bluuebunny/crossref_metadata_2025_split huggingface dataset:
Beiträge zur Strukturchemie phosphorhaltiger Ketten und Ringe, IX [1]. Die Molekül- und Kristallstruktur von Tri-tert-butylcyclotriphosphanpentacarbonyl- chrom(O), [(t-BuP)3Cr(CO)5] / Structural Chemistry of Phosphorus-Containing Chains and Rings, IX [1]. The Molecular and Crystal Structure of Tri-tert-butylcydotriphosphane-pentacarbonyl-chromium (0), [(t-BuP)3Cr(CO)5]
Authors: Tebbe Karl-Friedrich , Fehér Magda 
Published: February 2015

The structure of [(t-BuP)3Cr(CO)5], C17CrH27O5P3, has been determined by single crystal X-ray techniques, solved by ‘direct methods', and refined to R = 0.048, wR = 0.050 for 3657 reflections by blocked least squares. The compound crystallizes in the space group P 21/c with a = 1664.9 pm, b = 916.5 pm , c = 3089.8 pm, β= 91.45° and Z = 8 formula units.
The structure consists of two crystallographically independent but structurally nearly identical mononuclear [(t-BuP)3Cr(CO)5] complexes with the three-membered ring (t-BuP)3 as an unidentate σ-donor ligand. Compared to the free molecule (t-BuP)3 the cyclophosphane ligand is slightly distorted on account of its coordination to the Cr(CO)5-group.
Die Kristallstruktur von PPh3Me[NbOCl4(CH3CN)] / The Crystal Structure of PPh3Me[NbOCl4(CH3CN)]
Authors: Hiller W. , Strähle J. , Prinz H. , Dehnicke K. 
Published: February 2015

The X-ray structure of PPh3Me[NbOCl4(CH3CN)] at 210 K was solved (space group P1̄, two formula units per unit cell, a = 1173.5(5), b = 1130.1(4), c = 946.8(3) pm, α = 97.70(4), β = 93.57(3), γ = 78.62(3)°, 3688 inde­pendent reflexions, R = 0.025).
The material consists of cations [P(C6H5)3CH3]⊕ and anions [NbOCl4(CH3CN)]⊖. The nitrogen atom of the acetonitrile solvate molecule is coordinated to the niobium centre in the trans-position to the oxo ligand; the NbO bond length of 169 pm corresponds to a double bond.
Impedance of an Oxygen Reducing Gas-Diffusion Electrode
Authors: Wabner Dietrich , Holze Rudolf , Schmittinger Peter 
Published: February 2015

The impedance of teflon bonded electrodes was measured in the frequency domain. These electrodes based on activated carbon as electrocatalyst were developed for fuel cell applications. When feeding the electrode with air or oxygen the impedance spectra could be explained by two Nernst diffusion processes and a small charge transfer process.
Two methods for separating the measured impedance into partial impedances related to different steps of the electrode reaction are presented. A least square fit procedure is described which has been applied successfully to the impedance analysis of porous electrodes
Fluorescence Properties of Hydroxy- and Methoxyflavones and the Effect of Shift Reagents
Authors: Wolfbeis Otto S. , Begum Monowara , Geiger Hans 
Published: February 2015

The fluorescence spectra of 42 hydroxy- and methoxyflavones in methanol solution have been investigated. The following findings are considered to be useful in structure elucidation and identification of flavonoids: (a) The maxima of the absorption and fluorescence bands give, in most cases, a unique combination; (b) flavones exhibit exceptionally large Stokes’ shifts (6,800 to 10,000 cm-1); (c) most flavones fluoresce blue, but flavonols fluoresce yellow or green; the fluorescence of flavonols consists frequently of two bands; (d) fluorescence is zero or very weak for 5-hydroxyflavones; (e) 5-hydroxyflavones become increasingly fluorescent with in increasing number of oxygen functions being present in the molecule; a 3-hydroxy group has a particular beneficial effect; (f) hydroxyflavones fluoresce less intense than the corresponding m ethoxyflavones; (g) fluorescence intensity is distinctly higher in polar protic than in apolar solvents.
The effects of three groups of shift reagents on the spectra has also been investigated. The first group involves water, 10% and 50% sulphuric acid. The second group consists of basic reagents (sodium acetate, sodium hydrogen carbonate and sodium carbonate), and the third group of com plexing reagents such as aluminum trichloride, borax and magnesium sulphate. The following generalisations may be made: (a) Water causes a bathochromic shift in emission with 7-hydroxyflavones, but a hypsochromic shift with flavonols; (b) 50% sulphuric acid is able to protonate (and thus to longware-shift the em ission maximum) of all flavones except for the 3-, 5-, and 8-hydroxy isomers; (c) sodium acetate and hydrogen carbonate cause characteristic shifts with 7-hydroxyflavones and, occasionally, with 4 '-hydroxyflavones lacking a 7-hydroxy group; (d) aluminum trichloride produces a longware shift and an enorm ous increae in fluorescence intensity with flavonols; (e) borax can be used to detect sensitively the presence o f a 3 ',4 '-dihydroxy group
Bioactive Polymers, XIV. Immobilization of Ampicillin on BIOZAN R
Authors: Simionescu Cr. , Popa M. I. , Dumitriu S. 
Published: February 2015

The ampicillin coupling on BIOZAN R (a polysaccharide of microbial synthesis Xanthomonas campestris) is studied by the activation of carboxylic groups by dicyclohexylcarbodiimide. The following optimum reaction parameters are settled on the basis of an experimental program: time = 7.5 h, temperature = 10 °C, dicyclohexylcarbodiimide concentration = 1.10-3 mole, ampicilline concentration = 2.4·10-3 mol. Under these conditions up to 37% of ampicillin with respect to the polymer is coupled.
The microbiological and hydrolysis studies under the conditions of the human physiological pH attest the ampicillin maintains its activity and may be released in oral administration.
Oberflächenverbindungen von Übergangsmetallen, XXVII [1] Lumineszenzerscheinungen an Oberflächenverbindungen des Chroms auf Silicagel/Surface Compounds of Transition Metals, XXVII [1] Luminescence Phenomena of Chromium Surface Compounds on Silicagel Supports
Authors: Morys Peter , Gorges Ulrich , Krauss Hans-Ludwig 
Published: February 2015

The red chem iluminescence (CL) of coordinatively unsaturated surface chromium(II) compounds in their reaction with O2 has been studied at various reactivities of the products and various reaction temperatures. With compounds of high reactivity, two CL’s were observed: the first - spectrally unstructured - appears at T ≧ -130 °C, the second - being more intense and spectrally well structure - at T ≧ -90 °C. In course of both these CL’s O2 is released. - Below -130 °C, oxidation takes place without any luminescence. On heating of the reaction product in
vacuo, the luminescence phenomena are observed as a two-stage thermoluminescence (TL).
With the final oxidation product, a photoluminescence (PL) can be stimulated by UV irradiation which is identical with the second CL and shows a well resolved vibrational fine structure at -196 °C. Probably this PL as well as the second CL is produced essentially by an undisturbed monochromate surface species. The first CL and a small part o f the PL is attributed to a topologically broad population of a “disturbed” chromate surface species.
Surface chromium(II) compounds of low reactivity show a one-component CL, TL and PL, almost identical with the first CL mentioned above; they obviously contain the ‘"disturbed” species only.
The mentioned species, defined by their luminescence behaviour, are postulated to be members of the known families of surface chromium occurring in Phillips catalysts, CrA
II and CrB
II, respectively.
Studien zum Vorgang der Wasserstoffübertragung, 71 [1] Tertiäre Phosphine mit ortho-ständigen chelatisierungsfähigen funktionellen Gruppen als Co-Katalysatoren der Homogenhydrierung mit Rh(I)-Komplexen/Studies on the Occurrence of Hydrogen Transfer, 71 [1] Tertiary Phosphines with Functional Groups in the ortho-Position Capable for Chelatization as Co-Catalysts of the Homogeneous Hydrogenation with Rh(I)-Complexes
Authors: Horner Leopold , Simons Guido 
Published: February 2015

By systematic variation of the structure of tertiary phosphines with ortho-phenyl substituted groups as co-catalysts of the homogeneous hydrogenation with Rhodium complexes and hexene-1 as a model compound a collection of data is obtained. By investigating the influence of the variation of the Rhodium/Phosphine-Ratio (Rh/P) (1:1,1 and 1:2,2) on the rate of the hydrogentransfer indirect conclusion can be drawn on the composition of the complexes in the equilibria responsible for the hydrogen transfer.
Results:
1. Steric effects of substituents linked to the ortho-position of a phenyl group in the co-catalyst are very important (compare the Tables I-V especially Table VI).
2. The rate of hydrogenation is strongly influenced by tertiary phosphines with substituents in a ortho-phenyl group capable for coordination like NR2 and SR. With Rh/P = 1:1,1 the rate of the hydrogenation of hexene-1 is mostly faster as with Rh/P = 1:2,2. Depending on steric effects the rate data can be invers.
3. Tertiary arsines with o-dialkylaminophenyl groups are more effective co-catalyst as the corresponding phosphines (Table V).
4. Tertiary phosphines with an ortho-alkylmercaptophenyl group (38-41) are weakly active cocatalysts using Rh/P = 1:1,1.
The thioether 42 (in compounds 12 the diphenylphosphino group is exchanged by the methylmercapto group) is also a moderate active co-catalyst.
5. As a conclusion: it is assumed that complexes of the structure A can coordinate with the substrates hydrogen and olefine . Complexes of the structure B seen to be to stable for the activation of the substrates.
Studien zum Vorgang der Wasserstoffübertragung, 72 [1] Versuche zur enantioselektiven Homogenhydrierung von N-Acyl-α-aminozimtsäuren mit Rh(I)-Komplexen unter Verwendung neuer optisch aktiver Co-Katalysatoren/Studies on the Occurrence of Hydrogen Transfer, 72, [1] Investigation on the Enantioselective Homogeneous Hydrogenation of N-Acyl-α-aminocinnamic Acids with Rh(I)-Complexes Using New Optically Active Co-Catalysts
Authors: Horner L. , Simons G. 
Published: February 2015

3 Optically active compounds of the type I and 15 optically active compounds of the type II were investigated as co-catalysts in the homogeneous hydrogenation of N-acyl-α-aminocinnamic acids using standard conditions. In the co-catalysts of the type I the phosphorus atom is the center of the asymmetry. In the representatives of type II the side chain is optically active and the three bonded phosphorus either achiral or optically active.
The results of the homogeneous hydrogenation are deposited in the Tables I-IV. In the Tables I and IV the degree of the optical induction and the configuration of the excess enantiomer are determined using Rh/P-ratios 1:1,1 and 1:2,2. The Tables II and III show the results applying a Rh/P-ratio of 1:2,2. The observed degree of optical induction is low with the co-catalysts 1-18; only the co-catalyst 19 shows an optical induction of 68%.
A change of the configuration of the excess enantiomer of N-benzoylphenylalanine formed by the homogeneous hydrogenation of N-benzoyl-α-cinnamic acid for the first time was observed by varying the Rh/P-ratio of the co-catalysts 14, 17 and 18 from 1:1,1 to 1:2,2.
Synthese und Struktur einiger Methyl(dicarboxilato)stibane / Syntheses and Structure of Some Methyl(dicarboxilato)stibanes
Authors: Wieber Markus , Wirth Dieter , Burschka Christian 
Published: February 2015

Methyldiethoxistibane and maleic or phthalic acid in a ratio of 1:1 in ethanolic solution at -78 °C react to give methyl(maleato)stibane (1) and methyl(phthalato)stibane (2) respectively. At room temperature polymeric compounds of the same analytical composition are obtained (1a and 2a).
The crystal structure of the solid methyl(phthalato)stibane 2 was determined by X-ray diffraction. It shows that the central antimony atom is hexacoordinated by addition of a solvate ethanol. The correct formula for the solid should be
Ein- und Zweielektronen-Oxidation von Phosphor-Yliden mit Kupfer(II)-Salzen / One- and Twoelectron Oxidation of Phosphorus Ylides Using Copper(II) Salts
Authors: Bowmaker Graham A. , Dörzbach Cornelia , Schmidbaur Hubert 
Published: February 2015

The reaction of CuCl2 with equimolar quantities of an ylide R3P=CH2 (1a-c, R=CH3, C2H5, C6H5) in anhydrous tetrahydrofuran at low temperature leads to oxidative coupling, with ethylidene-1,2-bis-phosphonium salts R3P⊕-CH2-CH2-P⊕R3 2X⊖ (2, 3a-c) as high- yield products. The process is interpreted as a one-electron transfer to give radical cations R3P⊕-ĊH2 (II) which subsequently undergo dimerization. The initial counterions CuCl2
⊖ (in 2a-c) can be replaced by PF6
⊖ (as in 3a-c). (C2H5)3P=CHCH3 (1d) yields the cation (C2H5)3P⊕-*CH(CH3)-*CH(CH3)P⊕(C2H5)3 with two chiral centers as a mixture of diasteromers RR/SS, RS. The ratio of the components is 2,8:1. as evaluated by NMR spectroscopy.
The analogous reaction with (C6H5)3P=CHCH3 and (C6H5)3P=C(CH3)2 (1e, f) takes a very different course. Along with minor quantities of (C6H5)3P⊕CH2CH3/(C6H5)3P⊕CH(CH3)2 species, mainly 1-chloroalkyl-phosphonium cations are formed, which were again isolated as the hexafluorophosphates (4a, 4b: [(C6H5)3P⊕CH(CI)CH3]PF6
⊕, [(C6H5)3P⊕C(Cl)(CH3)2]Pf6
⊖). H-radical trapping from the medium by II ist proposed for the formation of the former, while a two- electron oxidation followed by addition of Cl⊖ is the most plausible mechanism for the generation of the latter
Darstellung und Kristallstruktur von Tl4TiS4, TI4SnS4 und Tl4TiSe4 / Preparation and Crystal Structure of Tl4TiS4, TI4SnS4 and Tl4TiSe4
Authors: Klepp Kurt O. , Eulenberger Günther 
Published: February 2015

Abstract
The isostructural compounds Tl4TiS4, Tl4SnS4 and Tl4TiSe4 crystallize in the monoclinic system, space group P21/c with a = 8.328, b = 8.191, c = 15.248 Å, β = 104.53°; a = 8.395, b = 8.280, c = 15.398 A, ft = 103.69°, and a = 8.517, b = 8.389, c = 15.672 Å, β = 103.50°, respectively. There are four formula units in the unit cell. The crystal structures were determined and refined from single crystal diffractometer data. They are characterized by isolated tetrahedral thioanions which are connected with each other by Tl+ ions. The mean bond lengths are Ti-S = 2.26 Å, Sn-S = 2.40 Å and Ti -Se = 2.38 Å. The Tl atoms are surrounded by six and seven chalcogen atoms, respectively, in an irregular and polar arrangement, thus indicating stereochemical activity of the lone electron pair of the Tl+ ions. Tl-S distances vary from 2.93 to 3.98 Å, Tl-Se distances from 3.03 to 3.96 Å. The Tl atoms have nearest Tl neighbours at distances ranging from 3.46 to 3.65 Å. The crystal structure can be described as built from pseudotetragonal slabs oriented parallel to (001) which contain the cations and the tetrahedral anions. It is shown that a similar description is valid also for the crystal structures of Tl4GeS4 [1] and Na4SnS4 [2, 3].
Der ThCr2Si2-Typ und verwandte Strukturen bei APd2X2- Verbindungen (A = Ca, Sr, Ba; X = P, As) / The The ThCr2Si2-Type and Related Structures of APd2X2-Compounds (A — Ca, Sr, Ba; X = P, As)
Authors: Mewis Albrecht 
Published: February 2015

Abstract
The compounds APd2X2 (A = Ca, Sr; X = P, As) have been prepared and their structures have been determined. They are isotypic and crystallize in the ThCr2Si2-type structure with the following lattice constants:
CaPd2P2 a = 414.5(1) pm, c = 965.9(2) pm;
CaPd2As2 a = 429.9(1) pm, c = 1010.2(2) pm;
SrPd2P2 a = 424.1(1) pm, c = 972.4(2) pm;
SrPd2As2 a = 438.3(1) pm, c = 1017.9(2) pm.
Tetragonal symmetry was also found for BaPd2P2 (a = 425,6 pm; c = 564.7 pm) and BaPd2As2 (a = 434.6 pm; c = 575.8 pm ), but these materials crystallize in a CeMg2Si2-type structure, whereas the lattice of some selected single crystals of BaPd2As2 have tetragonal symmetry (a = 448.7 pm; c = 2063.5 pm) and show structural elements of CaBe2Ge2 - like those of the CeMg2Si2-type structure.
Synthese und Kristallstruktur von Re(NBCl3)Cl2[P(CH3)2C6H5]3, ein Komplex mit einer Nitridobrücke zwischen Rhenium und Bor / Synthesis and Crystal Structure of Re(NBCl3)Cl2[P(CH3)2C6H5]3, a Complex with a Nitrido Bridge between Rhenium and Boron
Authors: Dantona Robert , Schweda Eberhard , Strähle Joachim 
Published: February 2015

Abstract
ReNCl2(PMe2Ph)3 reacts as a Lewis base and with BCl3 forms a nitrido bridge between Re and B. The resulting complex Re(NBCl3)Cl2(PMe2Ph)3 crystallizes orthorhombic in the space group Pn21 a with Z = 4. In the complex each Re atom has six nearest neighbours in an almost octahedral arrangement with the NBCl3 group being trans to one of the Cl ligands. The difference between the two Re-Cl bond lengths (239,4 and 243,9 pm) indicates a weak trans effect of NBCl3. The linear bridge Re≡N-B has bonding distances of Re-N = 172,8 and N-B = 153 pm. Bonding of BCl3 by the nitrido ligand causes a small increase in the Re-N bond distance.
K2SiP2, ein Phosphidopolysilikat(IV) / K2SiP2, a Phosphidopolysilicate (IV)
Authors: Eisenmann Brigitte , Somer Mehmet 
Published: February 2015

Abstract
The new compound K2SiP2 crystallizes in the orthorhombic system , space group Ibam. The unit cell with the lattice constants
a = 1292.6(6) pm, b - 686.7(4) pm, c - 610.7(4) pm
contains 4 formula units. In the structure SiP4 tetrahedra form chains by sharing common edges. The [(SiP2)2-] strings are isosteric to the SiS2 molecules.
Lichtabsorption von oxidischen Silber(I)-Verbindungen / Light Absorption of Silver(I)-oxides
Authors: Friebel Claus , Jansen Martin 
Published: February 2015

Abstract
Diffuse reflectance spectra of Ag2SO4, Ag3PO4, Ag2CO3, Ag2Ge2O5, AgBO2, Ag3BO3-II, Ag6Si2O7, Ag10Si4O13 and Ag10Ge4O13 in the region ν̄ = 10000-40000 cm-1 and generally at 298 K and ambient pressure were measured. Additional spectra were recorded at 5 K for Ag3BO3 and Ag3PO4, and under application of a static pressure of 80 kbar for Ag10Si4O13. As a common feature all spectra show a steep absorption edge, which is only structured in singular cases. The edges appear in the remarkably wide range from 33100 cm-1 (Ag2SO4) to 13500 cm-1 (Ag10Ge4O13). As the shifts correlate with the dimensions of the cluster-like silver partial structures, the absorptions have been attributed to 4d→5s band-band transitions, an interpretation, which is in agreement with the low temperature and high pressure spectra. However, effects originating from charge-transfer transitions cannot be absolutely excluded.
Darstellung von einigen Phenyldicarboxylatostibanen / Syntheses of Some Phenyldicarboxylatostibanes
Authors: Wieber Markus , Fetzer-Kremling Isa 
Published: February 2015

Abstract
Some phenyldicarboxylatostibanes of the general formula

were synthesized by simple metathesis reactions from phenyldiethoxystibane and carboxylic acids in the ratio 1:2. By reaction of 1,2-dicarboxylic acids with phenyldiethoxystibane in the ratio 1:1 phenyldicarboxylatostibanes are also obtained. Some properties and the 1H NMR spectra of these compounds are described, IR data are reported and discussed.
Radikalionen, 61 [1, 2]Dialkylamino-substituierte Acetylene und Allene:Ionisation, Oxidation und AlCl3-katalysierte Wasserstoffübertragung / Radical Ions, 61 [1, 2]Dialkylamino-substituted Acetylenes and Allenes:Ionisation, Oxidation and AlCl3-Catalyzed Hydrogen Transfer
Authors: Bock Hans , Kaim Wolfgang , Kira Mitsuo , Réné Louis , Viehe Heinz-Günther 
Published: February 2015

Abstract
The photoelectron (PE) spectra of bis(dialkylamino) acetylenes R2N-C≡C-NR2 and of tetrakis(dialkylamino) allenes (R2N)2C=C=C(NR2)2 with R = CH3, C2H5 exhibit characteristic ionization patterns which are assigned to π radical cation states of the two molecular halves twisted against each other. The low first ionization potentials between 7.0 eV and 7.7 eV stimu­lated attempts to oxidize using AlCl3 in H2CCl2 or D2CCl2. The hyperfine structured ESR spectra observed can be unequivocally assigned to the ethylene radical cations R2N-HC=CH -NR2˙⊕ which are formed from the obviously non-persistent species R2N-C≡C-NR2˙⊕ via a hydrogen transfer. During the oxidation of the dialkylamino-substituted allenes no paramagnetic intermedi­ates could be detected, presumably due to a rapid dimerisation of the allene radical cation (R2N)2C=C=C(NR2)2˙⊕.
Radikalionen, 62 [ 1—3]Bis(dimethyIamino)dibenzoheptafulven-Radikalkation /Radical Ions, 62 [1—3]Bis(dimethylamino)dibenzoheptafulvene Radical Cation
Authors: Bock Hans , Roth Bernhard , Daub Jörg 
Published: February 2015

Abstract
The neutral title compound, 8,8-bis(dimethylamino)dibenzo-[a,d]-heptafulvene, exhibits a first vertical ionization potential of only 6.98 eV and, therefore, can also be oxidized by AlCl3 in H2CCl2 solution. The radical cation generated shows a complex multiplet signal pattern, which is assigned based on additional ENDOR measurements. The photoelectron (PE) and ESR spectra of the 112 valence electron molecule are interpreted by “pararneter-optimized” HMO and by geometry-optimized MNDO calculations, which both suggest a non-planar π-type ground state with most of the charge and the spin distributed over the dibenzoheptatriene part of the radical cation.
Zur Reaktion von Hexamethyldistannoxan und Hexamethyldistannthian mit Phosphor-oxo- bzw. -thio-halogeniden. Schwingungsspektren von (Me2PS)2O und (Me2PS)2S / On the Reactions of Hexamethyldistannoxane and Hexamethyldistannthiane with Phosphorus-oxy and -thio-halides. Vibrational Spectra of (Me2PS)2O and (Me2PS)2S
Authors: Shihada Abdel-Fattah , Jasim Ihsan A. M. 
Published: February 2015

Abstract
Me3SnO2PCl2 and (Me2PS)2O are prepared from the reactions of (Me3Sn)2O with POCl3 (1:1) and with Me2PSCl (1:2), respectively. The reactions of (Me3Sn)2S with Me2PSCl and with PSBr3 lead to the formation of (Me2PS)2S and P4S9, respectively. POCl3 reacts with (Me3Sn)2S to give unidentified products as a result of O/S exchange. The i.r. and Raman spectra of the solids (Me2PS)2O and (Me2PS)2S and the Raman spectra of the molten compounds are reported and the frequencies assigned.
Graphite Intercalation Compounds with Trimethyltin Chloride
Authors: Schlögl Robert , Boehm Hanns-Peter 
Published: February 2015

Abstract
Intercalation compounds of graphite with Sn(CH3)3Cl have been prepared by UV irradiation, in the presence of graphite, of solutions of Sn(CH3)3Cl, Sn(CH3)4, or of Sn(CH3)4 + SnCl4 in CCl4. Mixtures of stage 1, stage 2, and stage 3 compounds have been obtained. They were characterized by X-ray diffraction, 119Sn Mossbauer spectroscopy, and by chemical analysis. Apparently an oligomeric, anionic species is intercalated together with some solvent.
Synthese und Eigenschaften von TrimethyIstannylmethyl-Indium(III)-Verbindungen / Preparation and Properties of Trimethylstannylmethyl Indium(III) Compounds
Authors: Schumann Herbert , Mohtachemi Reza 
Published: February 2015

Abstract
Trimethyltin methyllithium reacts with InCl3, CH3InCl2 and R2InCl (R = CH3, t-C4H9) with formation of the new compounds In(CH2SnMe3)3, CH3In(CH2SnMe3)2, (CH3)2InCH2SnMe3 and (t-C4H9)2InCH2SnMe3. The compounds are characterized by elemental analyses, 1H, 13C, 119Sn NMR and IR spectra.
Elektrochemische Synthesen, IX [1]Darstellung CO-freier Metallkomplexe / Electrochemical Synthesis, IX [1] Preparation of CO Free Metal Complexes
Authors: Joseph Grobe , Zimmermann Heinz 
Published: February 2015

Abstract
The electrochemical synthesis of metal acetylacetonates (M = Cr, Mo, V, Ti) from metal anodes and acetylacetone is reported. In the presence of oxygen the oxo compounds OM(acac)2 are formed for M = Mo, V and Ti instead of M(acac)3. The electrochemical production of| Ni(PPh3)4 and Fe(PMe3)4 starting from Ni(acac)2 and Fe metal, respectively, has been investi­gated. Successful carbonylation to Ni(CO)n(PPh3)4-n (n = 1,2) or Fe(CO)m(PMe3)5-m (m = 2, 3) proves the hypothesis that replacement of PR3 ligands by CO takes place after reduction of the central metal to the oxidation state 0.
Ferric Chloride Induced Dehydrodimerization of Tetrahydrocarbazole
Authors: Mester I. , Ernst L. , Das B. P. , Choudhury B. , Chowdhury D. N. 
Published: February 2015

Abstract
Ferric chloride induced dehydrodimerization of 1,2,3,4 -tetrahydro -9 H-carbazole (1) gives product 6 , the structure of which was established on the basis of its spectroscopic properties. The 1H and 13C chemical shifts of the aromatic part of 1, as well as of 4a-methyl-2,3,4,4a-tetrahydro-1 H-carbazole (7a) and 4a-phenyl-2,3,4,4a-tetrahydro-1H-carbazole (7b) have also been securely assigned.