectra show the NCO group to be bonded via its nitrogen atom.
Automatische Erzeugung pericyclischer Reaktionen/Automatic Generation of Pericyclic Reactions
Authors: Gasteiger Johann
Published: February 2015

A formal concept for the treatment of the bond and electron shifts in pericyclic reactions is developed. A new data structure for the representation of molecules allows the design of efficient algorithms. This resulted in a computer program for the exhaustive generation of pericyclic reactions.
Enhydrazine, XXV Einige Derivate des 1-Dimethylamino-2(1H)-chinolinons/Enehydrazines, XXV Some Derivatives of 1-Dimethylamino-2(1 H)-quinolinone
Authors: Wolf Ulrich , Sucrow Wolfgang , Vetter Hans-Jürgen
Published: February 2015

Reaction of the N,N-dimethyl enehydrazines 1 a-c with acetylene carboxylates gives the 1-dimethylamino-7,8-dihydro-2,5(1H,6H)-quinolinediones 5a and 6a-c together with some by-products of the enehydrazine (2a, 3a, 4a) and 4,5,6,7-tetrahydro-1H-indol-4-one type (7a-c). Compounds 6b and 6c have been degraded to the fully aromatic 1-dimethylamino- 2(1H)-quinolinones 12 b and 12 c.
Bakterieninhaltsstoffe, III 3-Alkyl-tetrahydrochinolinderivate aus Pseudomonas / Bacterial Constituents, III 3-Alkyl-tetrahydroquinoline Derivatives from Pseudomonas
Authors: Neuenhaus W. , Budzikiewicz H. , Korth H. , Pulverer G.
Published: February 2015

3-n-Heptyl- and 3-n-nonyl-3-hydroxy-1, 2, 3, 4-tetrahydroquinoline-2,4-dione have been isolated from the culture medium of Pseudomonas aeruginosa. Their structures have been elucidated.
The 185 nm Photolysis of 1,4-Dioxane in the Liquid Phase
Authors: Schuchmann Heinz-Peter , Bandmann Heinz , Sonntag Clemens von
Published: February 2015

The main products in the 185 nm photolysis of neat 1,4-dioxane are formaldehyde (Φ = 0.25), glycol monovinyl ether (0.17), and ethylene (0.15). Some hydrogen (0.04), carbon monoxide (0.01), acetaldehyde (0.03), oxetane (0.04), and bidioxanyl (0.01) are also formed. On N2O-saturation, the quantum yields of these products are diminished by about 30%, and N2 (0.59) and hydroxydioxane (0.4) become the main products. They are thought to be formed in the reaction sequence

In aqueous dioxane, photoionisation is possible due to a greater lowering of the ionisation threshold. In dioxane/water 20:80 the main products are H2 (0.50) and bidioxanyl (0.45), most likely formed in consequence of
Chemistry of Alkoxo Complexes, Part III *Synthesis and Characterization of Some Mono(carboxylato)mono (alkoxo)nickel(II) Complexes
Authors: Baranwal B. P. , Parashar G. K. , Mehrotra R. C.
Published: February 2015

A number of mono(carboxylato)mono(alkoxo)nickel(II) complexes of the general formula, Ni(OR)(OOCR′), (with R′ = C13H27, C15H35 and C17H35) have been synthesized (where R = Me and Pri) by the reactions of nickel methoxide and isopropoxide with the respective carboxylic acids in equimolar ratio and (where R = Et and But) by alcohol interchange reactions. A study of the molecular weight, infra-red and electronic reflectance spectra and magnetic susceptibility in addition to elemental analyses has been carried out to throw some light on the probable structure of these derivatives.
Derivatives of cis-NPCl2(NSOCl)2 and (NPCl2)2NSOCl, Part XII [1] Triphenylphosphazenyl Derivatives of NPCl2(NSOX)2 and (NPCl2)2NSOX with X = F, Cl or Ph
Authors: Jekel A. P. , Grampel J. C. van de
Published: February 2015

Reaction of the ring systems NPCl2(NSOX)2 and (NPCl2)2NSOX (X = F, Cl, Ph) with HNPPh3 in molar ratio 1:2 gives their mono(tripbenylphosphazenyl) derivatives. The compound NPCl(NPPh3)(NSOPh)2 forms a stable 1:1 adduct with acetonitrile. All compounds are characterized by NMR (31P, 19F), IR and mass spectra.
Eine unerwartet einfache Synthese von Dimethylphosphin / An Unexpectedly Simple Synthesis of Dimethyl Phosphine
Authors: Trenkle Armin , Vahrenkamp Heinrich
Published: February 2015

The desulfuration of Me2P(S)P(S)Me2 by tri-n-butyl phosphine in the presence of protic substances (water, alcohols, carbonic acids and others) is accompanied by hydrolytic cleavage of the P-P bond with formation of dimethyl phosphine.
Chinolizine und Indolizine, XII [1]. Zur Reaktion von Pyrophthalon mit reaktiven Malonsäurederivaten / Quinolizines and Indolizines, XII [1]. Reaction of Pyrophthalone with Reactive Malonyl Derivatives
Authors: Kappe Thomas , Hariri Mehdi , Stadlbauer Wolfgang
Published: February 2015

The reaction of 2-(2′-pyridyl)-indan-1,3-dione (pyrophthalone, 1) with reactive malonic acid derivatives (2) yields the indanoquinolizinone derivative (5) by rearrangement of the instable zwitter-ionic compound 3 and decarboxylation of the seven-membered intermediate 4. In order to support this mechanism the lactone 15 was thermolyzed to give fluorenone (16) by decarboxylation.
Synthese und Additionsreaktionen von 1.3.2λ2.4-Diazaphosphoniaahiminatacyclobutanen [1] / Synthesis and Addition Reactions of 1,3,2λ2,4-Diazaphosphoniaaluminatacyclobutanes [1]
Authors: Niecke Edgar , Kröher Rainer
Published: February 2015

N-silylated aminoiminophosphines react with aluminium trihalides to give acyclic zwitterions having two-coordinated phosphorus. At about room temperature these adducts decompose by elimination of silylhalide and formation of 1,3,2λ2,4-diazaphosphonia-aluminatacyclobutanes. Reaction of halogens and alkyl halides with the cyclic zwitterions results in formation of the corresponding 1,1-addition products. With alkyl-azides one obtains bicyclic phosphorus nitrogen heterocycles whilst in the reaction with trimethyl-silylazide the isomeric monocyclic azide derivative is formed. The IR and NMR spectra of the cyclic zwitterions are briefly discussed.
Semiempirische SCF-Rechnungen zur Hydroxypyrimidin-Pyrimidon-Tautomerie / Semiempirical SCF-Calculations on the Hydroxypyrimidine-pyrimidone Tautomerism
Authors: Fabian Walter
Published: February 2015

The electronic spectra of a series of substituted 4-hydroxypyrimidines are calculated by the INDO/CI method. Best agreement with the experimental values is obtained when the geometry of the 4(3H)-pyrimidone form is used. Calculated total energies seem to be less suitable for determining tautomeric equilibria than a comparision between experimental and theoretical transition energies.
Zur Polymorphie des Na2S2O3 / On Polymorphism of Na2S2O3
Authors: Benda Heike von
Published: February 2015

Na2S2CO3 crystallizes in 4 modifications. The familiar monoclinic a-form stable at ambient temperature transforms into the trigonal β-form at 330 °C which at 388 °C converts to b ccy-Na2S2O3. These transformations are reversible. Unstable orthorhombic α'-Na2S2CO3(Pna21) is obtained by dehydration of the pentahydrate or by cooling the β-phase. The γ-phase decomposes in sealed ampoule to Na2SCO4 and NaS5; decomposition is slow below and rapid above 440 °C. Equilibrium displacement by distillation of sulphur accelerates decomposition even for β-Na2S2O3, and maintaining low sulphur pressure by pumping gives Na2SO3. β- and γ-Na2S2CO3 are superionic conductors; a dynamic model is presented for the β-structure with Na+ conduction pathways originating from oscillation of the S2O3
2- tetrahedra. Structural relationships can be derived with respect to the arrangement of the thiosulphate groups.
Solvent Extraction Study of Mercury(II) with Zolon Red (HZR)
Authors: Patel A. N. , Qureshi A. M.
Published: February 2015

Zolon Red, Mercury(II) The extraction of mercury(II) from the aqueous solutions of mercury(II) nitrate and mercury(II) chloride with zolon red (HZR) dissolved in w-butanol has been studied. The extraction of mercury (II) from the aqueous nitrate system has been found to be much better compared to that from the aqueous chloride system in the pH range of 1 to 6. The extraction of mercury with zolon red is simple, fast and selective. The composition of the extracted mercury zolon red compound has also been studied. Regeneration of the extracting solution of zolon red is readily achieved by stripping the mercury(II) with an aqueous cyanide solution.
Neue mixed-valence-Verbindungen mit Sb(III) und Sb(V) vom Typ (RH+)8(C1-)4SbCl6
3- SbCl6
- / New Mixed-valence Compounds with Sb(III) and Sb(V) of the Structure (RH+)8(Cl-)4SbCl6
3-SbCl6
-
Authors: Eisinger H. K. , Latscha H. P.
Published: February 2015

New mixed-valence-compounds with Sb(III) and Sb(V) of the structure (RH+)8(Cl-)4SbCl6
3-SbCl6
- with R equal CH3CH(NH2)CH3, CH3CH(NH2)CH2CH3, CH3CH2CH2NH2,

and CH3CH(CH2NH2)CH3 are reported. Different methods of preparation for these compounds are described. Compounds with the structure (RH+)8(Br-)4SbCl6
3-SbCl6
- are obtained with R = CH3CH(NH2)CH2CH3 and CH3CH(NH2)CH3. All compounds are characterised, their formation is discussed
Compounds of Complex Halo and Pseudohalo Acids of the Group II B Metals, Part I Etherate, Pyridine and Aniline Compounds of Zn(II)
Authors: Galinos A. G. , Kouinis J. K . , Ioannou P. V. , Zafiropoulos Th. F . , Perlepes S. P.
Published: February 2015

The preparation of sixteen new etherate, pyridine and aniline compounds of complex halo and pseudohalo acids of Zn(II) is reported.

The study of some physical and chemical properties as well as the UV and IR spectra of these compounds are discussed. Tetrahedral structures are proposed for all compounds in the solid state
Redox-Chemie einfach arsenverbriickter Zweikernkomplexe ohne Metall-Metall-Bindung /Redox Chemistry of Singly Arsenic Bridged Dinuclear Complexes without Metal-Metal Bonds
Authors: Madach Thomas , Vahrenkamp Heinrich
Published: February 2015

The oxidations and reductions of 27 singly arsenic bridged dinuclear metal carbonyl complexes were investigated. There are indications that the complexes as a whole are involved in the redox process. However, the expected one and two electron oxidations with concomitant formation of metal-metal bonds were not observed. Electrochemical electron transfers were irreversible. Chemical oxidation and reduction of a selected example resulted in a series of products originating from the primary fission of one metal-arsenic bond.
Cyclopentyl-und Cyclohexyl-dimethyl-methylen-phosphoran aus w-Haloalkyl-trimethylphosphonium-salzen. Goldkomplexe mono-und difunktioneller Ylide / Cyclopentyl-and Cyclohexyl-dimethyl-methylene-phosphoranes from w-Haloalkyl-trimethylphosphonium Salts. Gold Complexes of Mono-and Difunctional Ylides
Authors: Schmidbaur H. , Scherm H. P.
Published: February 2015

(CH3)3 Pconvertsa,a,w-dibromopentaneand-hexane into w-bromoalkyltrimethylphos-phonium bromides,which undergo a cyclizationon treatment with NaNH2 in tetrahydro-furane to form the cyclopentyl-and cyclohexyl-dimethyl-methylenephosphoranes 4 and 5. From the bis-phosphonium salt(CH3)3P(CH2)6P(CH3)3
2⊕ 2Br⊖ the difunctional bis-ylide CH2=(CH3)2P(CH2)6P(CH3)2=CH2(7)is obtained. The ylide 4 was characterized by the crystalline metallocyclic Au(I)derivative 8.7 forms a polymeric gold complex.
Beiträge zur Chemie des Bors, CVII [1] Über Darstellung und Struktur eines tetraborylierten Hydrazins / Contributions to the Chemistry of Boron, CVII [1] On the Preparation and Structure of a Tetraborylated Hydrazine
Authors: Bharara P. C. , Nöth H.
Published: February 2015

N,N,N′-Tris- and N,N,N′,N′-tetrakis(1,3-dimethyl-1,3,2-diazaborolidinyl)hydrazine (4)were prepared via N,N′-lithiated N,N′-bis(1,3-dimethyl-1,3,2-diazaborolidinyl)hydrazine. 4 crystallizes monoclinic.The N-N axes of the 4 molecules coincide with the crystallo-graphic twofold axes. Its N-N bond is rather long(146.4qm and the ring BN bonds are shorter than the BN bond to the hydrazine nitrogen atoms. This indicates preferential electronic saturation of the boron atoms via ring BN II bonding.
121Sb - Mößbauer- Spektren von mixed-valence-Verbindungen des Typs (RH+)8(Cl)4SbCl6
3-SbCl6
- / 121Sb Mössbauer Spectra of Mixed Valence Compounds of the Structure (RH+)8(Cl-)4SbCl6
3-SbCl6
-
Authors: Dietrich W. , Eisinger H. K. , Latscha H. P. , Pebler J. , Schmidt K.
Published: February 2015

The 121Sb Mössbauer spectra of the mixed valence compounds (RH+)8(Cl-)4SbCl6
3-SbCl6
-with R equal CH3CH(NH2)CH3 (1), CH3CH(NH2)CH2CH3 (2) are reported and the results are discussed.
μ-Oxo-bis[trichloro-2.4-pentandionatoantimon(V)] Darstellung, Struktur und Spektren / μ-Oxo-bis[trichloro-2,4-pentanedionatoantimony(V)] Preparation, Molecular Structure and Spectra
Authors: Blösl Sigfried , Schwarz Wolfgang , Schmidt Armin
Published: February 2015

μ-Oxo-bis[trichloro-2,4-pentanedionatoantimony(V)] (2) is prepared by reacting d,h-μ- propionato-e-μ-hydroxo-f-μ-oxo-bis[trichloroantimony(V)] (7) with 2,4-pentandione. The crystal and molecular structure of 2 is determined and the vibrational spectrum assigned.
Zur Darstellung und Struktur von CaMnBi2 / On the Preparation and Crystal Structure of CaMnBi2
Authors: Brechtel Erwin , Cordier Gerhard , Schäfer Herbert
Published: February 2015

The new compound CaMnBi2 has been analytically and structurally characterized. CaMnBi2 crystallizes in the tetragonal system (a = 450 ± 1 pm, c = 1108 ± 2 pm, space group P4/nmm). Mn and Bi atoms form fourfold pyramids, connected by common edges in the basis to two-dimensional sheets. These sheets are separated by double layers of Ca atoms between which further Bi atoms are located forming squarenets. The structure is strongly related to that of SrZnSb2 which can be interpreted as a distorted variant of the new CaMnBi2 type.
Siliciumverbindungen mit starken intramolekularen sterischen Wechselwirkungen, IX [1]. tert-Butylsubstituierte Di- und Trisiloxane / Silicon Compounds with Strong Intramolecular Steric Interactions, IX [1]. tert-Butyl Substituted Di- and Trisiloxane s
Authors: Weidenbruch Manfred , Pesel Helge , Van Hieu Dang
Published: February 2015

The overcrowded molecules 1,1,3,3-tetra-tert-butyldisiloxane-1,3-diol (2) and penta-tertbutyldisiloxanol (4) have been obtained during the attempted synthesis of tri-tert-butylsilanol and di-tert-butylsilanediol by reaction of tri-tert-butylsilane and di-tert-butylchlorosilane, resp., with silver nitrate. Compounds 2 and 4 were also formed either by condensation of two molecules of di-tert-butylsilanediol or by co-condensation of the silanediol with tri-tert-butylsilanol in the presence of jo-toluenesulfonic acid. Reactions of tri-tert-butylsilanol with silicon tetrachloride yielded 1,1,1,5,5,5-hexa-tert-butyl-3,3-dichlorotrisiloxane.
Die Isopolymolybdationen in wäßrigen Medien im Bereich Z ≦ 1,14 / Concerning Isopolymolybdate Ions in Aqueous Media in the Range Z ≦ 1.14
Authors: Tytko Karl-Heinz , Petridis Georgios , Schönfeld Bernd
Published: February 2015

The system H+/MoO4
2- was investigated by Raman spectroscopy in the range Z = 0 to 1.14 at initial concentrations CMoO₄ 2- = 0.02 to 2M and concentrations of the ionic medium CMe+ = 2CMoO₄ 2- to 3M Me(Cl,NO3) (Me=Li, Na, K,NH4 , Mg/2). The mole-ratio method and intensity difference diagrams do not indicate any species between MoO4
2- and Mo7O24
6- contrary to propositions in recent papers. A detailed evaluation of the extensive data shows the possible portion of such species to be < 3 % , this value having a statistical certainty of 95%. Comparing the solutions having Z = 1.1 by fingerprint procedures, in all cases Mo7O24
6- is the first main product (detectable by static methods) irrespective of the nature and concentration of the ionic medium. Thus, Mg2+ ions do not influence the course of aggregation of molybdate ions as has been proposed in the literature. This is in accordance with theoretical investigations since the Mo7O24
6- ion has the distinction of a number of favourable structural parameters in the system that become operative in case of scarcity of H+ ions.
Charge Distribution and Structures of Halogenogallates and Halogenoaluminates of the Type MeIMeIIIX4, MeIMe2
IIIX7, and C6H6 CUAlCl4. An NQR Investigation ( 35Cl, 79Br, 127I, 63Cu, 69Ga)
Authors: Fichtner Winfried , Weiss Alarich
Published: February 2015

In polycrystalline samples of the halogenoaluminates MeIAlCl4 (MeI - Cu, Ag), CuAlBr4, C6H6 · CUAlCl4 and halogenogallates CuGaCl4, MeIGaBr4 (MeI = Cu, Na, K, NH4, Rb, Cs, Ga), MeIGaI4 (MeI = Cu, Cs), MeIGa2Br7 (MeI = K, NH4, Rb, Cs), CsGa2I7, the halogen, MeIII , and Cu-NQR spectra were studied, partly as a function of temperature. Phase transformations are found in NH4GaBr4, CsGaBr4, and RbGa2Br7. The spectroscopic results are discussed and a charge distribution analysis is given, based on the Townes-Dailey theory. Symmetry properties of the solids are pointed out in connection with multiplicity and intensity ratios of the NQR spectra.
NMR-Spektroskopie an paramagnetischen Komplexen, XX [1]. Störung der 13C-und 1H-Spektren dia-und paramagnetischer Moleküle durch radikalische Metallocene / NMR Spectroscopy on Paramagnetic Complexes, XX [1]. Errors in the 13C and 1H Spectra of Dia-and Paramagnetic Molecules Introduced by Metallocene Radicals
Authors: Köhler Frank H.
Published: February 2015

13C and 1H NMR spectra of ethyl and t-butyl substituted cobaltocenes dissolved in toluene, benzene and acetone are strongly dependent on concentration and temperature. With increasing metallocene concentration and decreasing temperature almost all 13C and 1H signals of the metallocenes as well as those of the solvents are shifted high field to a different degree. The additional shift is most pronounced for substituted aromatic ring carbons giving rise to a seriously disturbed signal ordering. Similar behavior is found for substituted vanadocenes and nickelocenes dissolved in toluene or THF. The effect is attributed to preferred mutual orientation of metallocene and solvent molecules thus inducing additional shifts in the metallocene themselves and in the solvent. From the results it is concluded that neither dipolar nor Fermi contact interaction can satisfactorily account for the effect. Instead it originates from susceptibility shifts which may not be ruled out by internal referencing and which are due to anisotropy and orientation of the molecules. For consequence quantitative comparison of paramagnetic NMR shifts from highly anisotropic molecules is only meaningful if concentrations are known. Measurement of magnetic moments may lead to errors.
Photoisomerisierung von trans-1-(3.5-Di-tert-butyl-4-hydroxyplienyl)-2-phenyldiazen / Photoisomerization of trans-1-(3,5-Di-tert-butyl-4-hydroxyphenyl)-2-phenyldiazene
Authors: Hofer Edgar
Published: February 2015

Light induced isomerizations of the title compound have been studied. The thermal cis-trans isomerization 3→1 occurs via the tautomeric quinonephenylhydrazone (2) as shown by 1H NMR, spectroscopy. The influence of solvent on the thermal cis-trans isomerization is discussed. 1H NMR data of 1, 2 and 3 are given. Values of the tautomeric equilibrium 1⇋2 are determined for various solvents and different temperatures.
Die Struktur der Phase BaNi2Si2 und ihre Verwandtschaft zum ThCr2Si2 -Strukturtyp / The Structure of BaNi2Si2 and its Relationshiptothe ThCr2Si2 Structure
Authors: Dörrscheidt Wolfgang , Schäfer Herbert
Published: February 2015

The new compound BaNi2Si2 crystallizes in the orthorhombic system, space group Cmcm-D2h
17 with a = 650 ± 1 pm, b = 535 ± 1 pm, c = 1133 ± 2 pm. The structure can be interpreted as a distorted variant of the ThCr2Si2-type.
Synthese und katalytische Aktivität einiger neutraler (η-Cycloenyl)(η-1.5-cyclooctadien)rhodium(I)-Komplexe / Synthesis and Catalytic Activity of Some Neutral(η-Cyck)enyl)(η-1,5-cyclooctadiene)rhodium(I) Complexes
Authors: Stühler Hans-Otto
Published: February 2015

[(COD)RhCl]2 (COD = 1,5-cyclooctadiene) reacts with i-C3H7MgBr in the presence of 4-vinylcyclohexene and 1-methyl-1,4-cyclohexadiene to give the neutral, diamagnetic π-complexes [(COD)Rh(subst.-cyclohexenyl)] in which the central metal achieves a 16-electron valence shell. The catalytic activity of these complexes is described.
Die Reaktion von Antimon(V)-chlorid mit p-Benzoehinon / The Reaction of Antimony(V) Chloride with p-Benzoquinone
Authors: Rettig G. , Latscha H. P.
Published: February 2015

The reaction of p-benzoquinone with an excess of SbCl5 gives 2,3,5,6 - tetrachloro-p-benzoquinone (“Chloranil”) in high purity and almost quantitative yield. 2,6- and 2,5-dichlorop- benzoquinone could be identified as intermediate products.
N-H-Aktivierung an Os3 -Clustern. Darstellung und Charakterisierung von Os3(CO)11(NH3), Os3(CO)11(NHC6H10) und OS3(CO)10(μ - H)(μ - NC6H10) / N-H Activation on 0s3 Clusters. Preparation and Characterization of Os3(CO)11(NH3), Os3(CO)11(NHC6H10) and Os3(CO)10(μ-H)(μ-NC6H10)
Authors: Süß-Fink Georg
Published: February 2015

The ammonia complex Os3(CO)11(NH3) was prepared by aminoxide induced carbonyl substitution of Os3(CO)12. Upon heating one hydrogen atom in Os3(CO)11(NH3) is transferred onto the metal frame to yield the complex Os3(CO)10(μ-H)(μ-NH2). Reaction of Os3(CO)11(NH3) with cyclohexanone affords the ketimine complex Os3(CO)11(NHC6H1O), which can be transformed thermally into Os3(CO)10(μ-H)(μ-NC6H10). The N-H bond of the ketimine ligand is activated under milder conditions than that of the ammonia ligand.
Biosynthesis of Riboflavin. Enzymatic Deamination of 2,5-Diamino-6-hydroxy-4-ribitylaminopyrimidine-5′-phosphate
Authors: Klein Gerhard , Bacher Adelbert
Published: February 2015

Cell extracts of Saccharomyces cerevisiae and Candida guilliermondii catalyze the hydrolytic deamination in position 2 of 2,5-diamino-6-hydroxy-4-ribitylaminopvrimidine 5′-phosphate. The deaminase activity is absent in rib 2 mutants of S. cerevisiae. These findings confirm the biosynthetic pathway proposed earlier on the basis of metabolic and genetic studies [2].
Darstellung und spektroskopische Charakterisierung von Tetrahalogenooxalato-Osmaten(IY) / Preparation and Spectroseopical Characterisation of Tetrahalooxalato-osmates(IV)
Authors: Homborg Heinrich , Preetz Wilhelm , Barka Günes , Schätzel Gernot
Published: February 2015

Reaction of [OsX6]2- (X = CI, Br, I) with oxalic acid in water gives the very stable and deeply coloured new complexes [OsX40x]2- which can be precipitated as alkali or tetraalkylammonium salts. The salts with long-chain alkylammonium ions are soluble in all common no polar solvents. The IR and Ra spectra and the depolarization ratios are consistent with the local C2v-symmetry. The coupling between the vibrations of coordinated oxalate and with the skeletal [OsX4O2]-modes is apparently small. The optical spectra have been studied at low temperature (10 K). Analogous to [OsXe]2- the very intense absorptions in the UV and VIS are assigned to the electric dipole allowed electron transfer from "(π+σ)t1u, πt2U(γ7), πt2u(γ8) and (σ+π)t1u" to "dt2g". By the descent in symmetry each of these transitions is further split in three components (A1, B1, B2) corresponding to the three different groups of ligands, X2
tr-, X2
c. and ox. The distinction between the X2
tr. →Os and X2
c- → Os is caused by a static trans-effect and depends on the difference of the optical electronegativities induced by ox. This splitting is not observed for [OsCl4ox]2- but is about 900 cm-1 for [OsBr4ox]2- and 1200 cm-1 for [OsI4ox]2-. The well defined bands in the NIR and VIS are assigned to the intraconfigurational d-dtransitions between the spin-orbit components in the octahedral doublegroup Oh* splitted by the lower C2v-symmetry. Some of the zero-phonon transitions within the split of the 3Tlg, Oh-groundstate exhibit extremely high intensities (e~2500 cm2/mmol). The assignment of these transitions is improved by the electronic Ra spectra. The finestructure of some of the d-d-transitions originates from coupling with A1 vibrational modes especially with νs(C-O).
Röntgenstrukturanalyse und Schwingungsspektren von Trischwefeldistickstoffdioxid, S3N2O2 [1] / X-ray Structural Analysis and Vibrational Spectra of Trisulfurdinitrogendioxide, S3N2O2 [1]
Authors: Steudel Ralf , Steidel Jürgen , Rautenberg Norbert
Published: February 2015

A redetermination of the crystal and molecular structure of the chain-like molecule S(NSO)2 resulted in the following molecular parameters: d(SO) = 146.5(2), d(S = N) = 153.4(2), d(S-N) = 165.7(2) pm, bond angles OSN = 117.5(1)°, SNS = 123.6(2)°, and NSN = 97.2(1)°, torsion angles OSNS = -0.3(2)°, and SNSN = -177.7(2)° (molecular symmetry C2). Infrared and Raman spectra of S(NSO)2 are reported and assigned; there is no evidence for conformational changes on dissolution of crystalline S(NSO)2
Darstellung von Eisentetracarbonylkomplexen mit Thioacetamiden als Liganden / Preparation of Iron Tetracarbonyl Complexes with Thioacetamides as Ligands
Authors: Petz W.
Published: February 2015

The thioacetamids S = C(CH3)(NHR) (R = H, 1a; R = Ph, 1b) react with Fe2(CO)9 to form the iron tetracarbonyl complexes 2 and 3 with S-bonded ligands. IR, 1H, 13C and mass spectra of these new compounds are reported
Organometallphosphin-substituierte Übergangsmetallkomplexe, XXVII [1]. Trinitrosyl-organometallphosphin-mangan-Komplexe / Organometalphosphine-Substituted Transition Metal Complexes, XXVII [1]. Trinitrosyl(organometalphosphine)manganese Complexes
Authors: Schumann Herbert , Meissner Manfred
Published: February 2015

The reactions of carbonyl trinitrosyl manganese with tri-tert-butylphosphine, di-(tert-butyl)-trimethylsilyl-, -germyl-, -stannyl-phosphine, tert-butyl-bis(trimethylsilyl)-, -(germyl)-, -(stannyl)-phosphine, as well as with tris(trimethylsilyl)-, -(germyl)-, and -(stannyl)phosphine result in the elimination of the CO ligand and the formation of corresponding trinitrosyl(organometalphosphine)manganese complexes. The IR, UV, 1H, 31P, and 55Mn NMR spectra are reported and discussed
Alkinylverbindungen von Übergangsmetallen, XXXXI [1]. Planare Komplexe des Typs trans-[Pd(C≡CC6H4C≡CH)2(Pet3)2] / Alkynyl Compounds of Transition Metals, XXXXI [1]. Planar Complexes of the Type trans-[PdPd(C≡CC6H4C≡CH)2(Pet3)2]
Authors: Nast Reinhard , Beyer Axel
Published: February 2015

The diamagnetic trans-planar complexes [Pd(C≡CR)2(Pet3)2] (R = 1,2-C6H4C≡CH, 1,4-C6H4C≡CH; et = C2H5) are prepared according to the equation (1). The constitution and the structure of these compounds are demonstrated by their IR, 1H and 31P NMR spectra
(Hydroxyalkyl)- und (4-Hydroxyphenyl)- organoplumbylsulfide / (Hydroxyalkyl)- and (4-Hydroxyphenyl)-organoplumbyl Sulfides
Authors: Hager Claus-Dierk , Huber Friedo
Published: February 2015

Ph3PbOH (Ph = C6H5), (Ph2Pb)2O or Me2Pb(OH)2 (Me = CH3) and 2-mercaptoethanol (1), 3-mercaptopropandiol-1,2 (2) or 4-mercaptophenol (3) react in CHCl3 or ether to give Ph3PbSR′OH [R′ = CH2CH2 (4), CH2CHOHCH2 (5), C6H4], Ph2Pb(SR′OH)2 [R′ = CH2CH2 (7), CH2CHOHCH2(8),C6H4]and Me2Pb(SC6H4OH)2. According to spectroscopic data the ligands are bonded to tetracoordinated Pb through S, the molecules being H-bonded in the solid state. 7 redistributes above - 20 °C to give 4, (SR′OH)2 and Pb(SCH2CH2OH)2, 8 redistributes to give 5, 2, (SR′OH)2, and Pb(SCH2CHOHCH2O)
Die Weiterleitung von substituenten- induzierten 13C-NMR-chemischen. Verschiebungen in para-substituierten 3-Phenylpropansäure-methylestern / The Transmission of Substituent-Induced 13C NMR Chemical Shifts in para-Substituted 3-Phenyl Propanoic Acid Methyl Esters
Authors: Radeglia R. , Spassov S. L. , Stefanova R. , Sofia S. D.
Published: February 2015

Carbon-13 chemical shifts have been measured of para-substituted 3-phenyl propanoic acid methyl esters. The substituent-induced 13C shifts of the side chain were related to Hammett substituent effects by the dual substituent parameter method. The transmission of substituent effects and the factors that influence 13C shifts are discussed
Structure Determination of 3,5-Biscyclohexylidene-1,2,4-trithiolane / Structure Determination of 3,5-Biscyclohexylidene-1,2,4-trithiolane
Authors: Winter Werner , Bühl Hanspeter , Meier Herbert
Published: February 2015

Fragmentation of 1,2,3-thiadiazoles (1) leads to the compounds 5 - 8 with an increasing proportion of sulphur. Numerous structural possibilities exist for the products 7 with the general formula (R2C2)2S3. The number of proposals can be reduced by spectroscopic techniques, but the final structure determination is accomplished by an X-ray analysis of the title compound 7a. 7a crystallizes in the space group P21/c (Z = 4) with cell parameters of a = 9.714(1), b = 16.188(8), c = 9.149(2) Å and β = 98.93(1)°. The structure is solved by direct methods and refined to R = 0.053 with 1955 diffractometer data (I ≥ 2σ(I)). The trithiolane ring has a puckered conformation and the whole molecule shows nearly perfect C2-symmetry, which is not required crystallographically.
The Electronic Structure and the He(I) Photoelectron Spectrum of Tricarbonylcyclooctatetraene-iron [1]
Authors: Böhm Michael C. , Gleiter Rolf
Published: February 2015

The highest occupied molecular orbitals of tricarbonylcyclooctatetraene-iron (1) have been derived from those of tricarbonyl-butadiene-iron and butadiene. Based on this MO diagram and an INDO-type calculation the He(I) photoelectron (PE) spectrum of 1 could be interpreted. Using the ⊿ SCF and the transition operator method (TOM) the first five bands of the PE spectrum of 1 could be assigned.