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  • 1990-1994  (748)
  • 1890-1899
  • 1994  (393)
  • 1992  (355)
  • 1897
  • Physical Chemistry  (466)
  • crystal structure  (282)
Source
Material
Years
  • 1990-1994  (748)
  • 1890-1899
Year
Keywords
  • 101
    Electronic Resource
    Electronic Resource
    Anomalous polar substituent effect on 15N NMR chemical shifts of Aniline derivatives. Acylanilides and related compounds (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 280-286 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The 15N chemical shifts of various m- and p-substituted anilides and related derivatives, ZNHC6H4Y [Z = C6H5CO, CH3CO, CF3CO, CH3SO2, (C6H5O)2PO and H], were correlated with σ- constants. With all series of anilides investigated, the plotted points for the m- and p-substituted derivatives tend to be separated from each other and to lie on two different regression lines. Reinvestigation from this point of view revealed that similar separations occur generally with substituted aniline derivatives. The anomalous polar substituent effect was ascribed to the very large contribution of a resonance effect. In addition, the local π-polarization effect causes a negative slope for the m-substituted series in the case of carboxylic anilides.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070603
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  • 102
    Electronic Resource
    Electronic Resource
    Water-Catalysed hydrolysis of p-nitrobenzyl cellulose xanthate (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 287-295 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The spontaneous hydrolysis of p-nitrobenzyl cellulose xanthate (CelXNB) with a degree of substitution (DS) in the range 2-9 was studied in 10% aqueous ethanol at pH 10, and was followed spectrophotometrically by the appearance of p-nitro-α-toluenethiol, in a continuous-flow system where the reactor was shaken. CelXNB was characterized by solid-state 13C NMR spectra. The reaction occurs through two parallel processes due to two xanthate ester groups with different reactivities. The fast hydrolysis was ascribed to the reaction of the C-2 + C-3 isomers, whereas the slow hydrolysis was due to the C-6 isomer. The percentage of the latter is much higher than C-2 + C-3. The solvent isotope effect of the fast hydrolysis (k′H2O/)k′H2D 11 was 2·22 ± 0·16 and the proton inventory indicated that there is only one proton transfer involved in the transition state, where a second water (or a neighbouring OH group) acts as a general base. The entropy of activation of the fast hydrolysis was only 3·3 ± 0·8 e.u., suggesting that the water molecules involved are highly oriented with respect to the coordinates required to reach the transition state. It is proposed that they form part of the three-dimensional hydrogen-bonded ice-like structure that involves the cellulose matrix.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070604
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  • 103
    Electronic Resource
    Electronic Resource
    Spectrometry and reactivity of phenalenyl anions (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 296-302 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The aromatic odd-alternant phenalenyl anion and a number of its derivatives were prepared in order to study the perturbation of this conjugated anion by methyl and methoxy groups. The conjugated anions were studied by means of 1H and 13C NMR spectrometry, alkylation experiments and semi-empirical calculations. It was found that a substituent at a charged carbon atom perturbs the entire conjugated system, whereas substituents at inactive (uncharged) carbon atoms have a large effect on the positions ortho to the substituent.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070605
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  • 104
    Electronic Resource
    Electronic Resource
    Potentiometric evaluation of the ion-selective characteristics of 1,4-bridged cubyl diester crown ethers (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 303-308 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Cubane diester crown ethers were tested as ion-selective electrodes in poly(vinyl chloride) (PVC) membranes. The four ionophores studied proved to be good K+ neutral carriers, showing Nernstian and near-Nernstian responses to this ion, in the range 10-4-10-1 M. The fixed interferences method was used to determine relative selectivity coefficients for all the electrodes. The highest selectivity for potassium relative to sodium, lithium, calcium and magnesium ions using potassium tetrakis(p-chlorophenyl)borate (KTpClPB) as a resistance modifier and NPOE as a plasticizer was obtained with the 1,4-cubyl diester-25-crown-7 ether ionophore. The effects of KTpCIPB on membrane selectivity were assessed; its removal was found to increase the selectivity of the four ionophores for potassium relative to cesium, sodium, calcium and magnesium ions with minimal effects on lithium and ammonium ions. The compounds tested exhibited a fast Nernstian response to changes in K+ concentration which was stable to within 〈100 μV h-1.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070606
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  • 105
    Electronic Resource
    Electronic Resource
    Erratum (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 323-323 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070609
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  • 106
    Electronic Resource
    Electronic Resource
    Orbital-controlled reactions catalysed by zeolites: Electrophilic alkylation of aromatics (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 364-370 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The role of orbital control in product selectivity during electrophilic aromatic alkylation catalysed by zeolites was studied both theoretically and experimentally. In order to discuss this, the alkylation of toluene and m-xylene by methanol was carried out on a series of large-pore zeolites (HY). The changes in the para to ortho ratio observed on changing the framework Si/Al ratio of the zeolites were related to ab initio molecular orbital calculations of the LUMO energy of structurally alike model clusters but containing different tetrahedral cations around the active site. The observed correlation is discussed in terms of the HSAB principle by taking into account the influence of the catalyst composition on the reactivity of the electrophilic reagent.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070706
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  • 107
    Electronic Resource
    Electronic Resource
    Erratum (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 394-394 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070710
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  • 108
    Electronic Resource
    Electronic Resource
    Masthead (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994) 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070801
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  • 109
    Electronic Resource
    Electronic Resource
    The kinetics and mechanism(S) of nucleophilic attack by catecholate anion on epibromohydrin-d2 (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 395-398 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The reaction which forms hydroxymethylbenzodioxane from epibromohydrin and catecholate anion was examined by ultraviolet spectroscopy for the kinetics and by proton nuclear magnetic resonance spectroscopy to follow the fate of CD2 from reactant to product. Over the practical temperature range it was found that both CH2 positions in the epihalohydrin are attacked by catecholate anion to give product. Therefore, the difference in energy for the two pathways was small. The individual rate constants were obtained from the total rate constants. Further, the individual ΔH
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070802
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  • 110
    Electronic Resource
    Electronic Resource
    Mechanism of reaction of azobenzene formation from aniline and nitrosobenzene in basic conditions. General base catalysis by hydroxyide ion (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 399-402 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The reaction of nitrosobenzene with aniline, to give azobenzene, in basic conditions was studied. It was shown that the reaction exhibits general base catalysis by different buffers giving a Brønsted coefficient β = 0·318. As in previous studies, a two-step process with a first step of attack of aniline on nitrosobenzene to give an addition intermediate and a second step of dehydration of this intermediate is proposed to interpret the mechanism of the reaction. The analysis of the Brønsted relationship and of the intermediate of the reaction led to the suggestion that hydoxide ion catalyses the reaction by a mechanism of general base catalysis in the dehydration step.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070803
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  • 111
    Electronic Resource
    Electronic Resource
    Micellar catalysis of organic reactions. Part 36. Nucleophilic aromatic substitution reactions in hydroxy functionalized micelles with bulky head groups (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 442-447 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The reaction of several nitro activated aromatic halides with hydroxide ions was studied in the presence of hydroxy functionalized micelles containing bulky head groups, e.g. C16H33N+R2CH2CH2OH Br-, where R = Me, Et, Bu. In a biphasic reaction, the aryl halide is first converted into an aryl mincellar ether which subsequently reacts with hydroxide ions to form the phenolic product. Despite the increased nucleophilicity of hydroxide ions as water is squeezed away from the micelle surface by the bulky head groups, no direct reaction of the aromatic substrate with hydroxide ion is detectable. In the second phase of reaction, the breakdown of the aryl micellar ether to form the phenolic product, the order of reactivity in the different micelles is dependent on the steric interactions between substituents ortho to the reaction centre and the head group of the micelle. For compounds having one substituent ortho to the reaction centre, the order of reactivity is Bu 〉 Me 〉 Et, whereas for 2-chloro-1,3-dinitrobenzene, which has two substituents ortho to the reaction centre, the order is Me 〉 Et 〉 Bu.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070809
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  • 112
    Electronic Resource
    Electronic Resource
    Probing onium ions and carbocations by desorption/ionization mass spectrometry: Crossing the threshold between fragile salts and gaseous intact cations and subsequent guest-host and cation-molecule cluster chemistry (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 465-478 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The utility of desorption/ionization mass spectrometric (DI/MS) techniques in dealing with physical organic problems involving fragile onium salts and carbocation salts has been explored. The efficacy of these methods, especially when coupled to tandem mass spectrometry, goes much beyond the analytical aspects dealing with identity/purity determinations. For example, insight can be gained regarding the role of the counterion in subsequent cation decomposition pathways. Guest-host chemistry of onium ions and various hosts (crowns, calixarenes) can be probed. The decomposition chemistry of the resulting ion-molecule clusters can be studied. Examples of onium salts and carbocation salts that have been studied are few, probably because research in this area has been mainly a domain for analytical chemists. This paper calls attention to the possibilities for dealing with topical physical organic problems.
    Additional Material: 23 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070902
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  • 113
    Electronic Resource
    Electronic Resource
    Solvolysis of 3-substituted 4-homoadamantyl methanesulphonates. Can the β-substituent effect distinguish between classical and non-classical ion intermediates? (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 485-494 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The rates of the solvolysis of 3-R-4-homoadamantyl methanesulphonates (mesylates) (3) were determined in 80% aqueous ethanol. The relative first-order rate constants at 25 °C were 1·0 (R = H), 2·29 (R = Ph), 3·26 (R = p-anisyl), 73·6 (R = Me) and 209 (R = Et). The methanolysis of 3 gave rearranged methyl ethers and rearranged olefins as major products together with small amounts (0·9-3·4%) of unrearranged products. The order of the accelerating effect suggests that the transition states involve significant σ-participation, despite the fact that 3 (R = H) solvolyses via a classical ion intermediate. The logarithms of the solvolysis rate constants of 3 showed linear correlations with those of 1-R-2-adamantyl tosylates (1) and 1-R-exo-2-norbornyl tosylates (2), indicating that the linear free-energy relationship between the β-substituent effects on the solvolysis rate is not a definite measure to distinguish between classical and non-classical intermediates.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070904
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  • 114
    Electronic Resource
    Electronic Resource
    Intramolecular exchange coupling of arylnitrenes by OXYGEN (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 495-502 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A series of m,n′-diazidodiphenyl ethers (m ≤ n, m = 3,4; n = 3,4) was photolyzed at 77 K in frozen, glassy 2-methyltetrahydrofuran matrices to generate the corresponding diphenyl ether m,n′-dinitrenes for study by electron spin resonance (ESR) spectroscopy. 3,4′-Diazidodiphenyl ether gave an ESR spectrum dominated by a mononitrene peak with ∣D/hc∣ = 0·972 cm-1, and also showed a weak dinitrene quintet spectrum with ∣D/hc∣ = 0·162 cm-1 having ESR spectral intensity vs temperature dependence (Curie law) consistent with either a high-spin ground state or a very small singlet-quintet gap. Di(3-azidophenyl) ether gave a strong mononitrene peak with ∣D/hc∣ = 0·996 cm-1 and a quintet dinitrene ESR spectrum (∣D/hc∣ = 0·162 cm-1) which exhibited non-linear Curie law intensity behavior consistent with the quintet being a thermally populated excited state 40 cal mol-1 above a singlet ground state. Di(4-azidophenyl) ether gave a strong mononitrene peak with ∣D/hc∣ = 0·961 cm-1, but no observable spectrum related to a high-spin open-shell dinitrene. The results are consistent with oxygen being a weak exchange coupling linker in pi-conjugated open-shell molecules. The observed ground-state spin multiplicities are in accord with qualitative superexchange and connectivity models, despite any perturbations due to resonance effects between the oxygen linker and p-nitrene sites.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070905
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  • 115
    Electronic Resource
    Electronic Resource
    Kinetic studies of the reactions of phthalimide with ammonia and pyrrolidine (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 518-524 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The kinetics of the nucleophilic cleavage of phthalimide (PTH) in buffer solutions of ammonia and pyrrolidine were determined. The reaction rates for ammonolysis of PTH revealed a buffer-catalysed second-order term in the rate law, but the reaction rates for pyrrolidinolysis of PTH showed buffer-catalysed second- and third-order terms in the rate law. Both ammonia and pyrrolidine revealed nucleophilic reactivity towards ionized PTH (S-) only within the pH range of the present study. This is attributed to the occurrence of intramolecular general base-acid catalysis. General base catalysis is detected in the reactions of pyrrolidine with both non-ionized PTH (SH) and S-. The general base-catalysed third-order rate constant for pyrrolidinolysis of SH is nearly 28 times larger than that of S-.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070908
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  • 116
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    SINDO1 study of the photochemical synthesis of azacyclobutadiene from 1,4-oxazin-2-one (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 503-510 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The mechanism of the photochemical decomposition of 1,4-oxazin-2-one to azacyclobutadiene and carbon dioxide was investigated by the semi-empirical MO method SINDO1. The relevant singlet and low-lying triplet potential energy hypersurfaces were studied and intermediates and transition structures were optimized with limited configuration interaction. The first step transforms 1,4-oxazin-2-one into a bicyclic lactone via internal cyclization. Then a stepwise bond breaking mechanism on the first excited triplet state yields azacyclobutadiene and CO2, whereas a reaction on the first excited singlet state is not common. It is shown that a simultaneous bond-breaking mechanism on the first excited singlet or on the first excited triplet is possible.
    Additional Material: 13 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070906
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  • 117
    Electronic Resource
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    Unproductive sigma and pi complexes in the reaction of 2-chloroquinoxaline with piperidine in dimethyl sulphoxide (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 545-550 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The rate of the reaction of 2-chloroquinoxaline with piperidine in dimethyl sulphoxide was measured over a wide range of amine concentrations and at several temperatures. It was found that the order with respect to the nucleophile is close to 1 between 300 and 320 K, but is definitely less at lower and higher temperature. It is suggested that below 300 K an unreactive charge-transfer complex is formed between the reactants which dissociates at higher temperatures, whereas at temperatures higher than 320 K an unproductive σ complex is formed, the concentration of which increases with increase in temperature.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610071004
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  • 118
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    Linear solvation energy relationships between electrolyte pK values and solvent properties for several 2-methylpropan-2-Ol-cosolvent mixtures (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 696-704 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The dissociation pK values of picric acid, tetrabutylammonium picrate, bromide and hydroxide and tetramethylammonium hydroxide in some 2-methylpropan-2-ol-cosolvent mixtures were determined and correlated with the Taft and Kamlet solvatochromic parameters π*, δ, α and β. The results show the most important solvent properties that affect electrolyte dissociation are polarity, polarizability and hydrogen bond acidity. These results were confirmed by analysis of published literature data.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610071207
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  • 119
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    Hydrogen bonding. 38. Effect of solute structure and mobile phase composition on reversed-phase high-performance liquid chromatographic capacity factors (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 672-684 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Reversed-phase HPLC capacity factors, as log k′, have been correlated through the LFER equation: \documentclass{article}\pagestyle{empty}\begin{document}$${\rm log k}^\prime = {\rm c} + {\rm rR}_2 + {\rm s\pi }_2^{\rm H} + {\rm a}\sum {\rm \beta }_2^0 + {\rm vV}_{\rm X}$$\end{document} where k′ is the capacity factor for a series of solutes in a given stationary phase-mobile phase system, and the explanatory variables are the solute descriptors: R2 an excess molar refraction, π2H the dipolarity/polarizability, Σα2H the overall hydrogen-bond acidity, Σβ20 the overall hydrogen-bond basicity and Vx the McGowan volume. This equation was applied to various C18 stationary phases with methanol-water, acetonitrile-water and tetrahydrofuran-water buffered mobile phases. The solute and mobile phase factors that influence log k′ values are set out, and a comparison is made between log k′ values and water-octanol partition coefficients.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610071205
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  • 120
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    Topological analysis of electronic charge densities as a tool to study protonation effects on thiocarbonyl compounds (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 685-695 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The substituent effects on the intrinsic basicity of a wide variety of thiocarbonyl compounds were investigated by means of a topological analysis of the electronic charge densities and their Laplacians for the neutral and the protonated species, and also by means of their harmonic vibrational frequencies. For the sake of comparison, a similar analysis was carried out for a reduced set of carbonyl compounds with similar substituents. The results show that the behaviour of the thiocarbonyl group with regard to the protonation process is similar to that predicted for the carbonyl group, in the sense that both groups are not much affected by protonation. The charge transferred to the proton results basically in a polarization and, in some cases, in a depopulation of the bonds in which the thiocarbonyl carbon atom participates. Accordingly, the intrinsic basicities of these kinds of compounds depend strongly on the ability of the substituents to be polarized. This conclusion seems to be ratified also by the shiftings undergone by the C=S stretching frequencies on protonation.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610071206
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  • 121
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    Carbonyl oxygen as a hydrogen-bond super-base: The amidates (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 705-711 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: An infrared spectroscopic study of the 1 : 1 hydrogen-bond association of amidates with both methanol and 4-fluorophenol showed that the site of complexation is the oxygen of the amidate function. However the formamidate HCON2Me3 forms a second 1 : 1 complex on the nitrogen of the amidate. The formation constants of the hydrogen-bond complexes of the amidates with the reference hydrogen-bond donor 4-FC6H4OH indicate that the amidates are stronger hydrogen-bond bases than are amides and amide vinylogues. As such, the amidates constitute the strongest carbonyl bases hitherto investigated on the hydrogen-bond basicity scale.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610071208
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  • 122
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    Hydrogen bonding. 39. The partition of solutes between water and various alcohols (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 712-716 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The general solvation equation \documentclass{article}\pagestyle{empty}\begin{document}$${\rm logSP} = {\rm c} + {\rm rR}_2 + {\rm s\pi }_2^{\rm H} + {\rm a}\sum {\rm \beta }_2^{\rm H} + {\rm vV}_{\rm X}$$\end{document} was applied to the partition of solutes between water and isobutanol, pentanol, hexanol, octanol, decanol and oleyl alcohol. It is shown that the two main factors that influence partitioning are solute hydrogen-bond basicity Σβ2H and solute volume Vx. The b coefficient becomes steadily more negative along the above series of alcohols, showing that the alcoholic phases, which are all less acidic than water, become less and less acidic as the chain length increases, and the water content of the alcoholic phase decreases. The v coefficient, on the other hand, becomes gradually more positive, indicating that as the chain length increases and the water content decreases, the alcoholic phase becomes more and more hydrophobic. Of great significance is that for all six alcohols, the a coefficient is effectively zero, so that all alcoholic phases have the same basicity as bulk water, no matter what their water content is. It is suggested that, contrary to results of solvatochromic measurements, the alcohols have similar hydrogen-bond basicity to water.
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610071209
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    Superbases in the gas phase. Part II. Further extension of the basicity scale using acyclic and cyclic guanidines (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 725-733 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The superbase gas-phase scale has been further extended up to proton affinities of ca 1080 kJ mol-1 by use of cyclic and acyclic guanidines and vinamidines. Structural features such as Y-conjugation, vinylogy and intramolecular ionic hydrogen bonding leading to their superbasic behaviour are analysed. Solvation effects by water and acetonitrile on basicity are discussed. From a correlation pKa(acetonitrile) vs gas-phase basicity, proton affinity values in the range 1070-1410 kJ mol-1 are predicted for Schwesinger phosphazene compounds.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610071211
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    Rechecking of the equilibrium gas-phase basicity scale for low-basicity compounds using fourier transform ion cyclotron resonance spectrometry (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 717-724 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Fourier transform ion cyclotron resonance (FT-ICR) spectrometry was used to study and recheck the proton transfer equilibria for a large number of low-basicity compounds, particularly those which are less basic than H2O. The data obtained were used for the construction of a continuous scale of the relative gas-phase basicities between H2S and SO2F2. The present results are compared with the results obtained by McMahon and co-workers using ICR spectrometry and high-pressure mass spectrometric (HPMS) techniques. Satisfactory agreement is found with the existing ICR spectrometric data. The results, however, show unexplained variances with earlier and recent HPMS results that also not internally self-consistent. The substituent effects for some families of low-basicity compounds (nitriles, carbonyl compounds, ethers and some others) are discussed.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610071210
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    Model solvent systems for QSAR. Part IV. The hydrogen bond acceptor behaviour of heterocycles (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 743-750 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: An LSER analysis based on the partitioning of 15 proton acceptor heterocycles has succeeded in extracting Σβ values, but only at the cost of demonstrating solvent dependence for some of them. As noted by Abraham, the division lies between protic and aprotic organic phases. His observation that pyridine and quinoline are less effective acceptors when surrounded by solvent than in 1 : 1 association was confirmed, and possible reasons for this are discussed. Two other such cases are N-methylimidazole and pyridazine, both of which give lower Σβ values in octanol than in PGDP. For both, Σβ in PGDP is what would be expected on the basis of log Kβ. The value for pyridazine in octanol suggests that, here, the ‘α-effect’ is no longer operative; it is possible that this result can be generalized to other such heterocycles. Elsewhere, the most remarkable finding is that, where there are two proton acceptor sites in one heterocyclic ring, Σβ is the simple unattenuated sum of the separate βf values. If this result is general, it leads to a very simple way of estimating Σβ for heterocycles by calculation where data are unavailable. Evidence was also found, in certain cases, for hydrogen bonding to the π-donor heteroatom or the aromatic ring. The QSAR implications of these results are discussed.
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610071213
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    Distinguishability of liquid environments in the presence of brownian noise (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 734-742 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: This paper extends previous work on the dynamic averaging of distinct liquid environments by cage exchange to include potential energy fluctuations at the cage centers due to Brownian motions of molecules in the cage walls. After a brief review of the effect of cage exchange on the Schrödinger wave train associated with the electronic ground state of the caged molecule, typical magnitudes and time-scales for the Brownian potential energy fluctuations are estimated. Then a zig-zag model for the resulting noise in the wave trains is developed, and applied to analyze distinguishability in the presence of noisy cage exchange. When distinguishability survives the noise, the distinct caged species are fully fledged environmental isomers. Applications of these concepts are discussed.
    Additional Material: 10 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610071212
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    Cryptate acidity scales. Solvent polarity effect on ion-pair and free ion acidity of organic compounds (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 181-191 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: [2.1.1] Cryptated lithium salts of a wide range of CH-acids were studied spectrophotometrically and conductimetrically in solvents of low polarity. Such salts exist in media of different dielectric constants in the form of cryptand-separated ion pairs which are identical in their spectral and conductance properties with common solvent-separated ion pairs. No formation of higher ionic clusters was observed for the studied ions at concentrations below 10-3 mol-1 even in the benzene. The relative equilibrium acidities in benzene, N-methylmorpholine and tetrahydrofuran for a number of CH-acids are reported. Solvent polarity does not influence the cryptate ion-pair acidity of the investigated compounds. The relative free ion acidities were calculated for some of the studied acids in different solvents by combination of the ion-pair acidity values with the conductimetric data on dissociation constants of the cryptate ion pairs. A linear relationship between the free ion acidity and the reciprocal of the dielectric constant was found. An extrapolation method is suggested for the calculation of gas-phase acidity from the data obtained in solution.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610070404
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    Selectivity of nitration reactions of aromatic compounds on zeolites H-Y and H-ZSM-11 (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 385-393 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Substrate and positional selectivity in the nitration reactions of benzene and its derivatives (halobenzenes, toluene and o-xylene) by nitric acid and acyl nitrates supported on zeolites H-Y and H-ZSM-11 were studied. The reaction mechanism and effects governing selectivity of the process are discussed.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610070709
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    Polyaniline intercalated into zeolites, zirconium phosphate and zirconium arsenate (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 371-376 
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    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Aniline (or aniline hydrochloride) was intercalated into zeolite, zirconium phosphate and zirconium arsenate (proton form and sodium form) and subsequently oxidized to polyaniline (PAN) by ammonium peroxodisulphate. The structure of PAN in the host was studied by electron paramagnetic resonance spectroscopy. PAN in the host gave a free-radical EPR signal at 2·0035-2·0037 for the hydrogen or 2·0047-2·0049 for the sodium form of the host, similarly to the ermeraldine salt (PAN-2S) or emeraldine base (PAN-2A) form of PAN. Saturation occurs in PAN-HZ and PAN-HS. In contrast, the intrachannel PAN in HY was unsaturated under the same conditions. Conduction in PAN-HZ and PAN-HS was predominately carried out by variable-range hopping and tunnelling respectively, and PAN-HY showed insulating properties.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610070707
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    Catalytic and computer simulation studies of carbon-sulphur bond cleavage over zeolite-YNCL Communication No. 5768. (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 377-384 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: N-Substituted carbonimidodithioic acid dimethyl esters, when reacted with an active methylene compound such as nitromethane, undergo carbon-carbon bond formation followed by carbon-sulphur bond cleavage in the presence of zeolite catalysts to give 1-substituted amino-1-methylthio-2-nitroethenes. This carbon-sulphur bond cleavage is facilitated by the presence of rare earth cations in the zeolite-Y framework. The shape selectivity of the zeolite also plays an important role in this cleavage reaction. Force field calculations adopted for the molecules involved in the reaction indicate the geometry and conformational flexibility of these molecules. The computer-simulated model for the zeolite-Y is correlated with the conformation and shape of the reactant and product molecules to explain the variation in yields obtained in the conversion of substituted dimethyl esters.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610070708
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    σ-π and η-π Stabilization energies in vinyl and phenyl compounds (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 403-411 
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    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A means for determining the stabilization energies, Ec(X), resulting from σ-π and n-π interactions in vinyl and phenyl compounds is described. It is based on extensions of the additivity principle for thermochemical data for organic compounds. The results also provide a method for predicting heats of formation of unsaturated compounds from those of (known) saturated analogues. It is shown that there is a linear relationship between the stabilization energies Ec(X) and the Hammett substituent constants σp+(X). The new results have been used to predict the heats of formation of a number of saturated and unsaturated Si-, Ge-, Sn-, P-, As-, Se-, Zn-, Cd- and Hg-containing species.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610070804
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    Salt and solvent effects on alkaline hydrolysis of N-hydroxyphthalimide. Kinetic evidence for ion-pair formation (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 412-419 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The effects of the concentrations of LiCl, NaCl, KCl, CsCl, Na2CO3 and BaCl2 on the rates of reactions of hydroxide ion with ionized N-hydroxyphthalimide (NHP-) at 30°C and in H2O-MeCN solvents containing 10, 50, 60, 66, 70, 76 and 80% (v/v) MeCN reveal the formation of ion-pair complexes between cations of the salts, which probably exist in solvent-separated loose ion-pair forms (Mn+⃛Xk-) and NHP-. An increase in MeCN content from 2 to 76% (v/v) causes an increase in the association constants (K) by factors of 40, 21 and 9 for LiCl, NaCl and KCl, respectively, while the respective increase in the rate constants (k′s1) for the collapse of the ion-pair complexes to product is ca two-fold. The values of k′s1 remain almost unchanged whereas the values of K increase 7·5-fold with an increase in MeCN content from 2 to 70% (v/v) for CsCl. Ion-pair complex formation was not detected in the presence of Me4NCl at 70% (v/v) MeCN. The observed pseudo-first-order rate constants are highly sensitive to the valence state of cations and almost insensitive to the valence state of the anions of the salts.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610070805
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    Bimolecular nucleophilic substitution at a resonance-stabilized carbenium ion: Elevated value of cross-interaction constant, imbalanced transition state and the non-interactive phenomenon (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 448-454 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A characteristic feature in the bimolecular nucleophilic substitution reactions at a resonance-stabilized carbenium ion has been shown to be an imbalanced transition state resulting in an elevated value of the cross-interaction constant, which in turn leads to a non-interactive phenomenon. Examples of the reactions of ring-substituted phenylethyl and benzhydryl cations are given.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610070810
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    Masthead (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994) 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610070901
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    Solvolyses of 4-methylene-2ax- and -2eq-adamantyl p-toluenesulphonates: Intermediacy of classical carbocation in the axial and π-bridged carbocation in the equatorial ptoluenesulphonate solvolyses (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 455-464 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The rates and products of solvolyses of 4-methylene-2ax- and -2eq-adamantyl p-toluenesulphonates (tosylates) (4a-OTs and 4e-OTs, respectively) were studied. Compound 4a-OTs solvolysed more slowly than 2-adamantyl tosylate (1) in methanol and 2,2,2-trifluoroethanol (TFE) by factors of 2·3 and 2·5, respectively, at 25°C. However, by taking the inductive decelerating effect of a β-methylene substituent into account, the rates were revealed to be enhanced by α-participation by a factor of 50. The products of solvolyses of 4a-OTs in methanol, 80% acetone and TFE at 100°C were 2ax- and 2eq-alkoxy(or hydroxy)-4-methyleneadamantanes (4a-OR and 4e-OR, respectively), exo-4-alkoxy(or hydroxy)-5-methyleneprotoadamantane (exo-5-OR) and 5-[alkoxy(or hydroxy)methyl]-4-protoadamantene (6-OR) with adamantyl to protoadamantyl product ratio of 39:61 (in methanol), 56:44 (in 80% acetone) and 71:29 (in TFE). Despite the nearly symmetric nature of the intermediate cation, the 4a-OR: 4e-OR product ratio was essentially constant with 83:17 (in methanol), 85:15 (in 80% acetone) and 82:18 (in TFE). The formation of considerable amounts of 4e-OR was interpreted as showing the intermediacy of a pair of rapidly equilibrating classical ions. The rates of 4e-OTs were 2300-4300 times faster than those expected from inductive electron-withdrawing effect of a β-methylene substituent. The major product (84·5% in methanolysis and 98·7% in trifluoroethanolysis) was 4e-OR accompanied by small amounts of 2-alkoxy-2,4-methanoadamantane (9-OR) and 2-(alkoxymethyl)-2,4-didehydroadamantane (10-OR), no formation of 4a-OR having been observed. These results suggested that 4e-OTs solvolyses via a π-bridged intermediate cation.
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    URL: http://dx.doi.org/10.1002/poc.610070811
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    Determination of complex stabilities with nearly insoluble host molecules. Part I. Spectrophotometric detection (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 479-484 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The determination of stability constants by measuring the increase in solubility of a nearly insoluble host molecule due to complex formation with a soluble guest is discussed. If the host molecule absorbs in the UV-visible region, spectrophotometric measurements are easily performed to obtain the stability constants. The solubilities of the crown ether dibenzo-18-crown-6 and of the cryptand (222BB) in aqueous solutions and the molar absorptivities of these ligands and their complexes with alkali and alkaline earth metal cations were determined. The increase in solubility of these ligands due to complex formation with cations was used to calculate the stabilities of the complexes formed. Even under the assumption that neither the molar absorptivities nor the solubilities are known, the calculated stability constants agree very well with those obtained using the measured values of the molar absorptivities and solubilities. The accuracy of the stability constants even increases with decreasing solubility of the ligands.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610070903
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    Acidity and basicity of thiocarboxamides in the gas phase (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 511-517 
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    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The gas-phase acidity and basicity of thioacetamide and the basicity of N,N-dimethylthioformamide were measured by Fourier transform ion cyclotron resonance (FT-ICR) mass sectrometry under conditions which minimized the extent of their decomposition. Thiocarboxamides are both much stronger acids and stronger bases than carboxamides. The relative stabilities of individual neutral and ionic species were assessed in terms of isodesmic reactions, using the published or estimated enthalpies of formation. The neutral molecules of carboxamides and thiocarboxamides are stabilized by interaction between the C = X and NH2 functional groups. This interaction is of a similar magnitude in the corresponding protonated forms but it is of greater strength in the deprotonated forms. With regard to the difference between thiocarboxamides and carboxamides, the most significant factor is probably the Ione pair-Ione pair repulsion operating in the anions.
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    URL: http://dx.doi.org/10.1002/poc.610070907
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    Masthead (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994) 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610071001
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    Kinetics and mechanism of the interaction of amines with aryl β-haloethyl sulphones (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 525-533 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The influence of a number of factors, i.e. amine basicity, substrate structure, temperature and deuterium isotope effect, on the rate of phenyl β-bromoethyl sulphone and aryl β-chloroethyl sulphone 1,2-elimination by reaction with amines in acetonitrile was investigated. On the basis of a comparative analysis of the ρ0, β, kH/kD, ΔH
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610071002
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    Synthesis and photophysics of diaza-crown ether-based bisporphyrins (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 534-544 
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    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The bisporphyria N,N′-bis[4″-(meso-triphenylporphyrinyl)benzyl]-4,13-diaza-18-crown-6 and its mono- and dizinc derivatives were synthesized in 66%, 46% and 53% yields, respectively, from 5-(4′-bromomethylphenyl)-10,15,20-triphenylporphyrin or its zinc derivative and 4,13-diaza-18-crown-6. The zinc-containing bisporphyrins form dimers in solution at low temperature or at high concentration. The unsymmetrical bisporphyrin; monozinc N,N′-bis[4″-(meso-triphenylporphyrinyl)benzyl]-4,13-diaza-18-crown-6 shows singlet-singlet energy transfer from the zinc porphyrin moiety to the free base moiety in both the monomeric and the dimeric form. The energy transfer rates were determined using time-resolved fluorescence spectroscopy and were found to be 1·26 × 109 and 2·29 × 109 s-1 for the monomeric and dimeric form, respectively. The difference in energy transfer rates between the two forms can be rationalized by the difference in overlap between the donor fluorescence spectrum and acceptor absorption spectrum, donor-acceptor distance and donor-acceptor orientation.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610071003
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    Molecular mechanics (MM3) study of the structures and energetics of corannulene (C20H10), cyclopentacorannulene (C22H12) and the hemi-spherical C30H10 (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 551-554 
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    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Molecular mechanics (MM3) calculations were carried out on the title compounds. Comparison between the MM3 results and those of semi-empirical and ab initio calculations and experiment indicates that the MM3 results are at least as good as results of much more expensive calculations. The MM3 calculations predict that unlike corannulene and cyclopentacorannulene, the transition state of the bowl-to-bowl inversion of the related C30H10 is non-planar, and the activation barrier is too high for this motion to occur.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610071005
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    Calorimetric study of the anomeric effect in 2-carboethoxy-1,3-dithianes (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 561-566 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The enthalpic contribution to the anomeric effect in r-2-carboethoxy-trans-4,trans-6- and r-2-carboethoxy-cis-4,cis-6-dimethyl-1,3-dithianes was determined by reaction-solution calorimetry. The enthalpy of solution of both isomers in pure p-dioxane and the enthalpy of solution and isomerization in the same solvent and in the presence of trifluoroacetic acid were experimentally measured. From these results the corresponding enthalpies of isomerization in solution were calculated, and were found to be ΔHax→eq = -0·16 ± 0·04 kcal mol-1 (-0·67 ± 0·18 kJ mol-1) and ΔSax→eq = -2·68 ± 0·1 cal K-1 mol-1 (-11·2 ± 0·4 J K-1 mol-1). The slightly negative ΔH term nevertheless reflects a substantial anomeric effect owing to the countervailing steric effects in the axial isomer. The significant entropy loss in the equatorial isomer was explained in terms of intramolecular electrostatic effects. The results are in agreement with those obtained from NMR studies of the conformational behaviour of 2-carboethoxy-5-methyl-5-aza-1,3-dithiacyclohexane.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610071007
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  • 143
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    Masthead (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994) 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610071101
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  • 144
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    Reactions of iminodimagnesium reagents with 1,4-quinones: Their structural factors governing the modes of reactionsAryliminodimagnesium Reagents. Part XXVI. For Part XXV, see M. Okubo, Y. Inatomi, I. Eguchi, H. Nishida, S. Gotoh and K. Matsuo, J. Phys. Org. Chem. 7, 18 (1994). (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 567-577 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Reactions of benzo-, naphtho- and anthraquinone derivatives (unsubstituted and substituted) with aryliminodimagnesium [ArN(MgBr)2] and aryloxymagnesium of a weak electron-donating ability were studied. In addition to the reduction products (quinhydrones and hydroquinones), nuclear substitution and condensation products were formed. The efficiency of single electron transfer (SET) from ArN(MgBr)2, evaluated by the relative values of the difference between the oxidation and reduction potentials of the reactants (ΔE = Eox - Ered), varies with the electron-accepting power of quinones. ΔE governs the modes of semiquinone appearance (ESR signals) and the relative amounts of the heat of reactions, reflecting the types and yields of the products. It is concluded that condensation products of both components are produced in the reactions of quinones with the lower SET efficiency by the presence of a fused benzene ring or MeO substituent. The structure-reactivity relationship proposed previously for reactions of various magnesium reagents is extended in the reactions with a variety of quinones even in cases of higher SET efficiency.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610071008
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  • 145
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    An unusual parabolic dependence of rate on acidity in the fischer indole reaction (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 625-628 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Over the H0 acidity range from + 2 to -8, four different mechanistic variations occur in the Fischer indole reaction, leading to an unusual parabolic dependence of the rate constants on the acidity of the medium. In strongly acidic media kinetic isotope effects indicate that the rate-determining step is deprotonation to form the ene-hydrazine tautomer, whereas in weakly acidic media the tautomerization is so rapid that [3,3]-rearrangement becomes rate limiting. At an intermediate acidity, the deprotonation is rate determining, with the rate being strongly dependent on the concentration of the anionic counter ion.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610071106
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  • 146
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    Kinetics and mechanism of aminolysis of propargyl and 1-methyl-propargyl arenesulphonates (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 629-633 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Kinetic studies were carried out on the aminolysis of propargly and 1-methylpropargyl arenesulphonates in acetonitrile at 45·0°C. The cross-interaction constants, ρxz and βxz, are similar to, but smaller than, those for the SN2 processes at other primary and secondary carbon centers. Compared with the allyl series, the smaller magnitude of ρxz and βxz reflects a looser transition state, which in turn leads to a lower rate despite the greater Taft's σ* value and the lower intrinsic (ΔE0≠) and thermodynamic barriers (ΔE0).
    Additional Material: 7 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610071107
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  • 147
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    The meta versus para substituent effect in the gas phase: Separation of inductive and resonance components (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 615-624 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Substitutent effects of acceptor groups were measured for the gas-phase basicities of some substituted benzonitriles, methyl benzoates and acetophenones, and for gas-phase acidities of some substituted benzoic acids. Substitutents considered were NO2, CN, SO2CH3, SO2F, CF3, CH2Cl, COCH3 and COOCH3, always in the meta and para positions. By combination with the literature data, a general conclusion is drawn that the substituent effects are proportional in the two positions and almost equal (the para:meta ratio is 1·06). No sign of any resonance effect was detected within the accuracy of the approach. The substituent effects in solution were recalculated statistically and the result was similar with a higher ratio, 1·09-1·19. It follows that the conjugation of acceptor groups, particularly of NO2 as a typical example, has been overestimated by current theories when compared with the much stronger conjugation of typical donors. Moreover, the inductive effect is propagated more effectively from the para than from the meta position. Many correlations in the literature, neglecting this situation, have been in fact controlled by the more complex, and more striking, behaviour of donors, which has obscured the simpler and more monotonous effect of acceptors, usually less represented in the sample.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610071105
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  • 148
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    An E ⇌ Z isomerization of an electrophilic vinyl azide by 15N3-. A probe for internal rotation processes in the carbanionic intermediate of nucleophilic vinylic substitutionDedicated to Professor G. Modena on the occasion of his 70th birthday. (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 652-654 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The label incorporation and Z → E isomerization in the reaction of 3-azidomethylenedihydro-(3H)-furan-2-one with Na15NN2 in 1:1 water-acetone were measured as a probe for internal clockwise vs anticlockwise rotation in the intermediate carbanion.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610071111
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  • 149
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    Similarity in physical organic chemistry: Substituent effects on the intrinsic basicity of 4-substituted pyrazoles (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 657-662 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The gas-phase basicities of eight pyrazoles substituted only at position 4 (R4 = H, NO2, F, Cl, CO2C2H5, CH3, NH2, 1-adamantyl) were measured by Fourier transform ion cyclotron resonance. The experimental values were treated in two ways, first by comparing these values with the AM1-calculated proton affinities. Since the correlation was reasonably good [PA(calc.) = -11·3 + 1·063PA(exp.), n = 8, r = 0·984], a set of 17 further 4-substituted pyrazoles and their cations were calculated using the AM1 approximation and their gas-phase basicities were estimated. Second, both the experimental and the AM1-calculated values were considered within the framework of the Taft-Topsom analysis of substituent effects. Comparison of the analyses for pyrazoles and pyridines led to the unexpected result that, in spite of differences in ring size and number of heteroatoms, both systems behave remarkably alike.
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610071203
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  • 150
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    Stabilities of some 2-(para-substituted-phenyl)-4,4,5,5-tetramethyl-1,3-dioxolanes relative to their conjugate dioxolenium ions, radicals and carbanions as determined by thermodynamics for hydride and electron transfer in solution (1994)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 7 (1994), S. 663-671 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A calorimetric method is described for the determination of the hydride affinities, ΔHH-(R+) of seven dioxolenium ions from the title compounds and also tropylium, trityl and 9-phenyl xanthylium cations by hydride transfer to the carbocations from BH3CN-. Cyclic voltammetric methods yield free energies for reduction of the cations to the conjugate radicals and to the carbanions. The ΔHH-(R+) values correlate well with the first reduction potentials of the cations.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610071204
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  • 151
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    Darstellung und Struktur von Tetraethylcyclotetraarsoxan-Komplexen von Kupfer(I)-Halogeniden (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 334-342 
    Details
    ISSN: 0044-2313
    Keywords: Copper(I) halide complexes ; tetraethylcyclotetraarsoxane copper(I) complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of Tetraethylcyclotetraarsoxane Complexes of Copper(I) HalidesThe polymeric complexes [Cu4Cl4{cyclo-(C2H5AsO)4}3]n (1), [Cu3Br3{cyclo-(C2H5AsO)4}2]n (2) and [Cu6I6{cyclo-(C2H5AsO)4}3]n (3) were prepared by the reaction of (C2H5AsO)n and CuX (X = Cl, Br, I) in acetonitrile and characterised by X-ray analysis. All three complexes contain only tetramers (C2H5AsO)4 as ligands, in which the As4O4 ring systems coordinate between two and four Cu-atoms. In each case one As4O4 ring with a crown-shaped conformation is observed, which coordinates either four (in 1) or three (in 2 and 3) axially sited Cu-atoms. In addition there are further (C2H5AsO)4 ligands, which display either a boat-chair- (in 1) or a twist-chair-conformation (in 1-3). The individual building units are connected to one another via Cu—X—Cu bridges (in 2 and 3) and/or centrosymmetric As4O4 ring systems (in 1-3) into chain (1) or layer structures (2 und 3).
    Notes: Die polymeren Komplexe [Cu4Cl4{cyclo-(C2H5AsO)4}3]n (1), [Cu3Br3{cyclo-(C2H5AsO)4}2]n (2) und [Cu6I6{cyclo-(C2H5AsO)4}3]n (3) wurden durch die Umsetzung von (C2H5AsO)n und CuX (X = Cl, Br, I) in Acetonitril dargestellt und durch Röntgenstrukturanalyse charakterisiert. Alle drei Komplexe enthalten lediglich Tetramere (C2H5AsO)4 als Liganden, wobei die As4O4-Ringsysteme zwischen zwei und vier Cu-Atomen koordinieren. Es wird jeweils ein As4O4-Ring mit Kronenkonformation beobachtet, der entweder vier (in 1) oder drei (in 2 und 3) Cu-Atome axial koordiniert. Außerdem liegen weitere (C2H5AsO)4-Liganden in boat-chair- (in 1) oder twist-chair-Konformation (in 1-3) vor. Die einzelnen Baueinheiten werden über Cu—X—Cu-Brücken (in 2 und 3) und/oder zentrosymmetrische As4O4-Ringsysteme (in 1-3) zu Ketten-(1) oder Schichtstrukturen (2 und 3) verknüpft.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200222
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  • 152
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    Über die Reaktion von Cp2TiCl2 mit [C(NMe2)3][(CO)4FeC(O)NMe2] - Kristallstruktur von [C(NMe2)3]2[FeCl4] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 343-345 
    Details
    ISSN: 0044-2313
    Keywords: Hexamethyl guanidinium cation ; tetrachloro iron(II) anion ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Concerning the Reaction of Cp2TiCl2 with [C(NMe2)3][(CO)4FeC(O)NMe2] - Crystal Structure of [C(NMe2)3]2[FeCl4]The title compound forms by the reaction of Cp2TiCl2 with [C(NMe2)3][(CO)4FeC(O)NMe2] in THF solution. It crystallizes in the space group Pbcn with a = 1 566.6(3); b = 976.4(2); c = 1 580.4(4) pm; Z = 4; R = 3.8%. Each [FeCl4]2- in is surrounded by eight cations. Two cations each are connected with one Cl atom by relatively short H … Cl contacts leading to a distortion of the tetrahedral geometry of the anion.
    Notes: Die Titelverbindung entsteht bei der Umsetzung von Cp2TiCl2 mit [C(NMe2)3][(CO)4FeC(O)NMe2] in THF-Lösung. Sie kristallisiert in der Raumgruppe Pbcn mit a = 1 566,6(3); b = 976,4(2); c = 1 580,4(4) pm; Z = 4; R = 3,8%. Jedes [FeCl4]2- Ion ist von acht Kationen umgeben. Je zwei Kationen sind über relativ kurze H … Cl Kontakte mit einem Cl-Atom verbunden, was zu einer Verzerrung der Tetraedergeometrie des Anions führt.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200223
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  • 153
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    Preparation and x-ray structure of 1,4,2,3,5,6-Dithiatetrazine (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 495-497 
    Details
    ISSN: 0044-2313
    Keywords: Dithiatetrazine ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Röntgenstrukturanalyse von 1,4,2,3,5,6-DithiatetrazinDie Umsetzung von Schwefeldichlorid mit sym-EtO2CNHNHCO2Et 1 ergibt S2[N(CO2Et)]4 2, das analytisch, durch NMR und röntgenographisch charakterisiert wird. Die Strukturanalyse von 2 zeigt, daß der S2N4-Ring Sessel-Konformation hat mit allen vier Estergruppen in pseudoaxialen Positionen. Die Bindungslängen und -winkel werden mit denen in 1 und S4(NR)2 verglichen.
    Notes: Reaction of sulfur dichloride with sym-EtO2CNHNHCO2Et 1 gives the title ring system which has been characterised by microanalyses, nmr, and X-Ray crystallography. The X-ray structure of S2[N(CO2Et)]4 2 reveals that the S2N4 ring adopts a chair conformation with all four ester groups in pseudo-axial positions. Bond lengths and angles are compared with 1 and S4(NR)2.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200316
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  • 154
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    o-1λ5,3λ5-Diphosphaphenylen-bis(diphenylphosphan) und seine chelatbildenden Eigenschaften (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 483-488 
    Details
    ISSN: 0044-2313
    Keywords: o-1λ5,3λ5-Diphosphaphenylene-bis(diphenylphosphane) ; nickel(II) chloride chelate complex ; crystal structure ; NMR, Ir spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: o-1λ5,3λ5-Diphosphaphenylene-bis(diphenylphosphane) and its Chelating PropertiesBis(diphenylphosphanyl)acetylene and 1,1′,3,3′-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete react at higher temperatures to yield the title compound 5, which forms easily the chelate complex 6 with nickel(II) chloride.
    Notes: Bis(diphenylphosphanyl)acetylen und 1,1′,3,3′-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet reagieren bei höheren Temperaturen zur Titelverbindung 5, die mit Nickel(II)-chlorid leicht den Chelatkomplex 6 bildet.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200314
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  • 155
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    Pb3Al2F12: Crystal structure of a cyclo-fluoroaluminate related to Ba3Al2F12 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1449-1454 
    Details
    ISSN: 0044-2313
    Keywords: Lead fluoroaluminate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Pb3Al2F12: Kristallstruktur eines mit zu Ba3Al2F12 verwandten cyclo-FluoroaluminatDas Fluoroaluminat Pb3Al2F12 wurde in Form von Einkristallen durch Hydrothermal-Synthese erhalten und kristallisiert monoklin in P 21/n mit a = 9,435(6) Å, b = 9,610(5) Å, c = 10,100(9) Å, β = 90,59(5)°, V = 915,7(2) Å3, Z = 4, MoKα, λ = 0,71073 Å, R = 0,0463, Rw = 0,0465, 3 044 symmetrieunabhängige gemessene Reflexe. Die Struktur zeigt tetramere, isolierte, von einem Unternetzwerk unabhängiger Fluoridpolyeder eingeschlossene Oktaeder und ist mit Ba3Al2F12 verwandt. Existenz und Struktur der A3M2F12-Verbindungen werden diskutiert.
    Notes: Pb3Al2F12 is a fluorometalate obtained in single-crystal form by hydrothermal synthesis. It crystallizes in the monoclinic system, space group P 21/n, with a = 9.435(6) Å, b = 9.610(5) Å, c = 10.100(9) Å, β = 90.59(5)°, V = 915.7(2) Å3, Z = 4. The structure was solved from single crystal using 3 044 unique reflections (MoKα, λ = 0.71073 Å), R = 0.0463, Rw = 0.0465. The structure exhibits isolated tetrameric groups of octahedra encaged in a subnetwork of independent fluoride polyhedra and is related to that of Ba3Al2F12. A discussion about the existence and the structure of A3M2F12 compounds is given.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200822
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    Ein Beitrag über Ba3Pt4HgO11: Das erste Erdkalimetall-Oxoplatinat(II,V)/Oxomercurat (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1471-1475 
    Details
    ISSN: 0044-2313
    Keywords: Barium, mercury, platinum, oxide ; crystal structure ; high pressure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Contribution on Ba3Pt4HgO11: The First Alkaline-Earth Oxoplatinate(II,V)/OxomercurateSingle crystals of Ba3Pt4HgO11 were prepared by oxygen high pressure technique (4 200-3 600 bar) and investigated by X-ray methods. It crystallizes with hexagonal symmetry, space group D3h4—P62c, a = 6.021, c = 17.374 Å, Z = 2. Ba3Pt4HgO11 represents a new structure type, showing structural relationships to Ba2Hg3Pd7O14 and to the precious metal 6L-perovskites. The Hg2+ ions show dumb-bell like coordination, Pt2+ a square-planar surrounding and Pt5+ face shared double octahedra.
    Notes: Ba3Pt4HgO11 wurde unter hohem Sauerstoffdruck (4 200-3 600 bar) einkristallin dargestllt und röntgenographisch untersucht. Die Verbindung kristallisiert hexagonal, Raumgruppe D3h4—P62c mit a = 6,021; c = 17,374 Å; Z = 2. Ba3Pt4HgO11 bildet einen neuen Strukturtyp, der kristallchemische Verwandtschaft zu Ba2Hg3Pd7O14 und den Edelmetall-6L-Perowskiten zeigt. Die Hg2+-Ionen weisen eine hantelförmige, Pt2+ eine quadratisch-planare Koordination auf. Pt5+ bildet mit O2- flächenverknüpfte Doppeloktaeder.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200825
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  • 157
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    Die Kristallstruktur von Tris(N,N-diethyl-N′-benzoylselenoureato)cobalt(III) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1479-1482 
    Details
    ISSN: 0044-2313
    Keywords: Tris(N,N-diethyl-N′-benzoylselenoureato)cobalt(III) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Tris(N,N-diethyl-N′-benzoylselenoureato)cobalt(III)Co(C12H15N2OSe)3 crystallizes in the trigonal space group P3. The cell parameters are a = 16.697(4), c = 8.557(8) Å, Z = 2. The structure was solved with Patterson and direct methods and was refined to a final R-value of 4.59%. CoIII is bidentally coordinated to three N,N-diethyl-N′-benzoylselenourea molecules to form a distorted octahedron with facial arrangement of the selenium and oxygen donor atoms. The Co—Se and Co—O bond lengths are 2.328(2) and 1.943(6) Å, respectively. The arrangement of the molecules within the unit cell leads to the formation of hexagonal channels parallel to the crystallographic c-axis. The wall of the channels is formed by carbon atoms of the phenyl group. The diameter of the channels is 8.148 Å.
    Notes: Co(C12H15N2OSe)3 kristallisiert in der trigonalen Raumgruppe P3 mit den Gitterkonstanten a = 16,697(4), c = 8,557(8) Å, Z = 2. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 4,59% verfeinert. CoIII bildet mit dem Liganden N,N-Diethyl-N′-benzoylselenoharnstoff einen oktaedrisch koordinierten Neutralkomplex, in dem drei Ligandmoleküle in facialer Anordnung bidental über Selen- und Sauerstoffatome an das Zentralatom gebunden sind. Der Co—Se-Abstand beträgt 2,328(2) Å, der Co—O-Abstand 1,943(6) Å. Die Anordnung der Komplexmoleküle in der Elementarzelle führt zur Ausbildung von hexagonalen Kanälen parallel zur kristallographischen c-Achse. Die Kanalwände werden von Kohlenstoffatomen der Phenylreste gebildet; der Durchmesser der Kanäle beträgt 8,148 Å.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200827
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    Hydrate schwacher und starker Basen. XI. Die Kristallstrukturen von NaOH · 3,5H2O und NaOH · 7 H2O. Eine PräzisierungProfessor Horst Sabrowsky zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1509-1513 
    Details
    ISSN: 0044-2313
    Keywords: Sodium hydroxide hydrates ; crystal structure ; hydrogen bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrates of Weak and Strong Bases. XI. The Crystal Structures of NaOH · 3,5H2O and NaOH · 7 H2O. A RefinementThe crystal structures of the hydrates NaOH · 3,5 H2O (space group P21/c, Z = 8 formula units per unit cell; lattice parameters: a = 6.481, b = 12.460, c = 11.681 Å, β = 104.12° at -100°C) and NaOH · 7 H2O (P21/c, Z = 4; a = 7.344, b = 16.356, c = 6.897 Å, β = 92.91° at -150°C) have been redetermined using MoKα diffractometer data. The obtained refinement of the structures, including the localization also of the H atoms for the first time, has led to new findings with respect to the H bonds. In particular, in both hydrates there is one such interaction of the rare type OH- … OH2, from an OH- ion to an H2O molecule, i. e. with the OH- ion as the proton donor.
    Notes: Die Kristallstrukturen der Hydrate NaOH · 3,5H2O (Raumgruppe P21/c, Z = 8 Formeleinheiten pro Elementarzelle; Gitterkonstanten a = 6,481, b = 12,460, c = 11,681 Å, β = 104,12° bei -100°C) und NaOH · 7 H2O (P21/c, Z = 4; a = 7,344, b = 16,356, c = 6,897 Å, β = 92,91° bei -150°C) wurden mit MoKα-Diffraktometerdaten einer Zweitbestimmung unterzogen. Die erreichte Präzisierung der Strukturen, einschließlich der erstmaligen Lokalisierung auch der H-Atome, führte zu neuen Erkenntnissen bezüglich der H-Brücken. Insbesondere gibt es in beiden Hydraten eine solche Wechselwirkung vom seltenen Typ OH- · OH2, von einem OH--Ion zu einem H2O-Molekül, also mit dem OH--Ion als Protondonor.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200903
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  • 159
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    Neue Silicate mit „Stuffed Pyrgoms“: CsKNaLi9{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4, RbNa3Li8{Li[SiO4]}4 [1] und RbNaLi4{Li[SiO4]}2 [2]Professor Horst Sabrowsky zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1495-1508 
    Details
    ISSN: 0044-2313
    Keywords: New Lithosilicates ; preparation ; crystal structure ; MAPLE and CHARDI calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: More Silicates with „Stuffed Pyrgoms“: CsKNaLi9{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4, RbNa3Li8{Li[SiO4]}4 [1] and RbNaLi4{Li[SiO4]}2 [2]Single crystals of the new silicates CsKNaLi9{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4, RbNa3Li8{Li[SiO4]}4 and RbNaLi4{Li[SiO4]}2 as well as powder (Rb-containing compounds only) were obtained for the first time. The samples were prepared by heating well ground mixtures of the binary oxides in Ni and Ag tubes, respectively. The structure determination was carried out by four-circle diffractometer data (MoKα radiation; Siemens AED 2):CsKNaLi9{Li[SiO4]}4: tetragonally prismatic crystals, light yellow; 726 I0(hkl), R = 4.4%, Rw = 2.8%; a = 1 102.0(6), c = 637.9(5) pm; Z = 2; space group I4/m; 2 CsO0.55 + Li4TlO4 + glas (560°C, 15 d).CsKNa2Li8{Li[SiO4]}4: tetragonally prismatic crystals, light yellow; 727 I0(hkl), R = 4.4%, Rw = 2.6%; a = 1 103.5(7), c = 637.7(4) pm; Z = 2; space group I4/m; 1.1 CsO0.61 + 1.1 KO0.55 + 1.4 NaO0.52 + 6.5 Li2O + 4 SiO2 (600°C, 60 d).RbNa3Li8{Li[SiO4]}4: tetragonally prismatic crystals, colourless; 600 I0(hkl), R = 2.3%, Rw = 2.0%; a = 1 092.08(6), c = 632.76(4) pm; Z = 2; space group I4/m; 4 RbO0.57 + 3 NaO0.52 + 6.5 Li2O + 4 SiO2 (650°C, 63 d).RbNaLi4{Li[SiO4]}2: monoclinic, ball-shaped, colourless; 1 224 I0(hkl), R = 3.1%, Rw = 3.1%; a = 1 573.10(13), b = 630.48(5), c = 781.25(8) pm, b = 90.566(8)°; Z = 4; space group C2/m; 1.1 RbO0.52 + 1.2 NaO0.45 + 5 Li2O + 4 SiO2 (700°C, 40 d).
    Notes: Einkristalle der neuen Silicate CsKNaLi9{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4, RbNa3Li8{Li[SiO4]}4 und RbNaLi4{Li[SiO4]}2, sowie Pulver der Rb-haltigen Verbindungen wurden dargstellt. Die Proben entstanden durch Tempern inniger Gemenge binärer Oxide in geschlossenen Ni- bzw. Ag-Bömbchen. Die Strukturaufklärung erfolgte jeweils durch Vierkreisdiffraktometerdaten (MoKα-Strahlung; Siemens AED 2):CsKNaLi9{Li[SiO4]}4: tetragonale Prismen, hellgelb; 726 I0(hkl), R = 4,4%, Rw = 2,8%; a = 1 102,0(6), c = 637,9(5) pm; Z = 2; Raumgruppe I4/m; 2 CsO0,55 + LiTlO4 + Duran-Glas (560°C, 15 d).CsKNa2Li8{Li[SiO4]}4: tetragonale Prismen, hellgelb; 727 I0(hkl), R = 4,4%, Rw = 2,6%; a = 1 103,5(7), c = 637,7(4) pm; Z = 2; Raumgruppe I4/m; 1,1 CsO0,61 + 1,1 KO0,55 + 1,4 NaO0,52 + 6,5 Li2O + 4 SiO2 (600°C, 60 d).RbNa3Li8{Li[SiO4]}4: tetragonale Prismen, farblos; 600 I0(hkl), R = 2,3%, Rw = 2,0%; a = 1 092,08(6), c = 632,76(4) pm; Z = 2; Raumgruppe I4/m; 4 RbO0,57 + 3 NaO0,52 + 6,5 Li2O + 4 SiO2 (650°C, 63 d).RbNaLi4{Li[SiO4]}2: monoklin, kugelförmig, farblos; 1 224 I0(hkl), R = 3,1%, Rw = 3,1%; a = 1 573,10(13), b = 630,48(5), c = 781,25(8) pm, b = 90,566(8)°; Z = 4; Raumgruppe C2/m; 1,1 RbO0,52 + 1,2 NaO0,45 + 5 Li2O + 4 SiO2 (700°C, 40 d)
    Additional Material: 17 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200902
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  • 160
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    Cs[Er10(C2)2]I18 und [Er10(C2)2]Br18: zwei neue Beispiele für „reduzierte“ Halogenide der Lanthanide mit isolierten [M10(C2)2]-Clustern (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1532-1536 
    Details
    ISSN: 0044-2313
    Keywords: Erbium Clusters, [Er10(C2)2] ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cs[Er10(C2)2]I18 and [Er10(C2)2]Br18: Two New Examples for Reduced Halides of the Lanthanides with Isolated [M10(C2)2] ClustersCs[Er10(C2)2]I18 is obtained from the reaction of ErI3 with caesium and carbon in sealed tantalum containers at 700°C and [Er10(C2)2]Br18 through the metallothermic reduction of ErBr3 with rubidium in the presence of carbon at 750°C in sealed niobium containers. The crystal structures {Cs[Er10(C2)2]I18: triclinic, P1; a = 1 105.2(8) pm, b = 1 112.0(7) pm; c = 1 122.9(8) pm; α = 66.91(3)°, β = 87.14(3)°; γ = 60.80(3)°; Z = 1; R = 0.049, Rw = 0.043; [Er10(C2)2]Br18: monoclinic, P21/n, a = 971.8(6) pm, b = 1 623.4(9) pm, c = 1 163.8(6) pm, β = 104.00(6)°; Z = 2; R = 0.077, Rw = 0.057} contain isolated dimeric [Er10(C2)2] clusters. Due to the inclusion of C2 units, the octahedra are elongated in the direction of the pseudo C4 axis. The connecting edges of the two octahedra are exceptionally short (316.7 pm and 314.8 pm respectively). The dimeric units are connected via Xi-a and Xa-i (X = Br, I) bridges according to [Er10(C2)2X10iX8/2i-a]X8/2a-i. Cs+ is surrounded by a cuboctahedron of iodide ions in Cs[Er10(C2)2]I18.
    Notes: Cs[Er10(C2)2]I18 entsteht bei der Umsetzung von Erl3 mit Caesium und Kohlenstoff in verschweißten Tantalampullen bei 700°C, [Er10(C2)2]Br18 bei der metallothermischen Reduktion von ErBr3 mit Rubidium in Gegenwart von Kohlenstoff bei 750°C in verschweißten Niobampullen. Die Kristallstrukturen {Cs[Er10(C2)2]I18: triklin, P1; a = 1 105,2(8) pm; b = 1 112,0(7) pm; c = 1 122,9(7) pm; α = 66,91(3)°; β = 87,14(3)°; γ = 60,80(3)°; Z = 1; R = 0,049, Rw = 0,043; [Er10(C2)2]Br18: monoklin, P21/n; a = 971,8(6); b = 1 623,4(9); c = 1 163,8(6); β = 104,00(6)°; Z = 2; R = 0,077, Rw = 0,057} beinhalten isolierte dimere [Er10(C2)2]-Cluster. Wegen des Einbaus der C2-Hantel sind die Oktaeder entlang ihrer pseudovierzähligen Achse gestreckt. Die verknüpfenden Oktaederkanten weisen einen besonders kurzen Metall-Metall-Abstand auf (316,7 bzw. 314,8 pm). Die dimeren Einheiten sind über Xi-a bzw. Xa-i-Brücken (X = Br, I) miteinander verknüpft, gemäß [Er10(C2)2X10iX8/2i-a]X8/2a-i. Cs+ ist in Cs[Er10(C2)2]I18 kuboktaederisch von Iodidionen umgeben.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200907
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  • 161
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    Zur Oxydation intermetallischer Phasen: Die Oxoplumbate(II) K6[Pb2O5] [1] und K4[PbO3] [2] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1549-1558 
    Details
    ISSN: 0044-2313
    Keywords: Potassium plumbates ; preparation ; crystal structure ; MAPLE and CHARDI calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Oxidation of Intermetallic Phases: The Oxoplumbates(II) K6[Pb2O5] [1] and K4[PbO3] [2]Very pale yellow crystals of K6[Pb2O5] were obtained by heating a wellground mixture of LiPb und K2O2 (K2O2: LiPb = 2.5:1) in Ag-tubes (550°C; 40 d). The crystal structure, triclinic, space group P1, a = 1 326.7(6); b = 758.8(4); c = 637.0(3) pm; α = 92.17(3)°; β = 94.41(3)°; γ = 112.85(4)°; Z = 2 was determined (four-circle diffractometer data, Mo—Kα-, 3 270 Io(hkl), R = 8.0%, Rw = 3.5%, parameters see text). The pale yellow crystals of K4[PbO3] were received by heating KPb and K2O2 (K2O2: KPb = 3.3:2) in Ni-tubes (450°C; 17 d). The crystal structure (orthorhombic, space group Pbca with a = 658.2(1); b = 1 131.8(4); c = 1 872.2(6) pm; Z = 8) was refined (four-circle diffractometer data, Mo—Kα-, 2 003 Io(hkl), R = 4.9%, Rw = 2.8%).The Madelung Part of Lattice Energy (MAPLE), Effective Coordination Numbers (ECoN), the Mean Fictive Ionic Radii (MEFIR) and the Charge Distribution (CHARDI) are being calculated for both oxides.
    Notes: Äußerst schwach hellgelbe Kristalle von K6[Pb2O5] entstanden beim Tempern inniger Gemenge von LiPb und K2O2 (K2O2: LiPb = 2,5:1) in Ag-Bömbchen (550°C; 40 d). Die Kristallstruktur, triklin, Raumgruppe P1 (I.T. No. 2), mit a = 1 326,7(6); b = 758,8(4); c = 637,0(3) pm; α = 92,17(3)°; β = 94,41(3)°; γ = 112,85(4)°; Z = 2 wurde aufgeklärt (Vierkreisdiffraktometerdaten, Mo—Kα-, 3 270 Io(hkl), R = 8,0%, Rw = 3,5%, Parameter siehe Text). Die blaß gelben Kristalle von K4[PbO3] entstanden beim Tempern von KPb mit K2O2 (K2O2: KPb = 3,3:2) in Ni-Bömbchen (450°C; 17 d). Die Kristallstruktur (orthorhombisch, Raumgruppe Pbca, a = 658,2(1); b = 1131,8(4); c = 1872,2(6) pm; Z = 8) wurde verfeinert (Vierkreisdiffraktometerdaten, Mo—Kα-, 2 003 Io(hkl), R = 4,9%, Rw = 2,8%).Für beide Oxide werden der Madelunganteil der Gitterenergie (MAPLE), Effektive Koordinationszahlen (ECoN), die Mittleren Fiktiven Ionenradien (MEFIR) sowie die Ladungsverteilung (CHARDI) berechnet.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200910
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  • 162
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    Ein weiteres Alkali-Erdalkalimetall-Oxoniccolat mit Perowskitstruktur: Sr12NaNi7O23 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1565-1568 
    Details
    ISSN: 0044-2313
    Keywords: Strontium, sodium, nickel, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Another Alkaline Alkaline-Earth Oxoniccolate of Perovskite Type Structure: Sr12NaNi7O23Single Crystals of Sr12NaNi7O23 were prepared in closed system by Na2O2 flux reaction. X-ray single crystal work show hexagonal symmetry, space group D32-P321, a = 9.429, c = 7.896 Å, Z = 1. Sr12NaNi7O23 is strongly related to the stackered perovskites containing consequently face shared Ni2O9 double octahedra and Na+ inside a trigonal prismatic coordination by oxygen. One underoccupied oxygen point position decreases the coordination number of one Ni3+ of the Ni2O9 groups and a second surrounded by trigonal prisms to corner connected Ni2O7 double tetrahedra. The crystal chemistry will be discussed with respect to compounds of the same structure.
    Notes: Einkristalle von Sr12NaNi7O23 wurden im geschlossenen System mit Na2O2 als Schmelzmittel dargestellt. Röntgenographische Untersuchungen zeigen hexagonale Symmetrie, Raumgruppe D32-P321; a = 9,429; c = 7,896 Å, Z = 1. Sr12NaNi7O23 ist eng mit den Stapelvarianten der Perowskite verwandt und zeigt flächenverknüpfte Ni2O9-Oktaederdoppel sowie Na+ in einer trigonal prismatischen Koordination von Sauerstoff. Eine unterbesetzte Sauerstofflage erniedrigt die Koordinationszahl von einem Ni3+-Ion in den Ni2O9-Gruppen und von einem weiteren in trigonal prismatischer Koordination. Es entstehen eckenverknüpfte Ni2O7- Doppeltetraeder. Die Kristallchemie wird mit Blick auf Verbindungen vom gleichen Strukturtyp diskutiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200912
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  • 163
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    Ein neues Kupferzinnboratoxid mit isolierten BO3-Baugruppen: Cu5Sn(BO3)2O4 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1578-1582 
    Details
    ISSN: 0044-2313
    Keywords: Copper, tin, borate, oxide ; synthesis ; crystal structure ; X-ray diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On a New Copper Tin Borate Oxide with Isolated BO3 Units: Cu5Sn(BO3)2O4Single Crystals of the new compound Cu5Sn(BO3)2O4 were obtained by a B2O3 fluxtechnique. They crystallize in a monoclinic distorted variant of a Ludwigite structure with a partly ordered metal distribution. X-ray investigations on single crystals led to the space group C2h5-P21/c (No. 14); a = 6.3526(7); b = 9.502(1); c = 12.100(9) Å; β = 93.30(3)°; Z = 4. All metal-sites are distorted octahedraly coordinated by oxygen-ions. The structure contains BO3-units and oxygen which is not coordinated to boron.
    Notes: Aus einer B2O3-Schmelze gelang die Synthese von Einkristallen der Substanz Cu5Sn(BO3)2O4, die in einer monoklin verzerrten Strukturvariante eines Ludwigites mit weitgehend geordneter Metallverteilung kristallisiert. Röntgenographische Untersuchungen an Einkristallen ergeben die Raumgruppe C2h5-P21/c (Nr. 14); a = 6,3526(7); b = 9,502(1); c = 12,100(9) Å; β = 93,30(3)°; Z = 4. Die Metallkationen sind verzerrt oktaedrisch von Sauerstoffionen koordiniert. Die Struktur weist sowohl isolierte, planare BO3-Baugruppen als auch nicht an Bor gebundenen Sauerstoff auf.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200914
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  • 164
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    Synthese und Kristallstrukturen von (PPh4)2[In(S4)(S6)Cl] und (PPh4)2[In(S4)Cl3] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1607-1612 
    Details
    ISSN: 0044-2313
    Keywords: Indium polysulfido complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of (PPh4)2[In(S4)(S6)Cl] and (PPh4)2[In(S4)Cl3]InCl and PPh4Cl yield (PPh4)2[In2Cl6] in acetonitrile. This reacts with Na2S4 in presence of PPh4Cl, forming (PPh4)2[In(S4)(S6)Cl]. Its crystal structure was determined by X-ray diffraction (R = 0.075, 2 282 observed reflexions). It is isotypic with (PPh4)2[In(S4)(S6)Br] and contains anions with trigonal-bipyramidal coordination of In, Cl occupying an axial position, and the S4 and S6 groups being bonded in a chelate manner. The reaction of (PPh4)2[In2Cl6] and sulfur in acetonitrile yielded (PPh4)2[InCl5] and (PPh4)2[In(S4)Cl3]. The crystal structure analysis of the latter (R = 0.072, 4 080 reflexions) revealed an anion with distorted trigonal-bipyramidal coordination of In, the S4 group occupying one axial and one equatorial position; the S4 group shows positional disorder.
    Notes: Aus InCl und PPh4Cl entsteht in Acetonitril (PPh4)2[In2Cl6]. Aus diesem wurde mit Na2S4 im Beisein von PPh4Cl (PPh4)2[In(S4)(S6)Cl] erhalten. Seine Kristallstruktur wurde mittels Röntgenbeugung bestimmt (R = 7,5%, 2 282 beobachtete Reflexe). Es kristallisiert isotyp zum (PPh4)2[In(S4)(S6)Br] und enthält Anionen mit trigonal-bipyramidaler Koordination des In; das Cl-Atom nimmt eine axiale Position ein und die S4- und S6-Gruppe ist jeweils chelatartig gebunden. Aus (PPh4)2[In2Cl6], PPh4Cl und Schwefel entstanden in Acetonitril (PPh4)2[InCl5] und (PPh4)2[In(S4)Cl3]. Nach der Kristallstruktur des letzteren (R = 7,2%, 4 080 Reflexe) ist im [In(S4)Cl3]2--Ion das In-Atom verzerrt trigonal-bipyramidal koordiniert, wobei die S4-Gruppe an eine axiale und eine equatoriale Position gebunden ist; die S4-Gruppe ist fehlgeordnet.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200919
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  • 165
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    Verfeinerung der Kristallstruktur von SrO2 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 879-881 
    Details
    ISSN: 0044-2313
    Keywords: Strontium peroxide ; crystal structure ; composition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Refinement of the Crystal Structure of SrO2Single crystals of SrO2 have been obtained after high pressure/high temperature reaction of a SrO/KClO3 mixture at 20 kbar, 1 400°C. The crystal structure was refined using 154 unique diffractometer data (I4/mmm; a = 3.5626(3), c = 6.6159(6) Å; Z = 2; R = 0.033, Rw = 0.022, S = 0.932). The O—O distance (1.493(4) Å) is significantly longer than the one previously assumed. From a refinement of the site occupation factor for oxygen a composition SrO1.95(2) has been found for the crystal investigated.
    Notes: Einkristalle von SrO2 wurden durch Hochdruck-Hochtemperatur-Reaktion eines SrO—KClO3-Gemisches bei 20 kbar, 1 400°C erhalten. Die Kristallstruktur wurde auf der Basis von Vierkreisdiffraktometerdaten (154 unabhängige Strukturfaktoren) verfeinert (I4/mmm; a = 3,5626(3), c = 6,6159(6) Å; Z = 2; R = 0,033, Rw = 0,022, S = 0,932). Der gefundene O—O-Abstand ist mit 1,493(4) Å deutlich größer als bisher angenommen. Eine Verfeinerung des Besetzungsfaktors von Sauerstoff ergab für den untersuchten Kristall eine Zusammensetzung SrO1,95(2).
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19946200521
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  • 166
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    Darstellung und Kristallstruktur von K6[Al2O6] und Rb6[Al2O6]Professor Heinz Dieter Lutz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 882-887 
    Details
    ISSN: 0044-2313
    Keywords: K6[Al2O6], Rb6[Al2O6] ; preparation ; crystal structure ; MAPLE ; CHARDI ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Crystal Structure of K6[Al2O6] and Rb6[Al2O6]Colourless single crystals of K6[Al2O6] have been prepared from intimate mixtures of KAlO2 and K2O (550°C, 90 d). The structure determination from four-circle diffractometer data (MoKα, 742 Io(hkl), R = 2.2%, Rw = 2.1%) confirms the space group C2/m with Z = 2; a = 698.25 pm, b = 1 103.54 pm, c = 646.49 pm, β = 102.49°.Colourless single crystals of hitherto unknown Rb6[Al2O6] have been prepared from intimate mixtures of RbAlO2 and Rb2O (520°C, 120 d). The structure determination from four-circle diffractometer data (MoKα, 1 240 Io(hkl)) results in the residual values R = 7.2%, Rw = 4.9%; space group C2/m; a = 725.92 pm, b = 1 143.33 pm, c = 678.06 pm, β = 104.05°; Z = 2.K6[Al2O6] and Rb6[Al2O6] are isostructural with K6[Fe2O6]. A characteristic structure unit is the anion [Al2O6]6- consisting of two edge-sharing [AlO4] tetrahedra.Effective Coordination Numbers (ECoN), Mean Fictive Ionic Radii (MEFIR), the Madelung Part of Lattice Energy (MAPLE) and the Charge Distribution (CHARDI) are calculated and discussed.
    Notes: Farblose Einkristalle von K6[Al2O6] wurden aus innigen Gemengen von KAlO2 und K2O erhalten (550°C, 90 d). Die Strukturaufklärung (Vierkreisdiffraktometer, MoKα, 742 Io(hkl), R = 2,2%, Rw = 2,1%) bestätigt die Raumgruppe C2/m mit Z = 2; a = 698,25 pm, b = 1 103,54 pm, c = 646,49 pm, β = 102,49°.Analog erhielten wir erstmals Rb6[Al2O6] aus RbAlO2 und Rb2O in Form farbloser Einkristalle (520°C, 120 d). Die Strukturaufklärung (Vierkreisdiffraktometer, MoKα, 1 240 Io(hkl)) ergab in C2/m die Residualwerte R = 7,2%, Rw = 4,9%; a = 725,92 pm, b = 1 143,33 pm, c = 678,06 pm, β = 104,05°.K6[Al2O6] und Rb6[Al2O6] sind mit K6[Fe2O6] isotyp; charakteristische Strukturelemente sind die Anionen [Al2O6]6-, die aus zwei kantenverknüpften [AlO4]-Tetraedern bestehen.Effektive Koordinationszahlen (ECoN), Mittlere Fiktive Ionenradien (MEFIR), der Madelunganteil der Gitterenergie (MAPLE) sowie die Ladungsverteilung (CHARDI) werden berechnet und diskutiert.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200522
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    Die Kristallstruktur von Bis(N,N-diethyl-N′ -benzoylselenoureato)nickel(II)Professor Hans Bock zum 65. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 177-182 
    Details
    ISSN: 0044-2313
    Keywords: Bis(N,N-diethyl-N′-benzoylselenoureato)nickel(II) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Bis(N,N-diethyl-N′ -benzoylselenoureato)nickel(II)Ni(C12H15N2OSe)2 crystallizes in the monoclinic space group P21/c. The cell parameters are a = 11.399(3), b = 16.016(4), c = 14.910(6) Å, β = 104.64(3)° and Z = 4. The structure was solved with Patterson and direct methods and was refined to a final R-value of 5.43%. Nickel is coordinated to two N,N-diethyl-N′ -benzoylselenourea molecules to form a bidentally coordinated chelate complex with cis arrangement of the donor atoms. Coordinaton around the nickel atom is planar while the chelate rings diverge from planarity. The ethyl groups of one diethylamino group are disordered. The Ni—Se bond lengths are 2.244(1) and 2.264(1) Å, the Ni—O bond lengths are 1.871(4) and 1.883(4) Å, respectively.
    Notes: Ni(C12H15N2OSe)2 kristallisiert in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 11,399(3), b = 16,016(4), c = 14,910(6) Å, β = 104,64(3)°, Z = 4. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 5,43% verfeinert. Nickel bildet mit dem Liganden N,N-Diethyl-N′-benzoylselenoharnstoff einen bidental koordinierten Chelatkomplex, in dem zwei Ligandmoleküle über Selen- und Sauerstoffatome in cis-Anordnung an das Zentralatom koordiniert sind. Die Koordinationssphäre um das Nickelatom ist planar, die Chelatringe weichen dagegen deutlich von der Planarität ab. Die Ethylgruppen einer Diethylaminogruppe sind fehlgeordnet. Die Ni—Se-Abstände betragen 2,244(1) und 2,264(1) Å, die Ni—O-Abstände 1,871(4) und 1,883(4) Å.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200129
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  • 168
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    CdHgO2: Ein Oxomercurat mit Verwandtschaft zur Crednerit-StrukturProfessor Wilhelm Preetz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1137-1141 
    Details
    ISSN: 0044-2313
    Keywords: Cadmium ; mercury ; oxide ; high pressure ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: CdHgO2: An Oxomercurate related to the Crednerite StructureSingle crystals of CdHgO2 were prepared by oxygen high pressure technique (600°C, 3900 bar) and investigated by X-ray technique. It crystallizes with monoclinic symmetry, space group C2h3-C2/m; a = 5.933, b = 3.452, c = 5.875 Å, β = 91.26°; Z = 2. The Hg2+ ions show dumb-bell like coordination, Cd2+ an octahedral one. CdHgO2 shows strong relationship to the Crednerite structure. The orientation of the O—Hg—O dump-bells to the CdO6 octahedra layers is discussed with respect to related oxomercurates.
    Notes: CdHgO2 wurde mit Sauerstoff-Hochdrucktechnik (600°C, 3900 bar) einkristallin dargestellt und röntgenographisch untersucht. Es kristallisiert monoklin, Raumgruppe C2h3-C2/m mit a = 5,933, b = 3,452, c = 5,875 Å, β = 91,26° und Z = 2. Die Hg2+-Ionen zeigen eine hantelförmige, Cd2+ eine oktaedrische Koordination. CdHgO2 zeigt große Ähnlichkeit zur Crednerit-Struktur. Die Anordnung der O—Hg—O-Hanteln zu den CdO6-Oktaederschichten wird unter Bezug auf verwandte Oxomercurate diskutiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200702
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  • 169
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    Cu3SbS3: Zur Kristallstruktur und PolymorphieProfessor Heinz Dieter Lutz zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1992-1997 
    Details
    ISSN: 0044-2313
    Keywords: Copper antimony sulfide ; sulfo salts ; crystal structure ; phase transitions ; Extended Hückel calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cu3SbS3: Crystal Structure and PolymorphismThe hitherto unknown crystal structure of β-Cu3SbS3 at room temperature could be determined from a twinned crystal. The compound crystallizes in the monoclinic system, space group P21/c (No. 14), with a = 7.808(1), b = 10.233(2) and c = 13.268(2) Å, β = 90.31(1)°, V = 1 060.1(2) Å3, Z = 8. An Extended-Hückel-Calculation shows weak bonding interactions between copper atoms which are coordinated trigonal planar. At -9°C a first order phase transition occurs and the crystals disintegrate. The low-temperature modification (γ) crystallizes in the orthorhombic system with a = 7.884(2), b = 10.219(2) and c = 6.623(2) Å, V = 533.6(2) Å3 (-100°C). At 121°C a phase transition of higher order is observed. The high-temperature polymorph (α) of Cu3SbS3 is orthorhombic again. From high-temperature precession photographs the space groups Pnma (No. 62) or Pna21 (No. 33) can be derived. The lattice constants at 200°C are a = 7.828(3), b = 10.276(4) and c = 6.604(3) Å, V = 531.2(2) Å3.
    Notes: Die bisher unbekannte Kristallstruktur von β-Cu3SbS3 bei Zimmertemperatur wurde anhand eines verzwillingten Kristalls ermittelt. Die Verbindung kristallisiert monoklin, RG P21/c (Nr. 14) mit a = 7,808(1), b = 10,233(2) und c = 13,268(2) Å, β = 90,31(1)°, V = 1 060,1(2) Å3, Z = 8. Eine Extended-Hückel-Rechnung ergibt schwach bindende Wechselwirkungen zwischen den trigonal-planar koordinierten Kupferatomen. Bei -9°C erfolgt eine reversible Phasenumwandlung 1. Ordnung, bei der die Kristalle zerfallen. Die Tieftemperaturmodifikation (γ) kristallisiert orthorhombisch mit a = 7,884(2), b = 10,219(2) und c = 6,623(2) Å, V = 533,6(2) Å3 (-100°C). Beim Aufheizen beobachtet man bei 121°C eine Phasenumwandlung höherer Ordnung. Die Hochtemperaturmodifikation (α) von Cu3SbS3 kristallisiert ebenfalls orthorhombisch. Aus Hochtemperatur-Präzessionsaufnahmen ergibt sich Pnma (Nr. 62) oder Pna21 (Nr. 33) als mögliche Raumgruppe. Die Gitterkonstanten bei 200°C sind nach Guinier-Aufnahmen a = 7,828(3), b = 10,276(4) und c = 6,604(3) Å, V = 531,2(2) Å3.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201126
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  • 170
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    Li10Si2PbIIO10 = Li20[(SiO4)4(OPbO2PbO)]  -  Das erste „gemischte“ Silicat-Plumbat(II)Professor Kurt Issleib in memoriam (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2026-2032 
    Details
    ISSN: 0044-2313
    Keywords: Lithium silicate plumbate ; preparation ; crystal structure ; MAPLE and CHARDI calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li10Si2PbIIO10 = Li20[(SiO4)4(OPbO2PbO)]  -  The first „mixed“ Silicate-Plumbate(II)Colourless crystals of Li10Si2PbO10 were obtained by heating a well-ground mixture of LiPb, Li2O2 and „SiO2“ (deriving from Duran glas) in Ag-tubes (650°C; 60 d). The crystal structure was determined (four-circle diffractometer data, Mo—Kα-, 1 474 Io(hkl), R = 4.2%, Rw = 2.8%, parameters see text). The silicate-plumbate crystallizes monoclinic (space group C2/m; I. T. No. 12) with a = 2985.1(4); b = 610.6(6); c = 512.8(1) pm, β = 99.70(9)° (four-circle data), Z = 4.Further the Madelung Part of Lattice Energy (MAPLE), Effective Coordination Numbers (ECoN), the Mean Fictive Ionic Radii (MEFIR) and the Charge Distribution (CHARDI) are being calculated.
    Notes: Farblose Kristalle von Li10Si2PbO10 entstanden beim Tempern inniger Gemenge von LiPb, Li2O2 und „SiO2“ (aus Duranglas) in Ag-Bömbchen (650°C; 60 d). Die Kristallstruktur wurde aufgeklärt (Vierkreisdiffraktometerdaten, Mo—Kα-, 1 474 Io(hkl), R = 4,2%, Rw = 2,8%, Parameter siehe Text). Das Silicat-Plumbat kristallisiert monoklin (Raumgruppe C2/m; I. T. No. 12) mit a = 2 985,1(4); b = 610,6(1); c = 512,8(1) pm; β = 99,70(9) (Vierkreisdaten), Z = 4.Ferner werden der Madelunganteil der Gitterenergie (MAPLE), Effektive Koordinationszahlen (ECoN), die Mittleren Fiktiven Ionenradien (MEFIR) sowie die Ladungsverteilung (CHARDI) berechnet.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946201203
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  • 171
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    Neue Rheniumkomplexe mit Trichalkogenido- und Tetrachalkogenido-Chelatliganden (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 299-303 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium complexes ; rhenium trichalcogenido, -tetrachalcogenido complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Rhenium Complexes Containing Trichalcogenido and Tetrachalcogenido Chelate LigandsThe reactions of Cp*ReCl4 with polychalcogenide salts such as Na2S4 or (NEt4)2Se6 lead initially to the violet trichalcogenido chelate complexes Cp*ReCl2(E3) (E = S (3a), Se (3b)) which, due to their functional chloro ligands, can be used as intermediates for further reactions. Upon hydrolysis in moist solvents or aminolysis with tert. butylamine 3a, b are converted into the tetrachalcogenido chelate complexes Cp*Re(O)(E4) (E = S (4a), Se (4b)) and Cp*Re(NtBu)(E4) (E = S (5a), Se (5b)), respectively. X-Ray structure analyses were carried out for the three mononuclear cyclo-oligoselenido compounds 3b-5b. It appears that the size of the Se2-n chelate ring (n = 3 or 4) essentially depends on steric factors within the coordination sphere of rhenium.
    Notes: Die Reaktionen von Cp*ReCl4 mit Polychalkogenid-Salzen wie Na2S4 oder (NEt4)2Se6 führen zunächst zu den violetten Trichalkogenido-Chelatkomplexen Cp*ReCl2(E3) (E = S (3a), Se (3a), die aufgrund der funktionellen Chloroliganden als Zwischenstufen bei weiteren Reaktionen verwendet werden können. Bei Hydrolyse in feuchten Solvenzien oder Aminolyse mit tert. Butylamin werden 3a, b in die Tetrachalkogenido-Chelatkomplexe Cp*Re(O)(E4) (E = S (4a), Se (4b) bzw. Cp*Re(NtBu)(E4) (E = S (5a), Se (5b) umgewandelt. Für die drei einkernigen cyclo-Oligoselenido-Verbindungen 3b-5b wurden Röntgenstrukturanalysen durchgeführt. Es scheint, daß die Größe des Se2-n-Chelatrings (n = 3 oder 4) im wesentlichen von sterischen Faktoren innerhalb der Koordinationssphäre des Rheniums abhängt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200214
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  • 172
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    Crystal Structure of a New Acentric Oxide Fluoride of VIV: BaVOF4 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 309-312 
    Details
    ISSN: 0044-2313
    Keywords: Barium vanadium oxide fluoride ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristallstruktur eines neuen azentrischen Oxidfluorids des VIV: BaVOF4Die Struktur von BaVOF4, erhalten durch hydrothermale Synthese, wurde röntgendiffraktometrisch aus Einkristalldaten bestimmt: Raumgruppe Fdd2 (azentrisch), Z = 16, a = 7,920(1), b = 27,608(2), c = 7,375(1) Å mit R = 0,0262, Rw = 0,0273 für 1 508 unabhängige Reflexe und 64 Parameter. Das Gitter wird von cis-verknüpften VOF5-Oktaedern aus gewinkelten unendlichen Ketten entlang [101] und [101] gebildet, die über Barium-Kationen verbunden sind. Die Lage der O2- und F- wird mittels Valenzband-Rechnungen diskutiert. Wie für BaTiOF4 und einige Verbindungen aus der Reihe AIIMIIIF5 (A = Ba, Sr und M = Ga, Al, Mn) kann die Struktur durch quasi-hexagonal dichteste Ebenen aus Stapeln von Ba2+, O2-- und F--Ionen beschrieben werden.
    Notes: The structure of BaVOF4 has been determined by X-ray diffraction data from a single crystal obtained by hydrothermal synthesis: S.G. Fdd2 (acentric), Z = 16, a = 7.920(1), b = 27.608(2) and c = 7.375(1) Å with R = 0.0262 and Rw = 0.0273 for 1 508 independent reflections and 64 parameters. The network is built up from cis-linked VOF5 octahedra forming infinite kinked chains running along the [101] and [101] directions, connected by barium cations. The location of O2- and F- ions is discussed using bond valence calculations. As for BaTiOF4 and some compounds in the series AIIMIIIF5 (A = Ba, Sr and M = Ga, Al, Mn), the structure can be described in terms of a quasi hexagonal compact planes stacking of Ba2+, O2- and F- ions.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200216
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  • 173
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    Synthese und Kristallstruktur von Ba25Cu142+Cu43+Zn4O49 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 313-318 
    Details
    ISSN: 0044-2313
    Keywords: Barium, copper, zinc, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Ba25Cu142+Cu43+Zn4O49Single crystals of Ba25Cu142+Cu43+Zn4O49 were prepared with solid state and flux reactions. X-ray investigations show tetragonal symmetry, space group D74th-P4/nmm, a = 18.2146, c = 9.3230 Å, Z = 2. The hitherto unknown structure type shows copper in square pyramids and planar polygones, connected to six member rings or Cu5O20 groups. Slightly bent Cu5O12 groups produced by edge connection of five CuO4 polygones are connected with ZnO4 tetrahedra forming Cu5Zn4O20 units. The complicated structure is shown step by step.
    Notes: Einkristalle von Ba25Cu142+Cu43+Zn4O49 wurden mit einer Kombination von Feststoff- und Schmelzmittel-reaktionen dargestellt. Diese Substanz kristallisiert tetragonal, Raumgruppe D74th-P4/nmm mit a = 18,2146, c = 9,3230 Å, Z = 2. Der bisher unbekannte Strukturtyp zeigt Kupfer in tetragonal pyramidaler und planarer Koordination. Diese Polygone sind zu Sechsringen oder Cu5O20-Baugruppen verknüpft. Schwach gebogene Cu5O12-Baugruppen, die durch Kantenverknüpfung von fünf planaren CuO4-Polygonen gebildet werden, sind mit ZnO4-Tetraedern verknüpft und bilden Cu5Zn4O20-Baueinheiten aus. Die komplizierte Kristallstruktur wird schrittweise aufgebaut.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200217
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  • 174
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    Ein Beitrag über ein cobaltreiches Oxoarsenat/-vanadat: Co5AsVO10 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 319-322 
    Details
    ISSN: 0044-2313
    Keywords: Cobalt, arsenic, nickel, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Contribution about a New Cobalt-rich Oxoarsenate/-vanadate: Co5AsVO10Single crystals of Co5AsVO10 were prepared by solid state reactions and investigated by X-ray structure determination. It crystallizes with monoclinic symmetry, space group C2h3-C2/m, a = 19.134, b = 6.095, c = 17.482 Å, β = 133.37°; Z = 8. The new structure type is characterized by layers of CoO6- and AsO6-octahedra with partly alternating occupation. The layers are connected by Co2+ within tetrahedral oxygen coordination and tetrahedra around statistically occupied point positions of V5+ /As5+.
    Notes: Einkristalle von Co5AsVO10 wurden durch Feststoffreaktionen erhalten und röntgenographisch untersucht. Diese Verbindung kristallisiert mit monokliner Symmetrie, Raumgruppe C2h3-C2/m; a = 19,134; b = 6,095; c = 17,482 Å; β = 133,37°; Z = 8. Der neue Strukturtyp ist durch CoO6- und AsO6-Oktaederschichten ausgezeichnet, die teilweise alternierend mit Co2+ und As5+ besetzt sind. Die Oktaederschichten werden durch Co2+ in tetraedrischer Koordination und statistisch mit V5+ und As5+ besetzte Punktlagen verknüpft.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200218
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    On the Crystal Structure of LaCaCuGaO5 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 326-328 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanum calcium copper gallate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zur Kristallstruktur von LaCaCuGaO5Die Kristallstruktur von LaCaCuGaO5 wurde röntgenographisch an Einkristallen untersucht. Es kristallisiert orthorhombisch in der Raumgruppe C2v22-Ima2 mit a = 15,8467, b = 5,5077, c = 5,3188 Å, Z = 4. LaCaCuGaO5 gehört zum Brownmillerit-Typ und zeigt somit Schichten von eckenverknüpften CuO6-Oktaedern, die über GaO4-Tetraeder vernetzt sind. Die La3+- bzw. Ca2+-Ionen besetzen eine Punktlage statistisch.
    Notes: The crystal structure of LaCaCuGaO5 has been investigated by single crystal X-ray analysis. It crystallizes with orthorhombic symmetry, space group C2v22-Ima2, a = 15.8467, b = 5,5077, c = 5.3188 Å, Z = 4. LaCaCuGaO5 belongs to the mineral Brownmillerite showing layers of corner connected CuO6 octahedra linked by GaO4 tetrahedra. The La3+ and Ca2+ ions are distributed statistically over one crystallographic point position.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200220
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    Einkristall-Röntgenstrukturanalyse von Sr3TiGa10O20 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 323-325 
    Details
    ISSN: 0044-2313
    Keywords: Strontium, titanium, gallium, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Single Crystal X-Ray Analysis of Sr3TiGa10O20Single crystals of Sr3TiGa10O20 were prepared by recrystallisation of a molten oxide mixture and investigated by X-Ray technique. It crystallizes with monoclinic symmetry, space group C2h3-C2/m, a = 15.451, b = 11.579, c = 5.051 Å, β = 108.57°, Z = 2. Sr3TiGa10O20 belongs to the Pb3GeAl10O20 type, showing Ga3+ in tetrahedral and octahedral coordination. The octahedral coordinated point positions are occupied by Ga3+ and Ti4+ statistically.
    Notes: Einkristalle von Sr3TiGa10O20 wurden durch Rekristallisation aus Schmelzen erhalten und röntgenographisch untersucht. Diese Verbindung kristallisiert mit monokliner Symmetrie, Raumgruppe C2h3-C2/m, a = 15,451; b = 11,579; c = 5,051 Å; β = 108,57°; Z = 2. Sr3TiGa10O20 gehört zum Pb3GeAl10O20-Typ und zeigt Ga3+ in tetraedrischer und oktaedrischer Koordination. Die oktaedrisch koordinierten Punktlagen sind mit Ga3+ und Ti4+ statistisch besetzt.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200219
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    Zur Existenz des Tetrahydrogenorthoperiodations Die Kristallstruktur von LiH4IO6 · H2O (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 805-808 
    Details
    ISSN: 0044-2313
    Keywords: Lithiumtetrahydrogenorthoperiodate monohydrate ; crystal structure ; tetrahydrogenorthoperiodate Ion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Existence of the Tetrahydrogenorthoperiodate Ion. The Crystal Structure of LiH4IO6 · H2OThe crystal structure of LiH4IO6 · H2O has been determined (P1; a = 564.74(12), b = 574.41(13), c = 970.4(6) pm, α = 101.37(2), β = 96.37(2), γ = 114.72(2)°; Z = 2; 5 731 independent reflections; R = 0.038). All hydrogen-atoms were localized from difference fourier map and refined without applying constraints. Thus the existence of the tetrahydrogenorthoperiodate-ion in the solid state is proved, unambigously. The crystal structure is discussed and compared to other alkaliorthoperiodates.
    Notes: Die Kristallstruktur von LiH4IO6 · H2O wurde bestimmt (P1; a = 564,74(12), b = 574,41(13), c = 970,4(6) pm, α = 101,37(2), β = 96,37(2), γ = 114,72(2)°; Z = 2; 5 731 unabhängige Reflexe, R = 0,038). Alle Wasserstofflagen konnten aufgefunden und frei verfeinert werden und beweisen erstmals die Existenz des Tetrahydrogenorthoperiodations im Festkörper. Die Kristallstruktur wird diskutiert und mit denjenigen anderer Alkaliorthoperiodate verglichen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200508
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    Synthesis of cis-Tetrabromobispyridinemolybdates(III) and the crystal structure of cis-(NH4)[MoBr4py2] · ⅓3 H2O (py = pyridine) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 950-954 
    Details
    ISSN: 0044-2313
    Keywords: Tetrabromobispyridinemolybdates ; preparation ; isomerisation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung von cis-tetrabromobispyridinemolybdaten(III) und die Kristallstruktur von cis-(NH4)[MoBr4py2] · ⅓ H2O (py = Pyridin)(NH4)2[MoBr5 · H2O] reagiert mit Pyridin im Acetonitril (CH3CN) bei Zimmertemperatur. Das Produkt ist ein Gemenge von cis- und trans-(pyH)[MoBr4py2], das auf Grund der Löslichkeitsunterschiede aufgetrennt werden kann. cis-M[MoBr4py2] · ⅓ H2O (M = NH4+, Rb+, Cs+), cis-(bipyH)[MoBr4py2] (bipy = 2,2′-Bipyridyl) und cis-(PPh4)[MoBr4py2] wurden aus cis-(pyH)[MoBr4py2] dargestellt.In siedendem Acetonitril (82°C) erfolgt irreversible cis-trans-Isomerisierung. Brom oxidiert das cis-Diastereoisomere zu trans-MoBr4py2.Die Verbindungen wurden durch chemische Analyse, Infrarot-, UV-VIS-Spektroskopie, Konduktometrie und Röntgen-Pulveraufnahmen charakterisiert.Die Kristallstruktur von cis-(NH4)[MoBr4py2] · ⅓ H2O wurde bestimmt: rhomboedrisch, R3c, (No. 161), a = 15,809(3) Å, β = 112,79(2)°, Z = 6, Dröntg. = 2,29, Dgemess. = 2,27(3) g/cm3, V = 2 601(1) Å3, R1 = 0,046, Rw = 0,068. Die mittleren Mo—Br und Mo—N(Pyridin)-Abstände sind 2,58(2) bzw. 2,20(2) Å. cis-Rb[MoBr4py2] · ⅓ H2O und cis-Cs[MoBr4py2] · ⅓ H2O sind isostrukturell mit cis-(NH4)[MoBr4py2] · ⅓ H2O.
    Notes: The reaction between (NH4)[MoBr5 · H2O] and pyridine in acetonitrile (CH3CN) at room temperature results in the mixture of cis- and trans-(pyH)[MoBr4py2] which can be separated on the basis of solubility. cis-M[MoBr4py2] · ⅓ H2O (M = NH4+, Rb+, Cs+), cis-(bipyH)[MoBr4py2] (bipy = 2,2′-bipyridil) and cis-(PPh4)[MoBr4py2], were prepared from cis-(pyH)[MoBr4py2].At the temperature of boiling acetonitrile irreversible cis to trans isomerisation takes place. Bromine oxydizes cis isomers at room temperature to trans-MoBr4py2.The compounds were characterised by chemical analysis, infrared, UV-VIS spectroscopy, conductivity measurements and powder diffraction.The crystal structure of cis-(NH4)[MoBr4py2] · ⅓ H2O has been determined: rhombohedral, R3c, (No. 161), a = 15.809(3) Å, β = 112.79(2)°, Z = 6, DC = 2.29, DO = 2.27(3) g/cm3, V = 2 601(1) Å3, R1 = 0.046, Rw = 0.068. Average Mo—Br and Mo—N(pyridine) distances within the anion are 2.58(2) and 2.20(2) Å. cis-Rb[MoBr4py2] · ⅓ H2O and cis-Cs[MoBr4py2] · ⅓ H2O are isostructural with cis-(NH4)[MoBr4py2] · ⅓ H2O.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200534
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    Synthesis, crystal structure, magnetism, and absorption spectra of A2UX5 Type Halides (A = K, Rb; X = Cl, Br, I)Dedicated to Professor Hugo F. Franzen on his 60th Birthday (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1339-1345 
    Details
    ISSN: 0044-2313
    Keywords: Alkali uranium halides, A2UX5 (A = K, Rb; X = Cl, Br, I) ; preparation ; crystal structure ; magnetic susceptibility ; UV-Vis spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Kristallstruktur, Magnetismus und Absorptionsspektren von Halogeniden des Typs A2UX5 (A = K, Rb; X = Cl, Br, I)Die ternären Uran(III)-halogenide A2UX5 (A = K, Rb; X = Cl, Br, I) wurden aus den binären Komponenten AX und UX3 in verschweißten Tantalampullen gewonnen. Nach Guinier-Aufnahmen (Raumtemperatur) kristallisieren sie sämtlich im K2PrCl5/Y2HfS5-Typ. Einkristall-Strukturverfeinerungen wurden für K2UI5 und Rb2UCl5 unternommen. Magnetische Suszeptibilitätsmessungen erfolgten mit einem SQUID-Magnetometer von Raumtemperatur bis zur Temperatur des flüssigen Heliums: Eindimensionale (innerhalb einer Kette) und dreidimensionale antiferromagnetische Ordnung wird bei tiefen Temperaturen, abhängig vom Abstand U3+—U3+, beobachtet. Absorptionsspektren wurden zwischen 4000 und 28000 cm-1 aufgenommen. Sie zeigen die für U3+ charakteristischen Übergänge und, abhängig vom Halogenid, sehr starke f - d Übergänge oberhalb 14000 bzw. 15000 cm-1.
    Notes: The ternary uranium(III) halides A2UX5 (A = K, Rb; X = Cl, Br, I) have been prepared from the binary components AX and UX3 in sealed tantalum containers. According to their Guinier X-ray powder patterns, they all crystallize with the K2PrCl5/Y2HfS5 type of structure. Lattice constants for ambient temperature are reported. Single-crystal structure refinemens were undertaken for K2UI5 and Rb2UCl5. Magnetic susceptibility data were recorded with a SQUID magnetometer from liquid helium to room temperature. One-dimensional (intrachain) and three-dimensional antiferromagnetic ordering occur at low temperatures dependent upon the U3+—U3+ distance. Absorption spectra were recorded between 4 000 and 28 000 cm-1. They show f - f transitions typical for U3+ and, depending on the halide, very strong f - d transitions above 14 000 to 15 000 cm-1, respectively.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200802
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    Na4[PbO4]  -  Darstellung neuer Plumbate(IV) durch Oxydation intermetallischer PhasenProfessor Hugo F. Franzen zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1346-1350 
    Details
    ISSN: 0044-2313
    Keywords: Sodium orthoplumbate ; preparation ; crystal structure ; MAPLE and CHARDI calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na4[PbO4]  -  Preparation of new Plumbates(IV) by Oxidizing Intermetallic PhasesBy oxidizing NaPb with Na2O2 (molar ratio Na2O2:NaPb = 2.04:1; Ag-tubes; 600°C/50d) we obtained for the first time small orange coloured single crystals of Na4[PbO4]: Na4[SiO4]-type [2], P—1 (I.T. No. 2) with a = 898.5(3); b = 675.6(3); c = 592.2(2) pm; α = 124.75(1)°; β = 96.75(1)°; γ = 100.18(2)°; Z = 2; (four circle diffractometer data (MoKα-; 3 251 Io(hkl); R = 3.4%; Rw = 3.0%), parameters see text. Furthermore the Madelung part of lattice energy (MAPLE), effective coordination numbers (ECoN), mean fictive ionic radii (MEFIR) and the charge distribution (CHARDI) are being calculated.
    Notes: Durch Oxydation von NaPb mit Na2O2 (mol. Verhältnis Na2O2:NaPb = 2,04:1; Ag-Bömbchen; 600°C/50d) wurden erstmals orangefarbene, gedrungene Einkristalle von Na4[PbO4] erhalten: Na4[SiO4]-Typ [2], P—1 (I.T. No. 2) mit a = 898,5(3); b = 675,6(3); c = 592,2(2) pm; α = 124,75(1)°; β = 96,75(1)°; γ = 100,18(2)°; Z = 2; (Vierkreisdiffraktometerdaten; MoKα-; 3 251 Iohkl); R = 3,4%; Rw = 3,0%), Parameter siehe Text. Ferner werden der Madelunganteil der Gitterenergie (MAPLE), Effektive Koordinationszahlen (ECoN), Mittlere Fiktive Ionenradien (MEFIR) und die Ladungsverteilung (CHARDI) berechnet.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200803
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    Synthese und Charakterisierung von Fluorenylgallaten und Fluorenylindaten (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2088-2098 
    Details
    ISSN: 0044-2313
    Keywords: Fluorenyl gallates ; Fluorenyl indates ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Characterization of Fluorenyl Gallates and Fluorenyl IndatesGaCl3 reacts with Fluorenyllithium (LiFl) in the ratio 1:4 in Et2O to [Li(THF)4][GaFl4] (1). The addition of DME (1,2-dimethoxyethane) to solutions of 1 in THF leads to [Li(DME)3][GaFl4] (2) under replacement of THF molecules by DME molecules in the coordination sphere of the Li+ ions.Treatment of InCl with LiFl in Et2O and recrystallization from THF gives [Li(THF)4][ClInFl3] (3), which is formed by an disproportionation reaction. 3 can also be obtained by the reaction of InCl with FlZnCl/LiCl in Et2O and recrystallization from THF.1 and 2 crystallize from THF and THF/DME as [Li(THF)4][GaFl4] · THF (1 · THF) and [Li(DME)3][GaFl4] · THF (2 · THF), respectively. Crystalline 3 is isolated from the reaction of InCl and FlZnCl/LiCl, while the reaction mixture of InCl and LiFl gives after recrystallization in THF 3 · 1,5 THF. The gallate ions in 1 and 2 differ mainly in the position of the fluorenyl ligands. The unit cells of 3 and 3 · 1,5 THF contain two crystallographic unique ion pairs of [Li(THF)4][ClInFl3].
    Notes: GaCl3 reagiert mit Fluorenyllithium (LiFl)Fl = Fluorenyl im Molverhältnis 1:4 in THF zu [Li(THF)4][GaFl4] (1). Durch Zugabe von DME (1,2-Dimethoxyethan) zu Lösungen von 1 in THF werden die THF-Moleküle aus der Koordinationssphäre der Li+-Ionen verdrängt, was zu [Li(DME)3][GaFl4] (2) führt.Bei Einwirkung von LiFl auf InCl in Et2O wird nach einer Disproportionierungsreaktion und Umkristallisieren in THF [Li(THF)4][ClInFl3] (3) gebildet. 3 kann ebenfalls durch die Umsetzung von InCl mit FlZnCl/LiCl in Et2O und Umkristallisieren aus THF erhalten werden.1 kristallisiert aus THF in Form von [Li(THF)4][GaCl4] · THF (1 · THF) und 2 aus THF/DME in Form von [Li(DME)3][GaFl4] · THF (2 · THF). Kristallines 3 wird aus der Reaktion von InCl und FlZnCl/LiCl isoliert, während die Reaktionsmischung von InCl und LiFl nach Umkristallisieren aus THF 3 · 1,5 THF liefert. Die Anionen in 1 · THF und 2 · THF unterscheiden sich nach den Ergebnissen der Röntgenstrukturanalysen hauptsächlich durch die Stellung der Fl-Liganden in den Gallat-Ionen. 3 und 3 · 1,5 THF enthalten zwei kristallographisch unabhängige Ionenpaare [Li(THF)4] · [ClInFl3] in der Elementarzelle.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946201211
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    Tri(1-cyclohepta-2,4,6-trienyl)phosphan, P(C7H7)3 und Tetra(1-cyclohepta-2,4,6-trienyl)phosphonium-tetrafluoroborat, [P(C7H7)4]BF4Professor Reinhard Schmutzler zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2108-2113 
    Details
    ISSN: 0044-2313
    Keywords: Cyclohepta-2,4,6-trienyl compounds ; synthesis ; crystal structure ; NMR spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tri(1-cyclohepta-2,4,6-trienyl)phosphane, P(C7H7)3, and Tetra(1-cyclohepta-2,4,6-trienyl)phosphonium Tetrafluoroborate, [P(C7H7)4]BF4The reaction of tris(trimethylsilyl)phosphane, P(SiMe3)3, with tropylium bromide, C7H7+Br-, in polar solvents such as dichloromethane or tetrahydrofuran gives P(C7H7)3 (1) and [P(C7H7)4]Br (2a). According to the X-ray crystallographic structure determinations, all 1-cyclohepta-2,4,6-trienyl substituents are present in the boat conformation in both P(C7H7)3 (1) and the phosphonium salt, [P(C7H7)4]BF4 (2b). The boat-shaped C7H7 rings are significantly more flattened if the phosphorus occupies the axial rather than the equatorial position at the ring substituent.Addition of a chalcogen to the lone pair at the central phosphorus atom of 1 leads to the chalcogena-phosphoranes EP(C7H7)3 (E = O (3a), S (3b), Se (3c)). The new 1-cyclohepta-2,4,6-trienyl-phosphorus compounds 1, 2 b and 3a-c were characterized by their 1H, 13C, and 31P NMR spectra in C6D6 solution.
    Notes: Die Umsetzung von Tris(trimethylsilyl)phosphan, P(SiMe3)3, mit Tropyliumbromid, C7H7+Br-, in polaren Solvenzien wie Dichlormethan oder Tetrahydrofuran ergibt P(C7H7)3 (1) und [P(C7H7)4]Br (2a). Nach den Kristallstruktur-Bestimmungen liegen alle 1-Cyclohepta-2,4,6-trienyl-Substituenten sowohl in P(C7H7)3 (1) als auch im Phosphoniumsalz [P(C7H7)4]BF4 (2b) in der Wannen-Konformation vor. Die wannenförmigen C7H7-Ringe sind deutlich stärker abgeflacht, wenn Phosphor die axiale anstelle der äquatorialen Position am Ringsubstituenten einnimmt.Addition eines Chalkogens an das freie Elektronenpaar am zentralen Phosphoratom führt zu den Chalkogena-phosphoranen EP(C7H7)3 (E = O (3a), S (3b), Se (3c)). Die neuen 1-Cyclohepta-2,4,6-trienyl-Phosphorverbindungen 1, 2 b und 3a-c wurden anhand ihrer 1H-, 13C- und 31P-NMR-Spektren in C6D6-Lösung charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19946201214
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    Darstellung und Kristallstruktur des ersten polymeren Phosphorselenids catena-(P4Se4)x (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1832-1836 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorus selenide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of the First Polymeric Phosphorus Selenide catena-(P4Se4)xCatena-(P4Se4)x was prepared in crystalline form from the elements using iodine as a catalyst, and characterized by means of X-ray diffraction and IR spectroscopy. Single-crystal investigations (space group P21/c, a = 1 119.2(3), b = 728.2(2), c = 1 142.5(3) pm, β = 115.91(2)°, V = 837.5(7) · 106 pm3) revealed parallel chains of P4Se3 hetero-norbornane units linked via Se atoms. Thus, being the first phosphorus selenide which does not contain discrete molecules, catena-(P4Se4)x can be regarded as a polymeric form of α-P4Se4 or as a crystalline modification of vitrous phosphorus selenide.
    Notes: Catena-(P4Se4)x wurde aus den Elementen unter dem katalytischen Einfluß von Iod in kristalliner Form dargestellt. Die Charakterisierung erfolgte röntgenographisch sowie IR-spektroskopisch. Nach einer Strukturbestimmung an einem Einkristall (Raumgruppe P21/c, a = 1 119,2(3), b = 728,2(2), c = 1 142,5(3) pm, β = 115,91(2)°, V = 837,5(7) · 106 pm3) liegen darin parallele Ketten Se-verbrückter P4Se3-hetero-Norbornan-Einheiten vor. Als erstes nicht aus diskreten Molekülen aufgebautes Phosphorselenid kann catena-(P4Se4)x sowohl als polymerisierte Form des α-P4Se4 wie auch als kristalline Modifikation eines Phosphoreselenidglases aufgefaßt werden.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201028
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    Zur Kenntnis einer modifizierten Form des β-CuNdW2O8-Typs: γ-CuTbW2O8Professor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1850-1854 
    Details
    ISSN: 0044-2313
    Keywords: Copper Terbium tungstate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On a Modified Form of the β-CuNdW2O8 Type: γ-CuTbW2O8Single crystals of γ-CuTbW2O8 were prepared by flux in closed copper tubes. X-ray investigations show triclinic symmetry, space group Ci1-P1, with a = 6.722, b = 9.831, c = 15.352 Å, α = 72.82, β = 88.53, γ = 71.76°, Z = 6. γ-CuTbW2O8 is closely related to β-CuNdW2O8. One significant difference can be seen in an alternate staggered location of Tb3+ ions along [110].
    Notes: Einkristalle von γ-CuTbW2O8 wurden in geschlossenen Kupferampullen dargestellt und röntgenographisch untersucht. γ-CuTbW2O8 kristallisiert mit trikliner Symmetrie, Raumgruppe Ci1-P1, a = 6,722, b = 9,831, c = 15,352 Å, α = 72,82, β = 88,53, γ = 71,76°, Z = 6 und zeigt enge Verwandtschaft zu β-CuNdW2O8. Signifikanter Unterschied ist eine abwechselnde Stapelung von Tb3+-Ionen längs [110].
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201103
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    N(B(NMe2)2)(Si(NMe2)3)(Ti(NMe2)3), [N(Si(NMe2)3)(Ti(NMe2)2)]2 und N(SiMe3)(Si(NMe2)3)(Ti(NMe2)3)  -  Synthese und Charakterisierung neuer molekularer Einkomponentenvorläufer für nitridische und carbonitridische Keramiken (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 366-370 
    Details
    ISSN: 0044-2313
    Keywords: Bis(dimethylamino)boryl-tris(dimethylamino)silyl-tris(dimethylamino)titanylamin ; N,N′-Bis(tris(dimethylamino)-silyl)-1,1,3,3-tetrakis(dimethylamino)cyclobistitanazan, Trimethylsilyl-tris(dimethylamino)silyl-tris(dimethylamino)titanylamin ; Trimethylsilyl-tris(dimethylamino)-silylamin ; synthesis ; nmr spectra ; mass spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N(B(NMe2)2)(Si(NMe2)3) (Ti(NMe2)3), [N(Si(NMe2)3)(Ti(NMe2)2)]2 und N(SiMe3)(Si(NMe2)3)(Ti(NMe2)3)  -  Synthesis and Characterization of New Molecular Single-source Precursors for Nitride and Carbonitride CeramicsSynthesis and spectroscopic data of the title compounds are reported. [N(Si(NMe2)3)(Ti(NMe2)2)]2 crystallizes in the space group P1, a = 8.406(7), b = 10.673(8), c = 10.872(6) Å, α = 68.45(4)°, β = 71.72(4)°, γ = 78.11(7)°, 2 877 diffractometer data (Fo ≥ 2σFo), R = 0.051. The compound is characterized by a planar four-membered Ti2N2-ring with exocyclic tris(dimethylamino)silyl substituents attached to the nitrogen atoms of the ring.
    Notes: Darstellung, kernresonanz- und massenspektroskopische Daten der Titelverbindungen werden mitgeteilt. [N(Si(NMe2)3)(Ti(NMe2)2)]2 kristallisiert in der Raumgruppe P1 mit den Gitterkonstanten a = 8,406(7), b = 10,673(8), c = 10,872(6) Å, α = 68,45(4)°, β = 71,72(4)°, γ = 78,11(7)°. 2 877 Diffraktometerdaten (Fo ≥ 2σFo), R = 0,051. Die Verbindung besitzt einen planaren Ti2N2-Vierring mit exocyclischen Tris(dimethylamino)silylsubstituenten an den Stickstoffatomen des Rings.
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    URL: http://dx.doi.org/10.1002/zaac.19946200228
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    The Molybdenum Stannide MoSn2In memoriam Konrad Schubert (1915-1992) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 467-470 
    Details
    ISSN: 0044-2313
    Keywords: MoSn2 ; crystal structure ; Pauli paramagnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Das Molybdän-Stannid MoSn2Die Titelverbindung wurde durch Tempern von Molybdän-Pulver mit einem Überschuß von Zinn hergestellt. Einkristalle wurden durch Auflösen der zinnreichen Matrix in Salzsäure erhalten. Sie sind Pauli-paramagnetisch. Die Kristallstruktur wurde aus Einkristall-Röntgen-Diffraktometer-Daten bestimmt: P6222, a = 548,8(1) pm, c = 1417,1(2) pm, Z = 6, R = 0,036 für 18 variable Parameter und 389 Strukturfaktoren. MoSn2 ist erst der zweite Vertreter der hexagonalen Mg2Ni-Struktur. Die Beziehung der Struktur zum CuAl2-Typ wird diskutiert.
    Notes: The title compound was prepared by annealing molybdenum powder with an excess of tin. Single-crystals were obtained by dissolving the tin-rich matrix in hydrochloric acid. They are Pauli paramagnetic. The crystal structure was determined from single-crystal X-ray diffractometer data: P6222, a = 548.8(1) pm, c = 1417.1(2) pm, Z = 6, R = 0.036 for 18 variable parameters and 389 structure factors. MoSn2 is only the second representative of the hexagonal Mg2Ni-type structure. The relation of the structure to the CuAl2-type is discussed.
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    URL: http://dx.doi.org/10.1002/zaac.19946200310
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    Synthetic and structural Studies on Organomolybdenum-Bismuth Halide Complexes (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 457-466 
    Details
    ISSN: 0044-2313
    Keywords: Organomolybdenum-bismuth halide complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Untersuchungen zur Synthese und Struktur von Organomolybdän-Bismuthalogenid-KomplexenDie Reaktionen von BiBr2Ph mit Na/K[Mo(CO)3(η—C5H5)], von [BiPh{Mo(CO)3(η—C5H5)}2] mit BiBr2Ph oder BiBr3 und BiPh3 mit [Bi{Mo(CO)3(η—C5H5)}3] ergeben den Komplex [BiBrPh{Mo(CO)3(η—C5H5)}] 1, der röntgenographisch charakterisiert worden ist. Der Komplex 1 besteht aus einem Bismutzentrum mit einem Bromatom, einer Phenylgruppe und einer Mo(CO)3(η—C5H5)-Einheit. Eine intermolekulare Wechselwirkung besteht zum Bromatom eines benachbarten Moleküls, wodurch sich eine eindimensionale polymere Struktur ergibt. Bei der Umsetzung mit einer Bromidabgebenden Verbindung wird zunächst der anionische Komplex [BiBr2Ph{Mo(CO)3(η—C5H5)}2]- 3- und bei längerer Reaktion [BiBr2{Mo(CO)3(η—C5H5)}2]- 5- gebildet, das als [Ph4P]+-Salz röntgenographisch charakterisiert wurde. Der Komplex 5-, der am Bi zwei Br und zwei Mo(CO)3(η—C5H5)-Einheiten enthält, liegt in einer Struktur zwischen unvollständig trigonal-pyramidal und tetraedrisch vor. Der Komplex [PPN]2[Bi2Cl6{Mo(CO)3(η—C5H5)}2] 8 wurde ebenfalls dargestellt und röntgenographisch charakterisiert. Es liegt ein dimeres Anion vor, das aus zwei quadratischen Pyramiden mit einer gemeinsamen Kante besteht, in denen die Chloratome in der Basisebene und die zwei Mo(CO)3(η—C5H5)-Einheiten sich an den Spitzen in gegenüberliegenden Positionen befinden.
    Notes: The reactions between either BiBr2Ph and Na/K[Mo(CO)3(η—C5H5)], [BiPh{Mo(CO)3(η—C5H5)}2] and BiBr2Ph, or BiBr3 and BiPh3 and [Bi{Mo(CO)3(η—C5H5)}3] afford the complex [BiBrPh{Mo(CO)3(η—C5H5)}] 1 which has been characterised by X-ray crystallography. Complex 1 comprises a bismuth centre bonded to a bromine atom, a phenyl group and a Mo(CO)3(η—C5H5) fragment together with a longer secondary intermolecular interaction between a bromine from an adjacent molecule which results in a one-dimensional polymeric structure. Addition of a source of bromide anion to 1 affords the anionic complex [BiBr2Ph{Mo(CO)3(η—C5H5)}]- 3- although prolonged reaction results in the complex [BiBr2{Mo(CO)3(η—C5H5)}2]- 5- which was characterised by X-ray crystallography as its [Ph4P]+ salt. Complex 5- comprises a mononuclear bismuth centre bonded to two bromine atoms and two Mo(CO)3(η—C5H5) fragments in a geometry which lies between equatorially vacant trigonal bipyramidal and tetrahedral. The complex [PPN]2[Bi2Cl6{Mo(CO)3(η—C5H5)}2] 8 has also been synthesised and characterised by X-ray crystallography. A dimeric dianion is observed which can be viewed as two edge-shared square-based pyramids with chlorine atoms in the basal planes and Mo(CO)3(η—C5H5) fragments in the apical positions on opposite sides of the Bi2Cl6 plane.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200309
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  • 188
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    Zwei neue Silicat-Chloride mit zweiwertigem Europium: LiEu3[SiO4]Cl3 und Li7Eu8[SiO4]4Cl7Professor Philipp Gütlich zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1351-1356 
    Details
    ISSN: 0044-2313
    Keywords: Silicate-chloride ; crystal structure ; europium ; lithium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Two New Silicate-Chlorides with Divalent Europium: LiEu3[SiO4]Cl3 and Li7Eu8[SiO4]4Cl7LiEu3[SiO4]Cl3 was prepared by reaction of LiCl with Eu2SiO4 and Li7Eu8[SiO4]4Cl7 from Li with Eu2O3, SiO2 and LiCl. The crystal structures of LiEu3[SiO4]Cl3 (Pmna, a = 946.95(13); b = 699.52(8); c = 1 368.0(2) pm; Z = 4; R1 = 0.0325, R2w = 0.0642) and Li7Eu8[SiO4]4Cl7 (P21/c; a = 851.85(5); b = 948.62(7); c = 1 679.0(2) pm; β = 96.221(8)°; Z = 2; R1 = 0.0352, R2w = 0.0744) were determined from four-circle diffractometer data. LiEu3[SiO4]Cl3 contains [Li(SiO4)2] units and LiCl6 octahedra while in Li7Eu8[SiO4]4Cl7 larger „lithosilicate“ groups are found. In both structures, the Eu2+ ions are coordinated mostly eightfold by O2- and Cl- ligands.
    Notes: LiEu3[SiO4]Cl3 wurde durch Umsetzung von LiCl mit Eu2SiO4 dargestellt, Li7Eu8[SiO4]4Cl7 durch Umsetzung von Li mit Eu2O3, SiO2 und LiCl. Die Kristallstrukturen von LiEu3[SiO4]Cl3 (Pmna, a = 946,95(13); b = 699,52(8); c = 1 368,0(2) pm; Z = 4; R1 = 0,0325, R2w = 0,0642) und Li7Eu8[SiO4]4Cl7 (P21/c; a = 851,85(5); b = 948,62(7); c = 1 679,0(2) pm; β = 96,221(8)°; Z = 2; R1 = 0,0352, R2w = 0,0744) wurden aus Einkristall-Vierkreisdiffraktometer-Daten bestimmt. LiEu3[SiO4]Cl3 enthält [Li(SiO4)2]-Einheiten neben LiCl6-Oktaedern, während in Li7Eu8[SiO4]4Cl7 größere „Lithosilicat“-Baugruppen vorliegen. Die Eu2+-Ionen sind in beiden Strukturen meist achtfach von O2-- und Cl--Liganden koordiniert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200804
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  • 189
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    Beiträge zur Chemie der Alkylverbindungen von Übergangsmetallen. 61. Darstellung und Kristallstruktur von Tetramethyltitan-1,2-bis(dimethylphosphino)ethan (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 523-526 
    Details
    ISSN: 0044-2313
    Keywords: Tetramethyltitanium-1,2-bis(dimethylphosphino)-ethane ; NMR data ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Transition Metal Alkyl Compounds. 61. Preparation and Crystal Structure of Tetramethyltitanium-1,2-bis(dimethylphosphino)ethaneThe title complex 1 was synthesized by addition of 1,2-bis(dimethylphosphino)ethane to a solution of tetramethyltitanium in diethylether. The complex was characterized by 1H, 13C and 31P NMR spectra and by X-ray crystal structure analysis. 1 consists of two independent molecules with distorted octahedral structure.
    Notes: Der Titelkomplex 1 wurde durch Addition von 1,2-Bis(dimethylphosphino)ethan an Tetramethyltitan in Diethylether erhalten. Der Komplex wurde 1H-, 13C- und 31P-NMR-spektroskopisch, sowie durch Röntgenkristallstruktur-analyse charakterisiert. 1 tritt in der Elementarzelle in zwei unabhängigen Molekülen mit verzerrt oktaedrischer Konstitution auf.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200322
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  • 190
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    Synthese und Kristallstruktur eines Natrium-tetraoxonitridowolframats(VI), Na5WO4N (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 535-538 
    Details
    ISSN: 0044-2313
    Keywords: Sodium tetraoxo nitrido tungstate(VI) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Sodium Tetraoxo Nitrido Tungstate(VI), Na5WO4NColourless crystals of Na5WO4N are obtained besides Na4WO2N2 [1] by the reaction of WO3 with NaNH2 (15:1) at 350°C ≥ T ≥ 750°C in autoclaves to prevent early decomposition of sodium amide. X-ray single crystal investigations are characterized by the following data:Na5WO4N: Cmc21 (No. 36), Z = 4a = 9.873(2) Å, b = 5.769(1) Å, c = 10.648(2) ÅZ(F2o)≥ 3σ(F2o) = 2182, Z(Var.) = 55, R/Rw = 0.029/0.039The structure contains the tetragonal pyramidal ion WO4N5- with nitrogen at the apex connected via Na+ ions irregularly coordinated by one nitrogen and four oxygen atoms of different anions.
    Notes: Farblose Kristalle von Na5WO4N entstehen neben Na4WO2N2 [1] bei der Umsetzung von WO3 mit NaNH2 (15:1) bei 350°C ≥ T ≥ 750°C in Autoklaven, die eine frühzeitige Zersetzung von Natriumamid verhindern. Die röntgenographische Strukturbestimmung an Einkristallen ist durch folgende Daten charakterisiert:Na5WO4N: Cmc21 (Nr. 36), Z = 4a = 9,873(2) Å, b = 5,769(1) Å, c = 10,648(2) ÅZ(F2o) ≥ 3σ(F2o) = 2182, Z(Var.) = 55, R/Rw = 0,029/0,039Die Struktur enthält das tetragonal pyramidale Ion WO4N5 mit Stickstoff in apikaler Position. Die Anionen sind durch Na+-Ionen verknüpft, die unregelmäßig von einem N- und vier O-Atomen unterschiedlicher Anionen koordiniert sind.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200325
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  • 191
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    Zur Kristallchemie eines neuen Barium-Lanthanoid-Oxozinkats: Ba2Er2Zn8O13 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 527-530 
    Details
    ISSN: 0044-2313
    Keywords: Barium ; rare earth ; zinc ; oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Chemistry of a New Barium Rare-Earth Oxozincate: Ba2Er2Zn8O13High temperature reactions led to single crystals of Ba2Er2Zn8O13. It crystallizes with orthorhombic symmetry, space group C122v—Cmc21, a = 6.276, b = 10.871, c = 10.195 Å, Z = 2. The hitherto unknown crystal structure shows Zn2+ with tetrahedral, Er3+ octahedral and Ba2+ cuboctahedral coordination by O2-. It will be shown that parts of the [Zn8O13] network are fragments of the ZnO structure showing O2- within a tetrahedral zinc coordination. A deficit of two O2- ions per unit cell is focused on two point positions.
    Notes: Durch Hochtemperaturreaktionen wurden Einkristalle von Ba2Er2Zn8O13 dargestellt und anschließend röntgenographisch untersucht. Die Verbindung kristallisiert in einem neuen Strukturtyp mit orthorhombischer Symmetrie, Raumgruppe C122v—Cmc21; a = 6,276; b = 10,871; c = 10,195 Å; Z = 2. Die bisher unbekannte Kristallstruktur zeigt Zn2+ in tetraedrischer, Er3+ in oktaedrischer und Ba2+ in kuboktaedrischer Koordination von O2-. Es wird gezeigt, daß das [Zn8O13]-Gerüst Fragmente der ZnO-Struktur mit O2- in tetraedrischer Zinkkoordination enthält. Ein Defizit von zwei O2 pro Elementarzelle verteilt sich auf zwei Punktlagen.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200323
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  • 192
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    Zur Reaktion von 2,2′-Dilithiumbiphenyl mit SmBr3 Die Struktur von [(C24H16)SmBr(thf)2]2 · [C24H14] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 703-706 
    Details
    ISSN: 0044-2313
    Keywords: SmIII dimeric complex ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reaction of Dilithiumbiphenyl with SmBr3. The Crystal Structure of [(C24H16)SmBr(thf)2]2 · [C24H14]In THF SmBr3 forms with [(biph)Li2] the dimeric complex [(quaph)SmBr(thf)2]2 · [C24H14]. The structure was characterized by X-ray single crystal structure analysis (space group P1 (No. 2), Z = 1, a = 943.3(6) pm, b = 1 350.3(1) pm, c = 1 599.9(9) pm, α = 64.99(5)°, β = 89.02(5)°, γ = 73.02(6)°). The Sm iones are bridged by two Br iones. Coordination by one quaph and THF ligands leads to distorded octahedra coordination of the Sm iones. Additionally crystallizes one molecule dibenzonaphthacene.
    Notes: SmBr3 reagiert mit [(biph)Li2] in THF zu dem zweikernigen Komplex [(quaph)SmBr(thf)2]2 · [C24H14]. Der Aufbau konnte durch eine Kristallstrukturanalyse geklärt werden (Raumgruppe P1 (Nr. 2), Z = 1, a = 943,3(6) pm, b = 1 350,3(1) pm, c = 1 599,9(9) pm, α = 64,99(5)°, β = 89,02(5)°, γ = 73,02(6)°). Die Sm-Ionen werden durch zwei Br-Ionen verbrückt. Durch zusätzliche Koordination eines quaph- und zweier THF-Liganden ist jedes Sm-Ion verzerrt oktaedrisch koordiniert. Zusätzlich kristallisiert ein Molekül Dibenzonaphthacen mit aus.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200420
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  • 193
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    Dimethylzinndithioquadratat: Die Kristallstruktur des Benzol-Solvats und des Dimethylsulfoxid-Addukts (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 723-729 
    Details
    ISSN: 0044-2313
    Keywords: Dimethyltin dithiosquarate benzene solvate ; Dimethyltin dithiosquarate-dimethylsulfoxide adduct ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimethyltin Dithiosquarate: The Crystal Structure of the Benzene Solvate and of the Dimethylsulfoxide Adduct(CH3)2SnS2C4O2 · 1/3 C6H6 (I) crystallizes in the orthorhombic space group Pnma. a = 14.393(2), b = 21.668(3), c = 10.424(1) Å, Z = 12.(CH3)2SnS2C4O2 · (CH3)2SO (II) is monoclinic, space group P21/n, a = 9.918(5), b = 12.028(6), c = 12.223(6) Å, β = 108.82(3)°, Z = 4.In I there are two independent dimethyltin dithiosquarate molecules. But in both molecules the Sn atoms display weak coordinative bonds to two O atoms of adjacent dithiosquarate groups. The distances amount 2.873 Å (2×), resp. 2.678 and 2.831 Å. The coordination number of tin becomes 6 and the structure gets connected in three dimensions.In II dimethylsulfoxide is bound with the O atom to Sn (2.345 Å) and the result is a distorted trigonal bipyramid. There a more distant O atom (2.944 Å) leads to a connection of the molecules to a ribbon. The changes of the geometrical parameters are described, which result from the progressive approach of the one O atom.
    Notes: (CH3)2SnS2C4O2 · 1/3 C6H6 (I) kristallisiert in der orthorhombischen Raumgruppe Pnma; a = 14,393(2); b = 21,668(3); c = 10,424(1) Å; Z = 12.(CH3)2SnS2C4O2 · (CH3)2SO (II) ist monoklin, Raumgruppe P21/n; a = 9,918(5); b = 12,028(6); c = 12,223(6) Å; β = 108,82(3)°; Z = 4.In I liegen zwei kristallographisch unabhängige Dimethyl-zinndithioquadratat-Moleküle vor. Bei beiden weisen jedoch die Sn-Atome schwache koordinative Bindungen zu zwei O-Atomen benachbarter Dithioquadratat-Gruppen auf. Die Abstände betragen 2,873 Å (2×) bzw. 2,678 und 2,831 Å. Dadurch erhält Zinn die Koordinationszahl 6, und es ergibt sich eine dreidimensional vernetzte Struktur.In II ist Dimethylsulfoxid über das O-Atom an Sn gebunden (2,345 Å), und es liegt eine verzerrte trigonale Bipyramide vor. Ein weiter entferntes O-Atom (2,944 Å) bewirkt hier die Vernetzung der Moleküle zu einem Band. Die Veränderungen der geometrischen Parameter als Folge der fortschreitenden Annäherung des einen O-Atoms werden beschrieben.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200423
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  • 194
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    Ein neues Mangan(II)-Oxowolframat: Mn3WO6 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 733-736 
    Details
    ISSN: 0044-2313
    Keywords: Manganese(II) oxotungstate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On a New Manganese(II) Oxotungstate: Mn3WO6Single crystals of Mn3WO6 were prepared by CO2-LASER technique in H2-atmosphere and investigated by single crystal X-ray work. It crystallizes with rhombohedral symmetry, space group C3i2—R3 with the hexagonal lattice constants a = 8.8931 Å; c = 10.4782 Å and Z = 6. Mn3WO6 is isotypic to Mg3TeO6 and α-Ca3UO6 and characterized by to each other isolated WO6 octahedra. The surrounding of them by six inner-sphere and six outer-sphere MnO6 polyhedra is discussed.
    Notes: Mn3WO6 wurde mit CO2-LASER-Technik in H2-Atmosphäre einkristallin dargestellt und röntgenographisch untersucht. Es kristallisiert rhomboedrisch in der Raumgruppe C3i2—R3 mit a = 8,8931 Å; c = 10,4782 Å und Z = 6. Mn3WO6 ist isotyp zu Mg3TeO6 und α-Ca3UO6 und durch isolierte Oktaeder WO6 ausgezeichnet. Deren Umgebung durch sechs Polyeder MnO6 in „innerer“ und sechs weiterer in äußerer Sphäre wird diskutiert.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200425
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    Die Kristallstruktur von Tris(N,N-Diethyl-N′-benzoylselenoureato)indium(III)Professor E. O. Fischer zum 75. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 737-742 
    Details
    ISSN: 0044-2313
    Keywords: Indium ; tris(N,N-diethyl-N′-benzoylselenoureato)indium(III) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Tris(N,N-Diethyl-N′-benzoylselenoureato)indium(III)In(C12H15N2OSe)3 crystallizes in the monoclinic space group P21/c. The cell parameters are a = 11.792(2), b = 36.797(4), c = 18.574(2) Å, β = 92.15(2)° and Z = 4. The structure was solved with Patterson and direct methods and was refined to a final R-value of 3.41%. The asymmetric unit contains two complex molecules. The indium atoms are bidentally coordinated by three N,N-Diethyl-N′-benzoylselenourea molecules to form distorted octahedra with facial arrangement of the selenium and oxygen donor atoms. The chelate rings diverge strongly from planarity. The In—Se bond lengths vary from 2.643(1) to 2.657(1) Å, the In—O bond lengths from 2.179(4) to 2.203(4) Å, respectively.
    Notes: In(C12H15N2OSe)3 kristallisiert in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 11,792(2), b = 36,797(4), c = 18,574(2) Å, β = 92,15(2)°, Z = 4. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 3,41% verfeinert. In der asymmetrischen Einheit befinden sich zwei In(C12H15N2OSe)3-Komplexmoleküle. Jeweils drei N,N-Diethyl-N′-benzoylseleno-harnstoff-Moleküle sind bidental über Selen- und Sauerstoffatome an die Zentralatome koordiniert. Das Koordinationspolyeder ist ein verzerrter Oktaeder mit facialer Anordnung der Donoratome. Die Chelatringe weichen deutlich von der Planarität ab. Die In—Se-Abstände in den beiden Oktaedern liegen zwischen 2,643(1) und 2,657(1) Å, die In—O-Abstände variieren von 2,179(4) bis 2,203(4) Å.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200426
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    [TMPA]4[Si8O20] · 34 H2O and [DDBO]4[Si8O20] · 32 H2O are heteronetwork clathrates with 1,1,4,4-tetramethylpiperazinium (TMPA) and 1,4-dimethyl-1,4-diazoniabicyclo[2.2.2]octane (DDBO) guest cations (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 757-765 
    Details
    ISSN: 0044-2313
    Keywords: Silicate hydrate ; 1,1,4,4-tetramethylpiperazinium ; 1,4-dimethyl-1,4-diazoniabicyclo[2.2.2]octane ; 1,1-dimethylpiperidinium ; clathrate ; crystal structure ; double four-ring silicate anion ; hydrogen bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [TMPA]4[Si8O20] · 34 H2O und [DDBO]4[Si8O20] · 32 H2O sind Heteronetzwerk-Clathrate mit 1,1,4,4-Tetramethylpiperazinium (TMPA) und 1,4-Dimethyl-1,4-Diazoniabicyclo[2.2.2]octan (DDBO) Gastkationen[TMPA]4[Si8O20] · 34 H2O (1) und [DDBO]4[Si8O20] · 32 H2O (2) wurden durch Kristallisation aus wäßrigen Lösungen der entsprechenden quartären Alkylammoniumhydroxide und SiO2 erhalten. Die Kristallstrukturen wurden mittels Einkristallröntgenbeugung bestimmt. 1: Monoklin, a = 16,056(2), b = 22,086(6), c = 22,701(2) Å, β = 90,57(1)° (T = 210 K), Raumgruppe C2/c, Z = 4. 2: Monoklin, a = 14,828(9), b = 20,201(7), c = 15,519(5) Å, β = 124,13(4)° (T = 255 K), Raumgruppe P21/c, Z = 2. Die Polyhydrate sind strukturverwandte Wirt-Gast-Verbindungen mit dreidimensionalen Wirtstrukturen aus über Wasserstoffbrücken verknüpften oligomeren Anionen [Si8O20]8- und H2O-Molekülen. Die Silicat-Anionen haben eine würfelförmige Doppelvierring-Struktur und eine lokale Umgebung, die von 24 H2O-Molekülen und sechs Kationen (TMPA, [C8H20N2]2+, oder DDBO, [C8H18N2]2+) gebildet wird. Die Kationen befinden sich als Gastspezies in großen, unregelmäßigen, käfigartigen Hohlräumen. Untersuchungen mittels der 29Si-NMR-Spektroskopie und der Trimethylsilylierungsmethode haben gezeigt, daß die gesättigten Lösungen von 1 und 2 hohe Anteile an Doppelvierring-Anionen enthalten. Derartige Anionen sind auch in der gesättigten Lösung des Heteronetzwerk-Clathrats [DMPI]6[Si8O18(OH)2] · 48,5 H2O (3) mit 1,1-Dimethylpiperidinium-Kationen (DMPI, [C7H16N]+) als Gastspezies enthalten.
    Notes: [TMPA]4[Si8O20] · 34 H2O (1) and [DDBO]4[Si8O20] · 32 H2O (2) have been prepared by crystallization from aqueous solutions of the respective quaternary alkylammonium hydroxide and SiO2. The crystal structures have been determined by single-crystal X-ray diffraction. 1: Monoclinic, a = 16.056(2), b = 22.086(6), c = 22.701(2) Å, β = 90.57(1)° (T = 210 K), space group C2/c, Z = 4. 2: Monoclinic, a = 14.828(9), b = 20.201(7), c = 15.519(5) Å, β = 124.13(4)° (T = 255 K), space group P21/c, Z = 2. The polyhydrates are structurally related host-guest compounds with three-dimensional host frameworks composed of oligomeric [Si8O20]8- anions and H2O molecules which are linked via hydrogen bonds. The silicate anions possess a cube-shaped double four-ring structure and a characteristic local environment formed by 24 H2O molecules and six cations (TMPA, [C8H20N2]2+, or DDBO, [C8H18N2]2+). The cations themselves reside as guest species in large, irregular, cage-like voids. Studies employing 29Si NMR spectroscopy and the trimethylsilylation method have revealed that the saturated aqueous solutions of 1 and 2 contain high proportions of double four-ring silicate anions. Such anions are also abundant species in the saturated solution of the heteronetwork clathrate [DMPI]6[Si8O18(OH)2] · 48.5 H2O (3) with 1,1-dimethylpiperidinium (DMPI, [C7H16N]+) guest cations.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200430
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  • 197
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    Eine neue Hochtemperaturform von TiO: H—TiOProfessor Wilhelm Preetz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1175-1178 
    Details
    ISSN: 0044-2313
    Keywords: Titanium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New High Temperature Form of TiO: H—TiOSingle crystals of a high temperature form of TiO (H—TiO) were prepared above 3 000°C by CO2-LASER technique. They crystallize with a hitherto unobserved crystal structure of oxides with titanium in the oxidation state two, isotypic to tungsten carbide with Ti2+ in a trigonal prismatic surrounding by oxygen. Space group D3h1-P6m2, a = 3.0310, c = 3.2377 Å, Z = 1.
    Notes: Mit CO2-LASER-Technik wurden bei Temperaturen oberhalb 3 000°C Einkristalle einer Hochtemperaturform von TiO (H—TiO) dargestellt. Sie kristallisieren mit einer an Oxiden des zweiwertigen Titans bisher nicht beobachteten Kristallstruktur, isotyp zu Wolframcarbid, mit Ti2+ in trigonal prismatischer Sauerstoffumgebung. Raumgruppe D3h1—P6m2; a = 3,0310; c = 3,2377 Å; Z = 1.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200708
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  • 198
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    Synthese und Kristallstruktur von Na10[P4(NH)6N4](NH2)6(NH3)0,5 mit dem adamantanartig aufgebauten Anion [P4(NH)6N4]4-Professor Wilhelm Preetz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1213-1218 
    Details
    ISSN: 0044-2313
    Keywords: Sodium imido nitrido phosphate(V) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Na10[P4(NH)6N4](NH2)6(NH3)0.5 with an Adamantane-like Anion [P4(NH)6N4]4-Crystals of Na10[P4(NH)6N4](NH2)6(NH3)0.5 were obtained by the reaction of P3N5 with NaNH2 (molar ratio 1:20) within 5 d at 600°C in autoclaves. The following data characterize X-ray investigations:Fm3m, Z = 8, a = 15.423(2) Å, Z(F02) = 261 with F02 ≥ 3 σ(F02) Z(Variables) = 27, R/Rw = 0.086/0.089The compound contains the hitherto unknown anion [P4(NH)6N4]4-, which resembles adamantane. The total structure can be described as follows: The centers of gravity of units of [Na8(NH2)6(NH3)]2+ - 8Na+ on the corners of a cube, 6NH2- on the ones of an inscribed octahedron with NH3 in the center - follow the motif of a cubic-closest packed arrangement. Units of [Na12(NH2)6]6+ - 12Na+ on the corners of a cuboctahedron and 6NH2- on the ones of an inscribed octahedron - occupy all octahedral and those of [P4(NH)6N4]4- all tetrahedral sites.
    Notes: Für eine Strukturbestimmung an Na10[P4(NH)6N4](NH2)6(NH3)0,5 geeignete Kristalle entstehen bei der Umsetzung von P3N5 mit NaNH2 (Molverhältnis 1:20) nach 5 d bei 600°C in Autoklaven. Folgende Daten charakterisieren röntgenographische Untersuchungen an der Verbindung:Fm3m, Z = 8, a = 15,423(2) Å, Z(F02) = 261 mit F02 ≥ 3 σ(F02) Z(Parameter) = 27, R/Rw = 0,086/0,089Die Verbindung enthält das bisher unbekannte Anion [P4(NH)6N4]4-, das adamantanartig aufgebaut ist. Die gesamte Struktur läßt sich folgendermaßen beschreiben: Die Schwerpunkte von Einheiten [Na8(NH2)6(NH3)]2+ - 8Na+ auf den Ecken eines Würfels, 6NH2- auf denen eines einbeschriebenen Oktaeders mit NH3 als Zentrum - bilden das Motiv einer kubisch dichtesten Kugelpackung. Diejenigen von Einheiten [Na12(NH2)6]6+ - 12 Na+ auf den Ecken eines Kuboktaeders und 6NH2- auf denen eines einbeschriebenen Oktaeders - besetzen darin alle Oktaederlücken und diejenigen von [P4(NH)6N4]4- alle Tetraederlücken.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200714
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  • 199
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    HgPb2O2Cl2, ein „perforiertes“ Blei(II)-oxidProfessor Friedo Huber zum 65. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 977-980 
    Details
    ISSN: 0044-2313
    Keywords: Mercury(II) lead(II) oxide chloride ; synthesis ; crystal structure ; structural comparison ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: HgPb2O2Cl2, a “Perforated” Lead(II) OxideSingle crystals of HgPb2O2Cl2 were grown in a HgCl2 flux by reaction of PbO with HgCl2. Crystal structure analysis by single crystal X-ray methods were carried out. HgPb2O2Cl2 crystallizes monoclinic with a = 11.788(2) Å, b = 3.910(1) Å, c = 7.749(2) Å, β = 122.64(3)°, space group C2/m (No. 12) and Z = 2. HgPb2O2Cl2 is the first member of a new structure type, closely related to the structure of PbO.
    Notes: Einkristalle von HgPb2O2Cl2 wurden durch Umsetzung von PbO und HgCl2 in HgCl2-Schmelzen gezüchtet. An ihnen wurde der Aufbau mittels Einkristallröntgenstrukturanalyse bestimmt. HgPb2O2Cl2 kristallisiert monoklin mit a = 11,788(2) Å, b = 3,910(1) Å, c = 7,749(2) Å, β = 122,64(3)°, Raumgruppe C2/m (Nr. 12) und Z = 2. HgPb2O2Cl2 ist der erste Vertreter eines neuen Strukturtyps, der kristallchemisch von der Struktur von PbO ableitbar ist.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200604
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  • 200
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    Eu3+ und Eu2+ in Oxometallaten der Zusammensetzung MBeLn2O5: SrBeEu2O5 und EuBeNd2O5 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1033-1036 
    Details
    ISSN: 0044-2313
    Keywords: Strontium, europium, beryllium, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Eu3+ and Eu2+ in Oxides of the Composition MBeLn2O5: SrBeEu2O5 and EuBeNd2O5Single crystals of (I): SrBeEu2O5 and (II): EuBeNd2O5 were prepared by CO2-LASER (I) in air and plasma torch (II) technique in H2 atmosphere. X-ray investigations led to orthorhombic symmetry, space group D2h16-Pnma; (I): a = 9.488, b = 7.156, c = 6.495 Å; (II): a = 9.534, b = 7.225, c = 6.544 Å, Z = 4. Sr2+ and Eu3+ as well as Eu2+ and Nd3+ are in statistical distribution within a Kagomé framework. Both compounds are discussed with respect to the monoclinic form of MBeLn2O5.
    Notes: Einkristalle von (I): SrBeEu2O5 und (II): EuBeNd2O5 wurden mit CO2-LASER- bzw. Plasmabrennertechnik an Luft bzw. unter H2-Atmosphäre dargestellt. Die röntgenographische Untersuchung führte zu orthorhombischer Symmetrie, Raumgruppe D2h16-Pnma, mit (I): a = 9,488, b = 7,156, c = 6,495 Å; (II): a = 9,534, b = 7,225, c = 6,544 Å, Z = 4. Sr2+ und Eu3+ sowie Eu2+ und Nd3+ besetzen in einem Kagomégerüst die Metallpositionen statistisch. Beide Verbindungen werden mit Blick auf die monokline Form von MBeLn2O5 diskutiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200614
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