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  • 1985-1989  (776)
  • 1910-1914
  • 1988  (776)
  • Inorganic Chemistry  (639)
  • Physical Chemistry  (137)
  • 1
    Electronic Resource
    Electronic Resource
    A novel oxygen induced reduction of α, β-unsaturated carbonyl compounds by benzeneselenol (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 115-117 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A novel oxygen induced reduction of α,β-unsaturated carbonyl compounds is discovered. The reduction of the carbon-carbon double bond of α,β-unsaturated carbonyl compounds by benzeneselenol was caused by an introduction of molecular oxygen into the reaction system. This reduction is likely to proceed via a radical chain pathway involving an SH2 type reaction between a phenylseleno radical and a 1,2-adduct of benzeneselenol to the carbonyl group of the α,β-unsaturated carbonyl compound to give an allylic radical which absracts a hydrogen atom from benzeneselenol to form the reduction product.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010207
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  • 2
    Electronic Resource
    Electronic Resource
    ESR studies of photochemical reaction of 2-methyl-3-acetylquinoxaline N,N′-dioxide(MAQO) (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 191-195 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The photochemical reaction of MAQO with various aromatic amines were studied by ESR. The results show that nitroxide radicals are stable productrs of the photooxidation of both diphenylamines and phenylamines. The photolyzed phenothiazine does not yield nitroxide as the final product, instead it gives the neutral radical as the stable final product.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010403
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  • 3
    Electronic Resource
    Electronic Resource
    Syntheses, spectroscopic characterization and electronic structure of cyclopropenylidene ligated platinum complexes (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 333-349 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: New series of platinum complexes of cyclopropenylidenes of the types of PtX2(CP)2 and trans-PtX(PBu3)2(CP) have been synthesized, where CP is di-t-butylcyclopropenylidene (BCP) or bis(diisopropylamino)cyclopropenylidene (ACP). The 13C-NMR chemical shifts, and 13C-195Pt coupling constants (1JPtC) for the complexes are discussed in comparison with those values derived from closely related series of compounds, trans-PtCl(PR3)2L; L — —CH3, —C6H5 and —C≡CBu-t. An excellent linear relationship through the origin was obtained between 1JPtC and the formal ‘s’ % character of the carbon directly bonded to Pt for the series trans-PtCl(PR3)2L in which the Pt—C bond is regarded as a pure σ-linkage, whereas 1JPtC deviates largely from this relationship when pπ—dπ bonding interaction possibly exists in the Pt—C bond. The NMR data suggest the strong nmr trans-influence of the cyclopropenylidenes and that in the Pt—CP bond the σ-interaction is appreciable but the π-interaction is negligible.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010604
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  • 4
    Electronic Resource
    Electronic Resource
    Masthead (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988) 
    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.610010301
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  • 5
    Electronic Resource
    Electronic Resource
    Photocyclization of N-Alkyl-N-(3-aryl-3-butenyl) ureas. Hydrogen transfer via charge transfer exciplexes in alkene photochemistry (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 123-131 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Photolysis of N-alkyl-N-(3-aryl-3-butenyl) ureas (1) in acetonitrile gave cyclization products, 3-aryl-3-methyl-pyrrolidines, in good yields, whereas irradiation of 1 in methanol afforded methanol adducts as well as the cyclization products. Both the reactions are singlet reactions, and the cyclization is presumed to proceed via 1,6-hydrogen transfer from exciplexes with charge transfer character.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010302
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  • 6
    Electronic Resource
    Electronic Resource
    The Effect of hydrophobic-lipophilic interactions on chemical reactivity. 12. Mechanistic investigations of NaCMA-catalyzed hydrolysis of esters (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 143-151 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The dependence of the catalytic efficiencies of sodium carboxymethylamylose (NaCMA) for the hydrolysis of N-lauryl-3-acetoxypyridinium iodide (1) and p-nitrophenyl dodecanoate (3) on its degree of substitution (D. S. = 0·00, 0·12, 0·18, 0·24, 0·29 and 0·35) and on the pH values of the solutions (pH = 7·32, 7·80, 8·10 and 9·30) have been studied. At fixed D. S. values, the observed hydrolysis rates of 1 and 3 increase with increasing concentrations of NaCMA and follow saturation kinetics. At fixed concentration of NaCMA, the rates increase with decreasing D. S. values until they reach maxima at D. S. = 0·00. Furthermore, at any D. S. value the catalytic efficiency increases with increasing pH values of the solutions. All these results indicate that the hydroxyl groups are actually the principal catalyzing groups.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010304
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  • 7
    Electronic Resource
    Electronic Resource
    Masthead (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988) 
    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.610010401
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  • 8
    Electronic Resource
    Electronic Resource
    Participation of beta carbon-silicon bonds in the development of positive charge in five-membered rings (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 169-178 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The development of positive charge β to silicon in a saturated five-membered ring has been studied in the cis- and trans-2-(trimethylsilyl)cyclopentyl trifluoroacetates. The cis substrate solvolyzes in 97% trifluoroethanol at 25° C about 5 times faster than the analogous six-membered ring, after correction for differences in ring strain. The trans substrate solvolyzes about 360 times more slowly than the analogous six-membered ring. These changes are in agreement with a hyperconjugative mechanism for interaction between the silyl group and the developing positive charge. The expected cosine-squared dependence of hyperconjugation on the Si—C—C—X dihedral angle suggests that the cis dihedral angle is reduced somewhat from the 60° in the six-membered ring, and the trans dihedral angle is reduced substantially from the 180° in the six-membered ring.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010307
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  • 9
    Electronic Resource
    Electronic Resource
    Acidities of radical cations derived from arylacetonitriles (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 209-223 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The equilibrium acidities of phenylacetonitrile, and 20 of its m- and p-substituted derivatives have been measured in Me2SO solution. Their pKa′s plot linearly with those of the corresponding anilines. Combination of the pKa′s of these acids with their oxidation potentials, Eox(HA), and those of their conjugate bases, Eox(A-), provide an estimate of the acidities of the corresponding radical cations. The pKHA+ values for ArCH2CN+., where Ar is Ph, 1- and 2-naphthyl, and 9-anthryl, are -32, -18·5, -17·5, and -11, respectively, compared to 21·9, 20·85, 20·65, and 19·8 for the corresponding ArCH2CN acids. Acidities of PhCH(Me)CN+., Ph2CHCN+., 9-CN-FlH+., and 9-CN-XnH+. are -33, -35, -25, and -27, respectively, compared to 23·0, 17·5, 8·3, and 13·6 for the corresponding acids from which they were derived. The homolytic bond dissociation energies (BDEs) for the benzylic C—H bonds in these arylacetonitriles, estimated by combining pKHA with Eox(A-), fall in the range of 69 kcal/mol for 9-CN-XnH to 82 kcal/mol for PhCH2CN. For GC6H4CH2CN+. radical cations the acidities are decreased, relative to G=H, when G is an electron donor substituent and increased when G is an acceptor. The BDEs of the benzylic C—H bonds in GC6H4CH2CN are weakened by up to 4 kcal/mol by para donors and strengthened by up to 1·2 kcal/mol by m- or p-acceptors. The significance of these changes in BDEs with regard to the use of σ. scales and the ΔAOP method for estimating substituent effects on radical stabilities is discussed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010405
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  • 10
    Electronic Resource
    Electronic Resource
    Oxygen-atom transfer chemistry of α-AZO hydroperoxides: Effect of competitive intramolecular hydrogen bonding and α-methyl substitution (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 259-265 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: 1-(Phenylazo)-1-(2-pyridyl)ethyl hydroperoxide, 1, 1-(phenylazo)-1-(2-furyl)ethyl hydroperoxide, 2, phenylazo(2-furyl)methyl hydroperoxide, 3, 1-(phenylazo)-1-(4-anisyl)ethyl hydroperoxide, 4, were synthesized in moderate yield by autoxidation of the phenylhydrazones in benzene. The ionic oxidation of benzyl methyl sulfide in benzene by 1-4 yielded the sulfoxide and the metastable α-azo hydroxides in essentially quantitative yield. The reaction was of the first order in α-azo hydroperoxide and sulfide, respectively. The relative reactivity series found was: 1(1.0) 〈4(1.4) 〈 phenylazo(4-anisyl)methyl hydroperoxide 5 (2·9) 〈2 (3·8) 〈 3 (9·6). α-Methyl substitution was found to slow the rate of oxygen-atom trasfer by a factor of 2 to 2.5. The low relative reactivity of 1 was opposite that expected based on electronic effects. Competitive intramolecular hydrogen bonding of the hydroperoxy proton to the pyridyl nitrogen in 1 accounted for the observed result.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010503
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  • 11
    Electronic Resource
    Electronic Resource
    Extrusions of dibromocarbene under neutral conditions (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 281-285 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The thermal and photochemical decompositions of 5 have been studied. Both reactions lead to CBr2 transfer in good to high yields. With the 2-pentenes as substrates, CBr2 transfer is stereospecific in the classical singlet carbene manner.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010506
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  • 12
    Electronic Resource
    Electronic Resource
    Homocub-1(9)-ene trapped (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 305-308 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Decomposition of the tosylhydrazone salts formed from cubyl carboxaldehyde and homocubanone, potential precursors of cubylcarbene (5) and homocubanylidene (6), leads in each case to products derived from 6. It is suggested that homocub-1(9)-ene (7) is the active ingredient in the formation of 6 from both precursors. The hydrazones formed from N-aziridylamines are useful photochemical sources of 6, and presumably other carbenes. Flash vacuum pyrolysis of the tosyl hydrazone salts and hydrazones at 600°C leads to indene.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010509
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  • 13
    Electronic Resource
    Electronic Resource
    Novel reactions of sterically protected fused 1,2,3-selenadiazole. A new aspect of reactivity of organoselenium intermediates (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 317-332 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Light- and heat-induced decompositions and reactions with nucleophiles of 6,6,8,8-tetramethyl-2-selena-3,4-diaza-7-oxabicyclo[3.3.0]octa- 1(5),3-diene have been studied. In contrast with the conversion to the cyclopentyne derivative (9), selenium containing intermediates (6a, 6b, and 7) were efficiently trapped using several reagents to give various kinds of organoselenium compounds. Of particular note is the isolation of a stable selenirane derivative (16) obtained by the cycloaddition of the photochemically generated selenirene intermediate (7) with furan. The character and reactivity of the intermediates are also discussed.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010603
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  • 14
    Electronic Resource
    Electronic Resource
    The solvatochromic equation and insight into chemical reactivity (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 359-362 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Reaction rates for solvolysis of a mustard analogue are accurately correlated by the solvatochromic equation without inclusion of a nucleophilicity term, and thus the equation is shown to reveal mechanistically significant information.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010606
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  • 15
    Electronic Resource
    Electronic Resource
    Masthead (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988) 
    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.610010501
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  • 16
    Electronic Resource
    Electronic Resource
    Concerning the weakness of intramolecular general acid catalysis in the hydrolysis of vinyl ethers. o-carboxy-α-methoxy-β,β-dimethylstyrene (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 247-257 
    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 hydrolysis of the aromatic vinyl ether o-carboxy-α-methoxy-β,β-dimethylstyrene was found to be accelerated 25-fold by ionization of its carboxylic acid group, but the effective molarity which may be calculated if all of this rate acceleration is ascribed to intramolecular general acid catalysis is only EM = 1 · 1 m. This is similar to the small effective molarities found before for intramolecular catalysis by carboxylic acid groups of aliphatic vinyl ethers, which shows that, unlike the situation in other intramolecular reactions, e.g. ketone enolization, the extra rigidity of aromatic over aliphatic systems does not improve the efficiency of intramolecular catalysis in vinyl ether hydrolysis.It is suggested that this behaviour is the result of reduced conjugation between the vinyl ether group and the aromatic ring in the transition state of the vinyl ether hydrolysis reaction, which retards the rate and offsets any improvement effected by increased rigidity of the aromatic system.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010502
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  • 17
    Electronic Resource
    Electronic Resource
    Synthesis of optically active 2,2′-diselenocyanato-1,1′-binaphthyl and its molecular structure. Hypervalent nature of divalent selenium atom in crystal state (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 179-184 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: 2,2′-Diselenocyanato-1,1′-binaphthyl(1), the first selenium-containing binaphthyl derivative, has been synthesized in optically active form the corresponding diamine by diazotization followed by the reaction with potassium selenocyanate. Its molecular structure is determined by X-ray diffraction method. It is revealed that selenium atoms have hypervalent penta-coordination in the crystal.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010308
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  • 18
    Electronic Resource
    Electronic Resource
    Ab initio Mo calculations on the rearrangements of 7-oxa-2-bicyclo[2.2.1]heptyl cations. The facile migration of acyl group in wagner-meerwein rearrangements (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 287-298 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Ab initio STO-3G and 6-31G minimized geometries of 5-oxo- (9), 6-oxo-7-oxabicyclo[2.2.1]hept-2-yl cation (12) and 7-oxabicyclo[2.2.1]hept-2-yl cation (15) were obtained. The energy barriers for their Wagner-Meerwein rearrangements to the more stable 5-oxo- (11), 6-oxo-3-oxabicyclo[2.2.1]hept-2-yl (13) and 3-oxabicyclo[2.2.1]hept-2-yl (17) cations, respectively, have been evaluated and compared with those calculated for the rearrangement of the 5-oxo (18) and 6-oxobicyclo[2.2.1]hept-2-yl cations (20). In agreement with experimental data, the ‘true migratory aptitude’ of an acyl group is higher than that of β-oxoalkyl group in competitive Wagner-Meerwein rearrangments that are ‘energetically unbiased’. The ease of the acyl group 1,2-shift toward an electron-deficient center is related to the electron-donating ability of the carbonyl group due to favorable n(CO) ↔ σ σ ↔ p(C+) hyperconjugative interaction.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010507
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  • 19
    Electronic Resource
    Electronic Resource
    Free radical chain reactions of ate complexes. Electron transfer processes 42 (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 299-303 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Iodide ion promotes the free radical reaction of isopropylmercury idide with bromotrichloromethane to yield isopropyl bromide with rate enhancement in the order of 104. The reaction involves electron transfer from i-PrHgI2- to the trichloromethyl radical in a long kinetic chain process. Iodide ion also promotes the free radical chain conjugate addition of tert-butylmercury chloride to α,β-unsaturated ketones, esters, phosphonate esters and sulfones. Competitive reactivity studies indicate that lithium di-tert-butylcuprates or tri-tert-butylzincates react with 2-cycloalkenones by a mechanism involving attack by tert-butyl radicals. No evidence for radical attack is observed for the corresponding n-butyl ate complexes of copper or zinc.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010508
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  • 20
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    Electronic Resource
    Effect of cosolvent additives on relative rates of photooxidation on semiconductor surfaces (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 103-114 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The effect of solvent additives on the course of TiO2 photocatalyzed oxygenation of α-methylstyrene has been studied. While the addition of small amounts of nonhalogenated alcohols to TiO2 powders suspended in acetonitrile was found to decrease the rate of photooxygenation, added halogenated alcohols increase the rate of reaction. In addition, the solvent additives affect the observed product distribution.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010206
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  • 21
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    Electronic Resource
    Oxygen induced reduction: Reaction of benzeneselenol with aromatic aldehydes in the presence of oxygen (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 119-121 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Reduction of aromatic aldehydes by benzeneselenol is found to be promoted by molecular oxygen to give corresponding alcohols in good yields. No reduction took place without oxygen.A free radical process involving SH2 reaction at the selenium atom is proposed where the phenylseleno radical attacks the selenium atom of selenohemiacetal, the adduct of benzeneselenol to aldehyde, to give the ketyl radical which then abstracts hydrogen from benzeneselenol. The intermediacy of selenohemiacetal is supported by a quantitative reduction of α-methoxybenzyl phenyl selenide, which is used as a model compound of the intermediate.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010208
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  • 22
    Electronic Resource
    Electronic Resource
    The effect of hydrophobic-lipophilic interactions on chemical reactivity. 11. The dependence of the wrapping-up capability of sodium carboxymethylamylose on its degree of substitution (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 133-141 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The dependency of the wrapping-up capability of sodium carboxymethylamylose (NaCMA) on its degree of substitution (D. S. = 0·00, 0·12, 0·18, 0·24, 0·29, 0·35 and 0·41) have been studied, using two guest species, iodine and cetyl-trimethylammonium bromide (CTAB). The λmax values of NaCMA-iodine helical inclusion complexes decrease with increasing D. S. values and the amounts of encapsulated iodine by NaCMA as measured by amperometric titrations also decrease with increasing D. S. values. With CTAB as the substrate, the largest number of binding sites, n, and the dissociation constants Kd have been determined by the method of surface tension versus the CTAB concentration plots. The results show that n decreases while Kd increases with increasing D. S. values. All these observations point to the fact that the wrapping-up capability of NaCMA decreases with increasing degrees of substitution. The results are discussed in terms of host-guest and host-solvent hydrophobic-lipophilic interactions as well as intramolecular hydrogen-bonding.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010303
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  • 23
    Electronic Resource
    Electronic Resource
    Reaction branching as a mechanistic alternative to tunneling in explaining anomalous temperature-dependencies of kinetic isotope effects (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 161-167 
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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 temperature-dependence of the kinetic isotope effects for branched reactions proceeding via a common intermediate has been simulated by calculations. It is shown that, under certain conditions, anomalously small isotope effects on the Arrhenius preexponential factors, as well as unusually large observed isotope effects, may originate from the branching.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010306
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    Non-planar structures of the pentafluoroallyl and 1,1-difluoroallyl anions (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 153-160 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The structures of the allyl anion (1) and two fluoro-substituted derivatives, perfluoro (2) and 1,1-difluoro (3) have been calculated by ab inito molecular orbital theory. Geometries were gradient optimized, and force fields and an MP-2 correlation correction were determined at stationary points. The calculations were done with a double zeta basis set augmented by d functions on carbon (DZ + Dc). Final self-consistent field (SCF) and MP-2 energy calculations were done with the DZ + Dc basis set augmented by diffuse functions. The ground state of 1 is the planar allyl anion (C2v). The rotation barrier in 1 is 21·1 kcal/mol at the MP-2 level. The cyclopropyl carbanion is 27·0 kcal/mol higher in energy at the MP-2 level. The perfluoroallyl anion is not planar, and the rotated structure is 25·7 kcal/mol more stable than the C2v structure at the MP-2 level. The lowest energy structure on the potential energy surface for 2 is the perfluorocyclopropyl carbanion which is 27·8 kcal/mol more stable than the C2v structure at the MP-2 level. The 1,1-difluoroallyl anion is also not planar. Here the most stable structure on the potential energy surface is the rotated allyl anion which is 8·3 kcal/mol more stable than the all-planar allyl anion structure.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610010305
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    Electronic Resource
    Electronic Resource
    Nonplanar phenyl ring and inverse order of solvolytic reactivity for tertiary benzylic substrates (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 241-245 
    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 solvolysis of l-aryl-l-phenyl-2,2-dimethylpropyl(1) p-nitrobenzoates and of aryldiphenylmethyl-p-nitrobenzoates (2) were measured in 80% acetone. An inverse order of reactivity, kp-CF3/km- CF3 〉 l was observed for 1 but not for 2. The X-ray crystallogoraphic study of the parent compounds, l,l-diphenyl-2,2-dimethylpropyl-p-nitrobenzoate (1b) and triphenylemethyl benzoate (3b), and of 2-phenyl-2-propyl-p-nitrobenzoate (4) indicated that in the highly congested system 1 both phenyl rings were nonplanar, whereas the phenyl rings in 3 and 4 were essentially planar.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010407
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  • 26
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    NMR studies on the restricted rotation of 1-[2-(1-phenyl) propyl]-2,5-dimethylpyrrole derivatives (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 185-190 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: From the 1H-NMR spectra of the various pyrrole compounds, 1-substituted 2,5-dimethylpyrroles having two substituent groups on the carbon adjacent to the nitrogen atom were found to be very much hindered compounds. 1-[(1-Substituted)-2-phenylethyl]-2,5-dimethylpyrroles showed the restricted rotation, and the phenyl group of the most stable conformer was in close proximity to the pyrrole group due to dipole interaction. These NMR observations were supported by force field conformational analysis.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010402
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    Electron spin resonance study on radicals stabilized by the σ-π captodative effect1 (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 197-207 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: ESR spectra of l-cyano-2-(trimethylsilyl)ethyl and related radicals were recorded. Temperature dependent ESR spectra of these radicals revealed that electron-releasing trimethylsilylmethyl and electron-withdrawing cyano groups synergetically functioned to stabilize the radical centers due to σ-π captodative effects.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010404
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    Acidities of benzyl phenyl sulfones and of the corresponding radical cations. Homolytic bond dissociation energies (BDEs) of α—C—H bonds in benzyl phenylsulfones (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 225-239 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The excellent linearity (R2 = 0·997) of a plot of pKa values for 17 m- and p-substituted benzyl phenyl sulfones, GC6H4CH2SO2Ph, vs. those for the corresponding arylacetonitrile, GC6H4CH2CN, demonstrates that substituent solvation and substituent solvation assisted resonance (SSAR) effects for p-CN, p-COPh, and p-SPh are nearly identical in these two substrates. The PhSO2 group in PhCH2SO2Ph increases the BDE of the α-C—H bond by 2 kcal/mol, relative to toluene. The α-C—H bonds in GC6H4CH2SO2Ph sulfones are stabilized by 1-2 kcal/mol by acceptor G′s (m-CN, p-CN, m-CF3, p-CF3), but weakened by 1 and 5 kcal/mol, respectively, by donors (p-OMe and p-NMe2). The GC6H4CH2SO2Ph+. radical cation with G = H has a pKHA+. = -25. Its acidity is increased when G is an acceptor by as much as 9 to 10 kcal/mol (G = 3-CN, 3-CF3, 4-CF3, 4-NO2), but is decreased when G is a donor by as much as 33 kcal/mol (G = NMe2). When G = 4-SPh the radical cation is stabilized, relative to G = H, by a larger amount (25 kcal/mol) than when G = 4-OMe (18 kcal/mol). Structural changes along the series PhCH2SO2Ph, 2-naphthyl-CH2SO2Ph, 9-anthryl CH2SO2Ph cause negligible changes in the acidities of these acids, but sizable decreases in the acidities of the corresponding radical cations. Introduction of a phenylsulfonyl group into the methyl group of 9-methylanthracene or the 9-position of fluorene or xanthene increase the BDEs by 3, 2, and 7 kcal/mol, respectively. These effects of PhSO2 groups are compared and contrasted with those of CN groups.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010406
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    Electronic Resource
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    The lone-pair orbitals of triaziridine (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 267-273 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The PE spectra of four stable bicyclic triaziridines with trifluoromethyl, methyl, phenyl, spirocyclopentane and spirocyclohexane substituents are measured. From a comparison of these experimental data with MNDO calculations the energies and the interactions of the nitrogen lone-pair orbitals were obtained. The trifluoromethyl group may be reliably simulated by a fluorine atom. The ionization potentials are unexpectedly high and so are the cyclovoltammetric anodic potentials. The MNDO valence electron densities are in agreement with the comparatively small differences in the chemical shifts of the differently substituted nitrogens of the triaziridine rings.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010504
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  • 30
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    2,3:5,6-bis(ethylenedithio)- and bis(trimethylenedithio)-N,N′- dicyanoquinonediimines as new electron acceptors (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 275-280 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: In order to examine the substituent effect of ethylenedithio and trimethylenedithio groups on electron acceptors, the two title compounds were prepared in one step from the corresponding quinones. These species behave as weak π-electron acceptors owing to the electronic and sterical effects of the fused groups. Only the bis(ethylenedithio) derivative formed a charge-transfer complex with tetrathiotetracene, which showed a moderate electric conductivity of 2·0 × 10-2 S cm-1. In addition, both species oxidized copper, sodium, and potassium iodides to give the corresponding deeply colored metal salts, most of which were semiconductive. The naphtho analogs were similarly studied, but hardly served as electron acceptors.
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610010505
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    Masthead (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988) 
    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.610010601
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  • 32
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    Photoinduced potentiometric response of poly(vinyl chloride)/spirobenzopyran/crown ether composite memberanes modified with urease (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 309-315 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Photoresponse of the poly(vinyl chloride) membranes, which contain spirobenzopyran and crown ether, covered with a urease layer was studied in the presence and absence of urea. In the absence of urea, UV light irradiation induced more than 160 mV of membrane potential change, whereas the photoresponse decreased with an increase in the concentration of urea in the solution. The effects of such operating variables as crown loading and pH and ionic strength in the aqueous phase on the potentiometric response were also elucidated in the presence of urea. The results were explicated using the fact that the local concentration on NH4+ and H+ ions changed as a result of the urease-catalyzed decomposition reaction of urea.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010602
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  • 33
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    Complex formation between 1,3,5-trinitrobenzene and 1,8-diazabicyclo-[5,4,0]-undec-7-ene (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 351-357 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The title reaction is an instance of a simple nucleophilic attack of neutral nitrogen on aromatic sp2 carbon. The kinetic data (obtained in dimethyl sulphoxide) are compared to the results reported by the literature for the same reaction of aliphatic amines. Some possible interactions (substrate/nucleophile, substrate/salt) preceding the attack of the nucleophile are discussed.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610010605
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    Structure of radical intermediates appearing in the grignard reaction of monoketones (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 21-27 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The structure of radical intermediates appearing in the reactions of MeMgBr with aromatic monoketones was investigated by using ESR and visible spectroscopy. Stable radical intermediates in the reacting solutions were assigned to the dimeric radical ion pairs.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010104
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    Circular dichroism of In-Situ trinuclear organotransition metal complexes with optically active ligands (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 33-38 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Several Cotton effects are developed within absorption bands of trinuclear organotransitionmetal complexes in the presence of acids, diols, amines and aminoalcohols even in the case of bulky substituents on nitrogen; with monohydroxy compounds no circular dichroism could be detected.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010106
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    Marcus-grunwald theory and the nitroalkane anomaly (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 29-31 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The Disparity reaction proposed in a recent application of Marcus-Grunwald theory to nitroalkane ionization is shown to put the reaction's transition state in an energy-diagram region where electronic rearrangement leads proton transfer, contrary to experimental evidence; it is suggested that addition of solvent reorganization to electronic rearrangement as the second reaction progress variable would remedy this situation.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010105
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    Reaction of triethylsilyl radical with sulfides, a laser flash photolysis study (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 39-46 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Triethylsilyl radical was generated by laser flash photolysis of a 1:1 (v/v) solution of triethylsilane and di-tert-butyl peroxide. The silicon centered radical was reacted with sulfides to give carbon centered radicals by displacement at sulfur. The carbon radicals were readily detected by their transient absorption spectra. The absolute rate of reaction of triethylsilyl radical with 9-fluorenylphenylsulfide, di-n-butylsulfide, di-sec-butyl sulfide, di-tert-butyl sulfide and di-n-butyl disulfide are 2.40 ± 0.12 × 108 M-1S-1, 1.1 × 107±0.89×106M-1S-1, 8.79± 0.73×106M-1S-1, 3.29±0.18×106 M-1S-1, and 3.41±0.09×108 M-1S-1, respectively.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010107
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    Editorial (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. ii 
    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.610010102
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    Masthead (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988) 
    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.610010101
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  • 40
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    Nucleophilic substitution at saturated carbon atoms. Mechanisms and mechanistic borderlines: Evidence from studies with neutral leaving groups (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 1-20 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Substrates with neutral leaving groups undergo unimolecular solvolysis in nonpolar solvents. Whereas t-alkyl substrates invariably solvolyze by a unimolecular mechanism, s-alkyl and primary alkyl substrates can undergo both uni and bimolecular reactions, and the bimolecular step can take place on either the substrate itself or on an intimate ion-molecule pair formed in either a pre-equilibrium or in a rate determining step. Study of reactions at borderlines indicates that the individual reaction types remain distinct and do not merge.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010103
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    Generation of α- oxo selenoaldehydes by treatment of α, α′ -diketo selenides with base (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 59-61 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Treatment of α, α′ -diketo selenides, which recently became readily obtainable, with base affords α-oxo selenoaldehydes and ketones. The seleno-carbonyl compounds thus formed are reactive transient species, but can be trapped by Diels-Alder reaction to give 3,6-dihydro-2H-selenapyran derivatives in moderate to good yields.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610010110
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    Ethenediylidene-2,2′ -bis(1,3-dithiole) and butatriene-1,4-diylidene-2,2′-bis(1,3-dithiole) (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 47-51 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: This paper describes the synthesis and electrochemical behavior of dicationic salts of ethenediylidene-2,2′ -bis(1,3-dithiole) (3) and butatriene-1,4-diylidene-2,2′ -bis(1,3-dithiole) (4). These are expected as donor components for developing organic conducting and superconducting materials, on the grounds of high electron donating ability and of rigid skeletal structure with two and four cumulenic carbons inserted between two 1,3-dithioles. These salts were obtained in good overall yields by several steps starting from (2-morpholino-4,5-dimethyl or -diphenyl)-1,3-dithiolylium salt. From the 1H and 13C NMR, and electronic spectra it is suggested that the π conjugation between two 1,3-dithiolylium ions through an acetylenic bond is less effective than that through an olefinic bond of the corresponding salts of ethanediylidene-2,2′ -bis(1,3-dithiole) (1) and 2-butene-1,4-diylidene-2,2′-bis(1,3-dithiole) (2). The cyclic voltammetric study shows that the corresponding radical cations, and in particular 3 and 4, are less stable even at -40°C, thus providing reasons for our current lack of success in isolation of 3 and 4. From comparison of the first redox potentials of neutral species, it is deduced that the donating ability increases in the order of TTF 〈 1 ⋍ 2 ≲ 3 ≪ 4.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010108
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    Reaction of sulfur ylides with elemental sulfur and selenium. Aspects and mechanistic considerations (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 53-57 
    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 sulfur ylides with elemental sulfur or selenium initially affords thio- or seleno-carbonyl compounds, which then react with starting ylides to give episulfides or episelenides from which the heteroatom (sulfur or selenium) is extruded to give olefins as the final product. In the case of carbonyl-stabilized ylides, the resulting thio- or seleno-carbonyl compounds react with starting ylides to afford 1,3-oxathioles or 1,3-oxaselenoles as previously reported. Supporting evidence for the intermediacy of thio(seleno)-carbonyl compounds and episulfides (episelenides) is presented.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/poc.610010109
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    Masthead (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988) 
    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.610010201
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  • 45
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    Study on 5, 15-dialkylporphyrins interconversion between two conformers in solution (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 63-73 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Novel structural features of 5, 15-dialkylporphyrins in solution are described. The 1H-NMR spectra of these compounds showed broad signals at room temperature, which split into two sets of signals at lower temperatures. This unusual phenomenon was ascribed to a dynamic interconversion between tow distorted structures. The 5, 15-dialkylporphyrin has a distorted ring due to the steric hindrance between the 5(or 15)-alkyl group and the 3, 7(or 13, 17)-alkyl groups and, depending on the position of the 5, 15-alkyl groups relative to the average ring plane, can exist in two conformations; syn (where the two alkyl groups are on the same side of the ring plane) and anti (on the opposite sides). Preliminary kinetic study of this interconversion using the NMR line shape analyses is also reported.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010202
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  • 46
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    Thiophilic reactions of 2,4,6-tri-t-butylphenyllithium with carbon disulfide and thiophosgene (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 75-81 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Highly sterically demanding 2,4,6-tri-t-butylphenyllithium (1) reacts with carbon disulfide to give 1,2-dibutylthio-1,2-bis(2,4,6-tri-t-butylphenylthio) ethene (3), l-butylthio-1-(2,4,6-tri-t-butylphenylthio)pent-l-ene (4), and 2-butylthio-3-(2,4,6-tri-t-butylphenylthio)-1,3-dithiole-2-thione (5) when 1 is prepared by the reaction of 1-bromo-2,4,6-tri-t-butylbenzene with n-butyllithium. When the reaction is carried out using 1 prepared from 2 and t-butyllithium and then quenched with l-iodoethane, 2-ethylthio-3-(2,4,6-tri-butylphenylthio)-1,3-dithiole-2-thione and 1,2-diethylthio-1,2-bis(2,4,6-tri-t-butylphenylthio) ethene are produced. The formation of all these products can be explained in terms of initial thiophilic attack of 1 on the sulfur of carbon disulfide and an intermediate with a dual property of carbanion and carbene (i.e., ArSC(Li)(=S) ⇌ ArSC̈SLi) is suggested. The reaction of 1 with thiophosgene affords 1,2-dichloro-1,2-bis(2,4,6-tri-t-butylphenylthio) ethene, bis(2,4,6-tri-t-butylphenylthio)acetylene, and 1-chloro 2,4,6-tri-t-butylbenzene, the first two of which are explained to be formed by thiophilic attack of 1 with thiophosgene.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010203
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    Intramolecular orientation at the micellar interface: Control of norrish type I and type II reactivity of benzoinalkylethers via conformational effects (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 91-102 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The photolysis of benzoinalkylethers 1-5 solubilized in detergents show a significant deviation from the course of reaction in isotropic organic solvents. Remarkable difference in photobehaviour is noticed between the short chain (1-3) and the long chain (4 and 5) benzoinalkylethers in the micellar media. However, the influence of the micellar media on the photobehaviour of alkyldeoxybenzoins 6 and 7 was small. The importance of ‘cage effect’ in controlling the product distribution was evident from its dependence on the micellar size and on the occupancy number. More importantly, a comparative analysis of the photobehaviour of the ketone 1-7 reveals that the micellar interface can be used to control the conformations of organic molecules.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/poc.610010205
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  • 48
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    Theoretical studies on the acylation reactions of ammonia by ketenes: Determination of reactivity by molecular orbital theory (part 54) (1988)
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 1 (1988), S. 83-90 
    Details
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Theoretical studies on the reactions of ammonia with ketene and dimethylketene using the MNDO method are reported. The single step addition of ammonia to the olefinic bond of ketenes was found to provide a lower energy-barrier path than the two step carbonyl addition mechanism. The barrier height was lower in the reaction of keten compared with that of dimethylketene in support of the faster rate of solution phase reactions of aniline and ketenes. The deformation energies of reactants had an overwhelming influence in determining the activation barriers in all the reactions investigated.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/poc.610010204
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  • 49
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    Zur Kenntnis von Alkalimetaselenoarseniten Darstellung und Kristallstrukturen von MAsSe2, M = K, Rb, Cs (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 561 (1988), S. 139-148 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Concerning Alkali Metal Metaselenoarsenites. Preparation and Crystal structures of MAsSe2, M = K, Rb, CsThe metaselenoarsenites MAsSe2, M = K, Rb, Cs were prepared by methanolothermal reaction of M2CO3 with As2Se3 at a temperature of 130°C. Their X-ray structural analyses demonstrated that the compounds contain polymetaselenoarsenite anions [AsSe2-]∞, in which the basic units are ψ-AsSe3 tetrahedra, which are linked via shared corners into infinite chains. Vierer single chains are observed for KAsSe2 and RbAsSe2, zweier single chains for CsAsSe2. The stretching units s are respectively 3,157, 2.336 and 3,378 Å. The relationship between the conformation of metaselenoarsenite chains and cation size is discussed.
    Notes: Die Metaselenoarsenite MAsSe2, M = K, Rb, Cs wurden durch methanolothermale Reaktion von M2CO3 mit As2Se3 bei einer Temperatur von 130°C dargestellt. Ihre Röntgenstrukturanalysen ergaben, daß die Verbindungen Polymetaselenoarsenit-Anionen [AsSe2-]∞ beinhalten, in denen die Grundelemente ψ-AsSe3-Tetraeder sind, die über gemeinsame Ecken zu unendlichen Ketten verknüpft sind. Für KAsSe2 und RbAsSe2 werden Vierer-, für CsAsSe2 Zweier-Einfachketten gefunden. Die Streckungseinheiten s betragen 3,157, 2,336 bzw. 3,378 Å. Die Beziehung zwischen Konformation von Metaselenoarsenitketten und Kationgröße wird erläutert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885610115
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  • 50
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    Study on A4BX6 Compounds. II [1]. Refinement of the Structure of Rb4PbBr6 and a Note on the Existence of “Rb4Hgl6” and “K4CdI6” (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 102-104 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Untersuchungen an A4BX6-Verbindungen. II. Strukturverfeinerung von Rb4PbBr6 und eine Bemerkung zur Existenz von „Rb4HgI6“ und „K4CdI6“Rb4PbBr6 wurde in einer Festkörperreaktion aus den binären Komponenten präpariert und die Struktur mit Einkristalldaten verfeinert (a = 1332,9(4), c = 1647,8(5) pm, R.Gr. R3c; K4CdCl6-Typ). Rb4HgI6 und K4CdI6 ließen sich nicht darstellen. Diese Ergebnisse werden im Zusammenhang mit dem Strukturfelddiagramm für A4BX6 Verbindungen diskutiert.
    Notes: Rb4PbBr6 was prepared by solid state reaction of the binary compounds and the structure refined with single crystal data (a = 1332.9(4), c = 1647.8(5) pm; space group R3c; K4CdCl6-type arrangement). Attempts to synthesize Rb4HgI6 and K4CdI6 were unsuccessful. The results are discussed on the basis of a structure field diagram for A4BX6 compounds.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19885620112
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  • 51
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    Die Kristallstruktur von Pb5(GeO4)2SO4 und Pb5(GeO4)2CrO4, zweier Bleiapatite mit unbesetzten Halogenlagen (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 131-140 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of Pb5(GeO4)2SO4 and Pb5(GeO4)2CrO4, Two Lead Apatites with Vacant Halogen SitesPb5(GeO4)2SO4 (a = 1005.8; c = 741.6 pm) and Pb5(GeO4)2CrO4 (a = 1010.5; c = 742.8 pm) are hexagonal, space group P63/m, Z = 2 formula units. They crystallize with the apatite structure type. The halogen positions in the channels are not occupied. This pecularity is caused by the Pb2+ ions on the 6h positions. Their lone pairs of electrons are sterically active, being directed into the channels. The electron lone pairs of the Pb2+ ions of the 4f positions also show sterical effect.
    Notes: Pb5(GeO4)2SO4 (a = 1005,8; c = 741,6 pm) und Pb5(GeO4)2CrO4 (a = 1010,5; c = 742,8 pm) sind hexagonal, Raumgruppe P63/m, Z = 2 Formeleinheiten. Sie kristallisierten in der Apatitstruktur, wobei die Halogenlagen in den Kanälen nicht besetzt werden. Diese Besonderheit ist durch die Pb2+-Ionen auf der Lage 6h bedingt. Ihre freien Elektronenpaare sind stereochemisch wirksam und weisen in die Kanäle hinein. Auch bei den Pb2+-Ionen auf der Lage 4f ist ein stereochemischer Einfluß des freien Elektronenpaares erkennbar.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885620116
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    Study on A4BX6 Compounds. III [1]. ns2 cations as a prerequisite for a structure type and their interaction in ternary halides with the formula type A4BX6 (A: In, TI; B: Cd, Pb, Ge; X: Cl, Br, I) (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 105-114 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Untersuchungen an A4BX6-Verbindungen. III. ns2-Kationen als Bedingung für einen Strukturtyp und ihre Wechselwirkung in ternären Halogeniden vom Typ A4BX6 (A: In, Tl; B: Cd, Pb, Ge; X: Cl, Br, I)Wir diskutieren die Art der Wechselwirkung von Kationen mit ns2-Konfiguration in ternären Halogeniden des Formeltypes A4BX6 (A: In, Tl; B: Cd, Pb, Ge; X: Cl, Br, I), die im Tl4HgBr6-Typ kristallisieren. Wir berichten über Hochdruckexperimente 'an solchen A4BX6-Verbindungen und über röntgenographische Untersuchungen und Kristallstrukturverfeinerungen an Mischkristallen des Typs A′xA4-xBX6, in denen die ns2-Kationen teilweise durch solche mit Edelgaskonfiguration substituiert sind. Die Ergebnisse unserer Experimente zeigen, daß die ns2-Kationen diesen ungewöhnlichen Strukturtyp durch Polarisationseffekte stabilisieren und durch ihre größere Elektronegativität im Vergleich zu der von Alkaliionen von ähnlicher Größe.
    Notes: We discuss the interaction of ns2-type cations in ternary halides of the formula type A4BX6 (A: In, Tl; B: Cd, Pb, Ge; X: Cl, Br, I) crystallizing in a Tl4HgBr6-type arrangement. We report on high pressure experiments on such A4BX6 compounds and on x-ray studies and structure refinements of mixed crystals of the type A′xA4-xBX6, where cations A′ with a closed shell configuration partly substitute for the ns2-type A ions. The results of our experiments show, that ns2-type cations stabilize this unusual structure type by polarization effects and by their higher electronegativity as compared with alkali ions of comparable size.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885620113
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  • 53
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    Ag2PdCl4, Kristallstruktur und die kristallchemische Beziehung zum NaCl-Typ (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 123-130 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ag2PdCl4, Crystal Structure and the Crystal Chemical Relation to the NaCl TypeAg2PdCl4 single crystals show orthorhombic symmetry with the space group Cmca (No. 64) and the lattice parameters a = 10.088(2), b = 8.051(5), c = 8.078(2) å, with 4 formular units per unit cell. The atomic arrangement of Ag2PdCl4 is explored by X-ray crystal structure analysis.Silver shows a distorted octahedral arrangement of chlorine atoms. Palladium forms typical, approximately square-planar PdCl4 groups. Ag2PdCl4 is a new variant of a partially occupied sodium chloride structure type.
    Notes: Die Kristallstruktur von Ag2PdCl4 wurde mit röntgenographischen Methoden an Einkristallen ermittelt. Ag2PdCl4 kristallisiert mit orthorhombischer Symmetrie: Cmca (No. 64), a = 10,088(2), b = 8,051(5), c = 8,078(2) å mit 4 Formeleinheiten pro Elementarzelle.Silber besitzt eine verzerrt oktaedrische Chlor-Nachbarschaft, während das Palladium annähernd quadratisch planare PdCl4-Gruppen bildet. Ag2PdCl4 stellt eine neue Variante einer teilbesetzten Natriumchloridstruktur dar.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885620115
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  • 54
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    Zum Einfluß der Halogenmodifizierung auf das acide Verhalten von γ-Al2O3 (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 145-152 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Influence of Modification of γ-Alumina by Halides on the Acidic BehaviourThe influence of modification of γ-alumina by Cl and F on the acidic properties was studied by means of i.r. spectroscopic methods using ammonia as probe molecule. The measurements show a significant rise in Lewis acidity.
    Notes: Mittels IR-spektroskopischer Methoden wurde der Einfluß der Halogen-modifizierung auf das acide Verhalten von γ-Al2O3 im Hinblick auf dessen Verwendung als Träger in Reformingkatalysatoren untersucht. Als Sondenmolekül diente NH3. Die Messungen wiesen eine deutliche Verstärkung der Lewis-aciden Eigenschaften des modifizierten Al2O3 aus.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885620118
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    27Al N.M.R. Studies on the Liquid Phases during Zeolite Synthesis (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 141-144 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 27Al-NMR-Untersuchungen der flüssigen Phasen während der Zeolithsynthese27Al-NMR-Untersuchungen der während der Synthese der Zeolithe A, X und Y vorliegenden flüssigen Phasen zeigen, daß der molekulare Aufbau und die Menge der in den wäßrigen Lösungen vorliegenden Alumosilicationen für den entstehenden Zeolithtyp charakteristisch ist. Die Zahl der gebildeten Si—O—Al-Bindungen und ihre Mannigfaltigkeit steigt mit steigendem SiO2-Gehalt der Lösungen. Diese Ergebnisse stützen die Vorstellung, daß die Synthese von Zeolithen unter Ausbildung definierter Alumosilicate über die Lösungsphase abläuft.
    Notes: 27Al n.m.r. spectroscopy of liquid phases obtained during zeolite A, X, and Y synthesis reveals that the amount and the type of the present soluble aluminosilicate anions is characteristic for the different zeolite type; the number of the formed Si—O—Al bonds and their variety increases with increasing content of SiO2. The results support the suggestion about the formation mechanism of zeolites via distinct aluminosilicate “precursors” in solution.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885620117
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  • 56
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    Über Chalkogenolate. 186 [1]. Untersuchungen über Salze der Pyruvinsäure 1. Darstellung und Charakterisierung von Pyruvaten (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 160-164 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 186. Studies on Salts of Pyruvic Acid. 1. Synthesis and Characterization of PyruvatesThe title compounds M[O2C—CO—CH3], where M = Na, K, NH4, Li = H2, Have been synthesized by neutralisation of pyruvic acid under different conditions.The pyruvates were characterized by means of electron absorption, infrared, nuclear magnetic resonance, and mass spectra.
    Notes: Die Titelverbindungen M[O2C—CO—CH3] mit M = Na, K, NH4, Li · H2O wurden durch Neutralisation der Pyruvinsäure unter verschiedenen Bedingungen synthetisiert.Die Charakterisierung der Pyruvate erfolgte mit Hilfe von Elektronenabsorptions-, Infrarot-, Kernresonanz- und Massenspektren.
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19885620120
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    Beiträge zur Chemie der Silicium-Schwefel-Verbindungen. 52 [1]. Reaktion von Trialkoxysilanthiolen mit Carbonsäuren. Darstellung und Hydrolyse der Trialkoxyacyloxysilane (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 153-159 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Silicon-Sulphur Compounds. 52. Reaction of Trialkoxysilanethiols with Carboxylic Acids. Preparation and Hydrolysis of TrialkoxyacyloxysilanesThe series of trialkoxyacyloxysilanes have been prepared almost quantitatively from trialkoxysilanethiols (RO)3SiSH (R = i-Pr, s-Bu, s-n-Am, s-i-Am) by the reaction with carboxylic acids R′COOH (R′ = Alkyl or Ph). Kinetics of the acidolysis of (RO)3SiSH as well as hydrolysis of (RO)3SiOCOR′ were investigated and consequently the reaction mechanisms are proposed.
    Notes: Durch Umsetzung von Trialkoxysilanthiolen (RO)3SiSH (R = i-Pr, s-Bu, s-n-Am, s-i-Am) und Carbonsäuren R′COOH (R′ = Alkyl bzw. Ph) wurden fast quantitativ mehrere Trialkoxyacyloxysilane (RO)3SiOCOR′ erhalten. Die Kinetik dieser Acidolysereaktion von (RO)3SiSH wie auch der Hydrolysereaktion von (RO)3SiOCOR′ wurde untersucht und in der Folge die Reaktionsmechanismen formuliert.
    Additional Material: 4 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19885620119
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    Zur Kenntnis von Na6Cu2O6 (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 79-86 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Knowledge of Na6Cu2O6For the first time black single crystals of Na6Cu2O6 are obtained with a = 1094.8(1), b = 1203.6(1), c = 1638.1(2) pm, space group Cmca, Z = 12. Cu3+ is coordinated by four O2-. CuO4 groups are bound to planar, isolated Cu2O66- anions. Cu—O bond distances are between 181.6(3) and 186.4(4) pm and O—Cu—O bond angels in the range 84.0(1)° and 93.7(1)°. Effective Coordination Numbers, ECoN, Mean Fictive Ionic Radii, MEFIR, and the Madelung Part of Lattice Energy, MAPLE, are calculated.
    Notes: Erstmals wurden schwarze Einkristalle von Na6Cu2O6 mit a = 1094,8(1), b = 1203,6(1), c = 1638,1(2) pm, R. Gr. Cmca, Z = 12 dargestellt. Cu3+ ist planar von vier O2-umgeben. Je zwei CuO4-Gruppen sind zu planaren, isolierten Anionen Cu2O66- verknüpft. Die Abstände Cu—O liegen zwischen 181,6(3) und 186,4(4) pm, die Winkel O—Cu—O zwischen 84,0(1)° und 93,7(1)°. Die Effektiven Koordinationszahlen, ECoN, Mittleren Fiktiven Ionenradien, MEFIR, und der Madelunganteil der Gitterenergie, MAPLE, wurden berechnet.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885630112
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    Synthese, IR- und EPR-Spektren sowie die Kristallstruktur von HPPh3[WOCl4(OPPh3)] (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 70-78 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, I.R. and E.P.R. Spectra, and Crystal Structure of HPPh3[WOCl4(OPPh3)]Partial hydrolysis of the alkyne complex [WCl4(PhC≡CPh)]2 in the presence of triphenylphosphine and dichloromethane as oxidizing agent and solvent yields dark green crystals of the complex HPPh3[WOCl4(OPPh3)]. Attempts to prepare the compound directly by the reaction of WOCl3 with PPh3, OPPh3 and HCl in dichloromethane were unsuccessful.HPPh3[WOCl4(OPPh3)] was characterized by its i.r. and e.p.r. spectrum. As shown by a crystals structure determination (1835 independent, observed reflections, R = 0.056) the complex crystallizes monoclinically in the space group P21/n with four formula units per unit cell. The complex consists of HPPh3+ and [WOCl4(OPPh3)]- ions, in which the tungsten atom is in a distorted octahedral environment, surrounded by four equatorial chlorine atoms, by one axial oxygen atom (bond length WO = 172 pm), and by the oxygen atom of the OPPh3 molecule (WO = 206 pm).
    Notes: HPPh3[WOCl4(OPPh3)] entsteht in Form dunkelgrüner Kristalle bei der partiellen Hydrolyse des Diphenylacetylenkomplexes [WCl4(PhC≡CPh)]2 bei Anwesenheit von Triphenylphosphan und Dichlormethan als Oxidations- und Lösungsmittel. Versuche, die Verbindung aus WOCl3, PPh3, OPPh3 und HCl in Dichlormethan direkt herzustellen, mißlangen.HPPh3[WOCl4(OPPh3)] haben wir durch das IR- und das EPR-Spektrum charakterisiert. Nach der röntgenographischen Strukturanalyse (1835 unabhängige, beobachtete, beobachtete Reflexe, R = 5,6%) kristallisiert die Verbindung monoklin in der Raumgruppe P21/n mit vier Formeleinheiten pro Elementarzelle. Sie ist aus HPPh3+-Ionen und Anionen [WOCl4(OPPh3)]- aufgebaut, in denen das Wolframatom verzerrt oktaedrisch von vier äquatorial angeordneten Chloratomen und axial von einem terminalen O-Atom (Bindungsabstand WO = 172 pm) und von dem O-Atom des OPPh3-Moleküls (WO = 206 pm) umgeben ist.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885630111
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    Komplexbildung mit sulfonamidsubstituierten Thionoliganden (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 105-115 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complex Formation by Sulfonamide Substituted ThionoligandsThionoligands containing arenesulfonamido or arenesulfonylhydrazido functions as a second donor group (STAT-, PST-, BPTS- and TPTH-, meaning of the abbreviations see text) form 1,2 complexes with nickel(II), cobalt(II), and zinc(II). The six-membered chelates M(STAT)2 (M = Co, Ni) are high-spin (\documentclass{article}\pagestyle{empty}\begin{document}$ \rm{S} \mathop {\rm N}\limits^ \ominus $\end{document} coordination). On the other hand no coordination of the RSO2N group is observed in the complexes M(PST)2 (M = Co, Mn, Fe), but the formation of a four membered ring including one nitrogen atom of the heterocycle. This statement is primarily based on a comparison with complexes of teh structurally related ligands PPT- and CPT- containing no \documentclass{article}\pagestyle{empty}\begin{document}$ \rm{RSO}_2 \mathop {\rm N}\limits^ \ominus $\end{document} groups. Evidently in the chelat Co(BPTS)2 the anionic RSO2N group is a weak bidentate donor.
    Notes: Thionoliganden, die Arensulfonylamido- bzw. Arensulfonylhydrazidofunktionen als zweite Donatorgruppen enthalten (STAT-, PST-, BPTS- und TPTH-, zur Bedeutung der Abkürzungen vgl. Text), bilden mit Nickel(II), Cobalt(II) und Zink(II) 1,2-Komplexe. Die Sechsringchelate M(STAT)2 (M = Co, Ni) gehören zum High-spin-Typ (\documentclass{article}\pagestyle{empty}\begin{document}$ \rm{S} \mathop {\rm N}\limits^ \ominus $\end{document})-Koordination. Dagegen erfolgt in den Komplexen M(PST)2 (M = Co, Mn, Fe) keine Koordination über die \documentclass{article}\pagestyle{empty}\begin{document}$ \rm{RSO}_2 \mathop {\rm N}\limits^ \ominus $\end{document} Funktionen sondern über ein Stickstoffatom des Pyrimidinrings (Bildung eines Chelatvierringes). Diese Aussage wird durch einen Vergleich mit Komplexen der strukturell verwandten Liganden PPT- und CPT- gestützt, die keine RSO2N-Gruppen enthalten. In dem Chelat Co(BPTS)2 koordiniert RSO2N- offenbar als zweizähliger anionischer Ligand mit schwacher Donatorwirkung. Die Charakterisierung der neuen Chelate erfolgt anhand der magnetischen Momente, der UV/VIS- und der ESCA-Spektren. Die vorliegenden und früheren Ergebnisse ermöglichen Aussagen über die Variabilität des RSO2N-Liganden: Normalerweise erfolgt die Koordination über den N-Ligator. Es ist aber auch eine Bindung über ein Sauerstoffatom, wenn dadurch ein stabiler Chelatsechsring gebildet werden kann, oder als zweizähliger anionischer Ligand geringer Donatorstärke möglich. Die art der Koordination des RSO2N-Liganden hängt vom Zentralatom ab. Bisher konnten keine Komplexe mit einer direkten koordinativen Bindung von \documentclass{article}\pagestyle{empty}\begin{document}$ \rm{RSO}_2 \mathop {\rm N}\limits^ \ominus $\end{document} an Eisen(II) oder Mangan (II) nachgewiesen werden.
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    Synthese und Strukturuntersuchungen von Iodocupraten(I). IX. Synthese und Kristallstrukturen von Cs3Cu2I5 und RbCu2I3 (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 96-104 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Structure Analyses of Iodocuprates (I). IX. Syntheses and Crystal Structures of Cs3Cu2I5 and RbCu2I3Cs3Cu2I5 and Rb∞1[Cu2I3] were prepared by the reaction of CsI or RbI with CuI in solution (acetonitrile or acetone) or by solid state reaction. The crystal structure analysis of Cs3Cu2I5 (orthorhombic, Pbnm, a = 1438.6(6), b = 1014.7(5), c = 1167.5(5) pm, Z = 4) shows, that the compound contains dinuclear anions Cu2I53- in which the I atoms are arranged to trigonal bipyramids; one CuI occupies one of the two I tetrahedral holes, the other a trigonal site of the neighbouring tetrahedron. Rb∞1[Cu2I3] (orthorhombic, Cmcm, a = 1070.6(7), b = 1338.3(8), c = 572.8(3) pm, Z = 4) is built up by CuI4 double chains; the compound is isomorphic with Cs∞1[Cu2I3].
    Notes: Cs3Cu2I5 und Rb∞1[Cu2I3] werden durch Umsetzung von CsI bzw. RbI mit CuI in Lösung (Acetonitril bzw. Aceton) oder durch Festkörperreaktion hergestellt. Die Kristallstrukturanalyse von Cs3Cu2I5 (orthorhombisch, Pbnm, a = 1438,6(6), b = 1014,7(5), c = 1167,5(5) pm, Z = 4) ergab, daß diese Verbindung zweikernige Anionen Cu2I53- enthält. Die Iodatome bilden eine trigonale Bipyramide mit einem CuI in einer der beiden Tetraederlücken. Das zweite CuI besetzt eine Dreiecksfläche des anderen Tetraeders. Im Rb∞1[Cu2I3] (orthorhombisch, Cmcm, a = 1070,6(7), b = 1338,3(8), c = 572,8(3) pm, Z = 4) liegen CuI4-Tetraederdoppelketten vor; die Verbindung ist isomorph mit CsCu2I3.
    Additional Material: 3 Ill.
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    Über Chalkogenolate. 187. Untersuchungen über Salze der Pyruvinsäure 2. Kristallstruktur von Kaliumpyruvat, Neubestimmung der Struktur von Natriumpyruvat (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 87-95 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 187. Studies on Salts of the Pyruvic Acid. 2. Crystal Structure of Potassium Pyruvate, Redetermination of the Structure of Sodium PyruvateThe title compounds M[O2C—CO—CH3], where M = Na and K, crystallize with Z = 4 in the monoclinic space group P21/n; cell dimensions see “Inhaltsübersicht”.The structure of the Na+ and K+ salt resp. has been determined from single crystal X-ray data measured at 20°C and refined to R's of 0.051 and 0.055 resp. (Rw = 0.055 and 0.057 resp.) for 1065 and 1308 resp. independent reflections.Both compounds are isostructural. The alkali metal ions are surrounded by seven oxygen atoms from five anions forming an irregular polyhedron.
    Notes: Die Titelverbindungen M[O2C—CO—;CH3] mit M = Na, K kristallisieren monoklin mit Z = 4 in der Raumgruppe P21/n; Na[O2C—CO—CH3] a = 21, 905(3) Å, K[O2C—CO—CH3] a = 22,027(2) Å, b = 5,269(1) Å, b = 5,835(2) Å, c = 3,671(1) Å, c = 4,004(4) Å, β = 91,34(2)°. β = 90,88(3)°. Für die Na+-bzw. K+-Verbindung wurde die Struktur aus bei 20°C vermessenen röntgenographischen Einkristalldaten unter Verwendung von 1065 bzw. 1308 symmetrieunabhängigen Reflexen bestimmt und bis auf Gütefaktoren von R = 0,051 bzw. 0,055 und Rw = 0,055 bzw. 0,057 verfeinert.Beide Verbindungen sind isostrukturell. Das jeweilige Alkalimetallion ist von sieben O-Atomen, die von fünf verschiedenen Anionen stammen, unregelmäßig koordiniert.
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    Untersuchungen an oxidischen Katalysatoren. XLV. Umwandlung von Aromaten an dealuminierten ZSM-5-Zeolithen (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 127-135 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Oxide Catalysts. XLV. Conversion of Aromatics on Dealuminated Zeolites ZSM-5The catalytic properties of zeolites ZSM-5 dealuminated by hydrochloric acid are investigated in the isomerization of m-Xylene, the disproportionation of toluene and in the alkylation of toluene with methanol. Besides the increase of the Si/Al ratio, the dealumination leads to an inversion of the Si/Al concentration gradient in crystallites, to a shift of acidity spectrum and consequently to a change in catalytic activity and selectivity.
    Notes: An säuredealuminierten HZSM-5-Proben werden die m-Xylen-Isomerisierung, die Toluendisproportionierung und die Toluenalkylierung mit Methanol untersucht. Die Säuredealuminierung bewirkt neben der Moduländerung eine Umkehr des Si/Al-Konzentrationsgradienten in den Zeolithkristalliten, eine Verschiebung des Aciditätsspektrums und damit eine Veränderung von Aktivität und Selektivität in den katalytischen Reaktionen.
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    URL: http://dx.doi.org/10.1002/zaac.19885630117
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    Imidodiphosphorsäuretetraphenylester als Ligand in Fluorokomplexen. 1. Fluorokomplexe des Titans (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 167-172 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetraphenyl Imidodiphosphate as Ligand in Fluoro Complexes. 1. Fluoro Complexes of TitaniumIn acetonitrile TiF4 reacts with tetraphenyl imidodiphosphate forming two tetrafluoro (I, II) and three trifluoro complexes (III, IV, V) as well as one difluorotitanium complex (VI). The difluoro complex VI is exclusively formed by sing an excess of the ligand. VI was isolated and analytically characterized. The constitution and configuration of the complexes are concluded from 19F and 31P n.m.r. data. The tetraphenyl imidodiphosphate is only bidentately bonded, i.e. as chelate or bridging ligand; in the substitution complexes III-VI it is coordinated as anion.
    Notes: TiF4 bildet mit Imidodiphosphorsäuretetraphenylester in CH3CN zwei Tetrafluoro- (I, II) und drei Trifluorokomplexe (III, IV, V) sowie einen Difluorotitan-Komplex (VI). Mit Ligandenüberschuß entsteht ausschließlich der Difluorokomplex, der isoliert und elementar-analytisch charakterisiert wurde. Die Konstitutions- und Konfigurationsaussagen zu den übrigen Komplexen basieren auf 19F- und 31P-NMR-Untersuchungen. Der Imidodiphosphorsäureestr ist in den Komplexen stets zweizähnig als Chelat- oder Brückenligand gebunden; in den Substitutions-komplexen III-VI ist er in seiner anionischen Form enthalten.
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    Methylmetall-bis(trimethylsilyl)amidoderivate des Aluminiums, Galliums und Arsens (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 116-126 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Methyl Metal Bis(trimethylsilyl)amido Derivatives of Aluminium, Gallium, and ArsenicMeAl[N(SiMe3)2]2 (Me = CH3) has been prepared by the reaction of AlMe3 with HN(SiMe3)2 in a 1:2 molar ratio. The homologue Gallium compound (as well as the Aluminium derivative) is formed in good yields by the interaction of MeMcl2 (M = Al, Ga) with Li- and Na[N(SiMe3)2], respectively. MeAs[N(SiMe3)2]2 is formed by the reaction of AsCl3 and Na[N(SiMe3)2] in a 1:3 molar ratio. These colourless amido derivatives are monomeric in solution, they have been characterized by analyses, mass, n.m.r. (1H and 13C), and especially by i.r. and Raman spectra.
    Notes: MeAl[N(SiMe3)2]2 (Me = CH3) wurde durch Umsetzung von AlMe3 mit HN(SiMe3)2 im Molverhältnis 1:2 dargestellt. Die homologe Galliumverbindung (wie auch das Aluminiumderivat) bildet sich in guten Ausbeuten aus MeMCl2 (M =; Al, Ga) und Li- bzw. Na[N(SiMe3)2]. Schließlich entsteht MeAs[N(SiMe3)2]2 bei der Reaktion von AsCl3 mit Na[N(SiMe3)2] im Verhältnis 1:3. Diese farblosen Amidoderivate sind in Lösung monomer; sie werden elementar-analytisch, mit Hilfe der Massen- und NMR-Spektren (1H und 13C) sowie vornehmlich schwingungs-spektroskopisch (IR und Raman) charakterisiert.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885630116
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    Polynuclear clusters of technetium. I. Synthesis, crystal and molecular structure of bromide octanuclear lrismatic and hexanuclear octahedral clusters of technetium (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 136-152 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: mehrkernige Technetium-Cluster. I. Synthese, Kristall- und Molekularstruktur der Bromide achtkerniger prismatischer und sechskerniger oktaedrischer Cluster des TechnetiumsE werden die Synthese, Kristall- und Molekularstruktur erster Vertreter mehrkerniger Technetium-Cluster er Zusammensetzung: [Tc8Br4μ—Br8]Br. 2 H2O; [H(H2O)2][Tc8Br4μ—Br8]Br; [H(H2O)2]2[Tc8Br4μ—Br8]Br2; [H3O(H2O)3]2[Tc6Br6μ3—Br5]; [(C4H9)4N]2[Tc6Br6μ3—Br5]; [H3O(H2O)3]2[Tc6Br6μ3—Br5]. 4 H2O beschrieben. Diese Verbindungen unterscheiden sich in ihrem Bau wesentlich von bekannten Clustern anderer d-Elemente. Die Kristall- und Molekularstruktur von Hexabromotechnetiumsäure, (H3O)2TcBr6, ist untersucht worden.
    Notes: The synthesis, crystal and molecular structure of the first representatives of polynuclear technetium clusters are described. The composition of these clusters is: [Tc8Br4μ—Br8]Br. 2H2O; [H(H2O)2][Tc8Br4μ—Br8]Br; [H(H2O)2]2[Tc8Br4μ—Br8]Br2; [H3O(H2O)3]2[Tc6Br6μ3—Br5]; [(C4H9)4N]2[Tc6Br6μ3—Br5]; [H3O3]2[Tc6Br6μ3—Br5]. 4 H2O. It is shown that these clusters strongly differ in their structure from the known clusters of other d-elements. The crystal and molecular structure of hexabromotechetium acid (H3O)2TcBr6 is studied too.
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    URL: http://dx.doi.org/10.1002/zaac.19885630118
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    (Pentacarbonyl)wolfram-Komplexe von Diphosphanylacetylenen (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 48-59 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (Pentacarbonyl)tungsten Complexes of Diphosphanyl AcetylenesPreparation and properties of the following compounds are described: (Pentacarbonyl)tungsten complexes of diamidophosphoryl-diaminophosphanyl acetylenes (3, 4), of diamidothiophosphoryl-diaminophosphanyl acetylenes (5, 6) and of bis(diaminophosphanyl)-acetylenemethiodides (7, 8). Furthermore, the (pentacarbonyl)tungsten complexes of numerous halogenated diphosphanyl acetylenes have been prepared (15-21). All compounds are characterized by their n.m.r., i.r., and partly their mass spectra. Of (Pentacarbonyl)bis[bis(diethylamino)phosphanyl]acetylenemethiodide tungsten, 7, the molecular and crystal structures are reported.
    Notes: Darstellung und Eigenschaften der folgenden Verbindungen werden beschrieben: (Pentacarbonyl)wolfram-Komplexe von Diamidophosphoryl-diaminophosphanyl-acetylenen (3, 4), von Diamidothiophosphoryl-diaminophosphanyl-acetylenen (5, 6) und von Bis(diaminophosphanyl)-acetylenmethiodiden (7, 8). Weiter wurden die (Pentacarbonyl)wolfram-Komplexe zahlreicher halogenierter Diphosphanyl-acetylene (15-21) dargestellt. Alle Verbindungen sind durch ihre NMR-, IR- und teilweise ihre Massenspektren charakterisiert. Von (Pentacarbonyl){bis[bis(diethylamino)phosphanyl]acetylenmethiodid}wolfram, 7, werden die Molekül- und Kristallstruktur mitgeteilt.
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    URL: http://dx.doi.org/10.1002/zaac.19885670106
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    Darstellung und Kristallstruktur von CsVHP3O10 (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 77-86 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of CsVHP3O10Hitherto unknown CsVHP3O10 crystallizes from melts prepared from Cs2CO3, V2O3 and H3PO4 (2 d at 350°C; cooling rate: 10°/h). Best yields were obtained at a molar ratio 1:1:3 of the components. According to an X-ray crystal structure determination (C2/c; a = 1208.7(5), b = 877.7(3), c = 894.4(3) pm, β = 110.76(3)°; Z = 4; R = 0.043) the title compound is a catena-triphosphate. Bond lengths and angles are compared to those of triphosphates investigated earlier.
    Notes: Vorher unbekanntes CsVHP3O10 kristallisiert aus Cs2CO3/V2O3/H3PO4-Schmelzen (2 d bei 350°C, Abkühlrate: 10°/h). Optimale Ausbeuten werden bei einem molaren Verhältnis der Komponenten von 1:1:3 erzielt. Nach der Kristallstrukturanalyse (C2/c; a = 1208,7(5), b = 877,7(3), c = 894,4(3) pm, β = 110,76(3)°; Z = 4; R = 0,043) liegt ein catena-Triphosphat vor. Die Bindungslängen und -winkel im Anion werden mit denjenigen früher untersuchter catena-Triphosphate verglichen.
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    Zum Aufbau von A2[HgO2] (A = K, Rb), Rb2[NiO2] und Rb1,4K0,6[NiO2] [1-4] (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 69-76 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Note on the Structure of A2[HgO2] (A = K, Rb), Rb2 [NiO2], and Rb1.4K0.6[NiO2]Single crystals of K2[HgO2] (I), Rb2[HgO2] (II), Rb2[NiO2] (III) and Rb1,4K0,6[NiO2] (IV) have been prepared [mercurates: colourless; niccolates: dichroitic ambercoloured/green (III) resp. yellow/green (IV)] mid characterized by X-riay single crystal methods. They crystallize tetragonally in the Na2[HgO2]-type of structure (space group I4/mmm, Z = 2) with I: a = 392.0(1), c = 1397.4(3) pm; II: a = 413.9(1), c = 1423.9(2) pm; III: a = 416.6(1), c = 1314.6(2) pm; IV: a = 409.2(2), c = 1304.4(6) pm. The crystal structures have been refined (four circle diffractometer). The Madelung parts of lattice energy, MAPLE, effective coordination numbers, ECoN, these via mean fictive ionic radii, MEFIR, are calculated and discussed.
    Notes: K2[HgO2] (I) wurde erneut, Rb2[HgO2] (II), Rb2[NiO2] (III) sowie Rb1,4K0,6[SiO2](IV) erstmals in einkristalliner Form dargestellt und röntgenographisch untersucht. Kristalle der Mercurate sind farblos, jene der Niccolate dichroitisch bernsteinfarben/grün (III) bzw. gelb/grün (IV). Die Oxide kristallisieren tetragonal im Na2[HgO2]-Typ (Raumgruppe I4/mmm, Z = 2) mit I: a = 392,0(1), c = 1397,4(3) pm; II: a = 413,9(1), c = 1423,9(2) pm; III: a = 416,6(1), c = 1314,6(2) pm; IV: a = 409,2(2), c = 1304,4(6) pm. Die Strukturparameter wurden verfeinert (Vierkreisdiffraktometerdaten). Der Madelunganteil der Gitterenergie, MAPLE, sowie Effektive Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, werden berechnet und diskutiert.
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    Properties of barium chlorophosphate (apatite) luminophors activated by divalent europiumDedicated to Professor Arthur Scharmann on the Occasion of his 60th Birthday (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 60-68 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Eigenschaften von Bariumchlorophosphat (Apatit)-Leuchtstoffen bei Aktivierung mit zweiwertigem EuropiumEine Reihe von europiumaktivierten Barium- bzw. Calciumchlorophosphaten wurde in Pulverform dargestellt. Diese Leuchtstoffe sind isomorphe Vertreter der hexagonalen Chlorapatite (Ba, Ca, Mg)10(PO4)6Cl2. Neben Röntgendiffraktogrammen wurden Anregungs- und Emissionsspektren der Lumineszenz bei Zimmertemperatur und bei tiefen Temperaturen (T ∽ 4 K) untersucht. Steigender Calciumanteil beeinflußt die Lumineszenzeigenschaften dieser festen Lösungen durch Veränderung des am Eu2+-Ion wirkenden Kristallfelds. Das Erscheinen einer neuen Emissionsbande mit höherem Ca2+-Gehalt bei tiefen Temperaturen deutet auf Einbau der Eu2+-Ionen auf zwei verschiedenen Ba-Plätzen, so daß zwei Arten von Lumineszenzzentren auftreten. Die Lumineszenz entsteht durch Übergänge von der 4f65d- zur 4f7-Konfiguration des Eu2+.
    Notes: A series of powder materials of barium and calcium chlorophosphate activated by divalent europium have been prepared. These luminophors are isomorphous representatives of the hexagonal chlorapatites (Ba, Ca, Mg)10(PO4)6Cl2. In addition to x-ray diffractograms, excitation and emission spectra of luminescence have been studied at room and low temperatures (T ∽ 4 K). An increasing calcium content affects the luminescence properties of the solid solutions by changing the crystal field acting upon the Eu2+ ion. The appearance of a new low-temperature emission band with higher Ca2+ content indicates that the Eu2+ ions substitute on two different barium sites thus forming two types of luminescent centres. The luminescence arises from transitions between 4f65d and 4f7 configurations of Eu2+.
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    Synthesen und Kristallstrukturen von CsM2P5O16 (M = V, Fe) (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 87-94 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of CsM2P5O16 (M = V, Fe)Upon heating of mixtures composed of Cs2CO3, H3PO4 and V2O3(Fe2O3) to 〉600°C, melts were formed, from which the title compounds crystallized during slow cooling. They form as well from CsVHP3O10 (CsFeHP3O10) by condensation, besides (CsPO3)n. According to crystal structure determinations (Pn; for M = V: a = 753.79(7), b = 941.05(12), c = 1 017.29(12) pm, β = 111.16(9)°; for M = Fe: a = 752.99(17), b = 937.77(44), c = 1 020.90(18) pm, β = 111.02(1)°; Z = 2) the anionic part of both compounds consists of catena-pentaphosphate groups. Systematic variations in the P—O bond lengths are discussed.
    Notes: Durch Erhitzen von Gemengen aus Cs2CO3, H3PO4 und V2O3(Fe2O3) auf 〉600°C entstehen Schmelzen, aus denen bei langsamem Abkühlen die vorher unbekannten Titelverbindungen kristallisieren. Sie bilden sich auch bei der thermischen Kondensation von CsVHP3O10 (CsFeHP3O10), wobei als Nebenprodukt (CsPO3)n anfällt. Nach der Röntgenstrukturanalyse (Pn; für M = V: a = 753,79(7), b = 941,05(12), c = 1 017,29(12) pm, β = 111,16(;9)° für M = Fe: a = 752,99(17), b = 937,77(44), c = 1 020,90(18) pm, β = 111,02(1)°; Z = 2) handelt es sich um catena-Pentaphosphate. Die systematische Variation der P—O-Bindungslängen im Anion wird diskutiert.
    Additional Material: 3 Ill.
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    Na2H3IO6, eine Variante der Markasitstruktur (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 95-100 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na2H3IO6, a Variant of the Marcasite StructureSingle crystals of Na2H3IO6 were grown for the first time. According to the results of an X-ray crystal structure determination(Pnnm; a = 469.7(3), b = 529.9(2), c = 1005.2(6) pm; Z = 2; 296 diffractometer data; RW = 0.051) iodine is in an octahedral coordination. Sodium is surrounded by six oxygen in a strongly distorted octahedral arrangement. IO6 and NaO6 groups are linked via common vertices and edges in the sense of the rutile or marcasite type of structure. The corresponding structural relationship is discussed.
    Notes: Erstmals wurden Einkristalle von Na2H3IO6 erhalten. Nach der Röntgen-strukturanalyse (Pnnm; a = 469,7(3), b = 529,9(2), c = 1005,2(6) pm; Z = 2; 296 Diffraktometerdaten, RW = 0,051) ist Iod oktaedrisch und Natrium stark verzerrt oktaedrisch von Sauerstoff koordiniert. Die Verknüpfung der Oktaeder erfolgt im Sinne der Rutil- bzw. Markasitstruktur; die entsprechende Strukturverwandtschaft wird diskutiert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885670111
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    NMR investigations on Stannabicycloundecanes of the type RSn(CH2CH2CH2)3N (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 122-130 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NMR-Untersuchungen an Stannabicycloundecanen des Typs RSn(CH2CH2CH2)3NEs werden 1H-, 13C- und 119Sn-NMR-Daten von sieben Stannabicycloundecanen des Typs RSn(CH2CH2CH2)3N (1, R = Cl; 2, R = Br; 3, R = I; 4, R = OH; 5, R = SPh; 6, R = Me; 7, R = Sn(CH2CH2CH2)3N) mitgeteilt. Aus den Protonen-NMR-Koaleszenzdaten bei tiefer Temperatur wird ΔGTc* für die Racemisierung des Bicyclo[3.3.3]-Gerüstes zu 37 ± 1 kJ/mol bestimmt. Die Werte sind unabhängig vom Substituenten R. In den entsprechenden Siliciumderivaten (R = Me) werden geringere Aktivierungsparameter gefunden.
    Notes: The 1H, 13C, and 119Sn NMR data of seven stannabicycloundecanes of the type RSn(CH2CH2CH2)3N (1, R = Cl; 2, R = Br; 3, R = I; 4, R = OH; 5, R = SPh; 6, R = Me; 7, R = Sn(CH2CH2CH2)3N) are reported. From 1H NMR coalescence data at low temperature the free activation enthalpies for the racemisation of the bicyclo[3.3.3]skeleton were estimated to be 37 ± 1 kJ/mol. They are independent of the substituent R. However, it decreases when the tin atom is replaced by silicon for R = Me.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885670114
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  • 74
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    Monohalogenobenzoylhydrazones. V. Spectral and Bonding Properties of Some Novel Antimony(III) Complexes of p-chlorobenzoyl-di-(2-pyridyl)ketohydrazone studied by experimental and quantum-chemical methods (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 161-172 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Monohalogenobenzoylhydrazone. V. Spektroskopische Untersuchungen und Bindungs-verhältnisse einiger neuer Antimon(III)-Komplexe von p-Chlorobenzoyl-di-(2-pyridyl)-ketohydrazon mittels experimenteller und quantenchemischer MethodenBei der Reaktion von Antimon(III)-chlorid, -bromid und -iodid mit dem p-Chlorobenzoylhydrazon des Di-(2-pyridyl)keton (DpClBHH) in methanolischer Lösung werden Komplexe des Typs SbX2(DpClBH) erhalten. Die Struktur dieser Verbindungen wird an Hand der spektroskopischen Daten diskutiert. Der Ligand koordiniert dreizähnig über die Carbonyl- und Azomethin-Gruppe sowie über den Stickstoff der Pyridyl-Gruppe. Eine verzerrt oktaedrische Koordination des Metalls wird vorgeschlagen. EH-MO-Rechnungen wurden zur Analyse der Elektronen-spektren und der Bindungsverhältnisse herangezogen. Weiterhin dienen Grenzorbital-Betrachtungen aus CNDO/2-Rechnungen zur Klärung der Metall-Liganden-Bindung.
    Notes: Reactions of antimony(III) chloride, bromide, and iodide with p-chlorobenzoylhydrazone of di-(2-pyridyl)ketone (DpClBHH) in methanolic solutions afford the complexes SbX2(DpClBH). The structures of the new compounds are discussed in relation to their spectroscopic properties. In these complexes the ligand behaved as terdentate, coordination occuring through the carbonyl and azomethine groups, as well as the nitrogen atom of the pyridyl group. Consequently, a distorted octahedral environment around the metal is proposed. Moreover, EHMO calculations have been used in the analysis of the bonding in the SbCl2(DpClBH) complex, as well as to interpret the electronic spectral data. In addition, CNDO/2 calculations performed on the aforesaid ligand have been used to throw light on the mode of attachment of the ligand to the metal ion by means of some quantum-chemical indices related to the frontier MO's.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885670118
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    Mößbauer-Untersuchungen von Thiospinellen. VII. Das System Cd0,9Fe0,1Cr2(SxSe1-x)4 (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 173-178 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mössbauer Studies of Thiospinels. VII. The System Cd0.9Fe0.1Cr2(SxSe1-x)4In order to investigate the influence of mixed anions on 57Fe-Mössbauer spectra of thiospinels with tetrahedral FeII polycrystalline samples of the spinel system Cd0.9Fe0.1Cr2(SxSe1-x)4 have been prepared in the range 0.22 ≤ x ≤ 1. Room temperature Mössbauer spectra consist of several overlapping doublets of almost identical isomer shifts but different quadrupole splittings. The FeII-doublets are attributed to the five different coordination polyhedras S4, S3Se, S2Se2, SSe3, and Se4.
    Notes: Um den Einfluß eines gemischten Anionengitters auf die 57Fe-Mößbauer-Spektren von Thiospinellen mit tetraedrischem FeII zu untersuchen, wurden von dem spinell-system Cd0,9Fe0,1Cr2(SxSe1-x)4 im Bereich 0,22 ≤ x ≤ 1 polykristalline Proben hergestellt. Die Raumtemperatur-Mößbauer-Spektren der Spinellmischkristalle bestehen aus mehreren überlappenden Dubletts nahezu gleicher Isomerieverschiebung aber verschiedener Quadrupolaufspaltung. Die FeII-Dubletts können den Koordinationspolyedern S4, S3Se, S2Se2, SSe3 und Se4 zugeordnet werden.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885670119
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    Zur Charakterisierung des Extragitter-Aluminiums in Y-Zeolithen mittels der FerronmethodeVgl. auch Z. Chem. 27 (1987) 194. (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 145-152 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Characterization of Non-Framework Aluminium in Zeolites Y by the Ferron MethodBy using the ferron method it is shown that the non-framework aluminium occuring in dealuminated zeolites Y exists in form of different kinds of Al-oxo-hydroxo-species. At the beginning of dealumination (673 K) besides polymeric species with relatively low degree of polymerization monomeric and a special kind of oligomeric cations occur. These special cations alter into a mixture of oligomeric species with increasing temperature of dealumination (813 K). Simultaneously the degree of polymerization of the polymeric species increases.
    Notes: Mit der Ferronmethode wird gezeigt, daß das in thermisch behandelten Y-Zeolithen auftretende Extragitter-Aluminium aus unterschiedlichen Arten von Al-oxo-hydroxo-Spezies besteht. Am Anfang der Dealuminierung (673 K) liegen neben monomeren spezielle oligomere Kationen vor; gleichzeitig werden aber auch polymere Spezies mit relativ niedrigem Polymerisationsgrad gebildet. Mit steigender Temperatur der thermischen Behandlung (813 K) entsteht aus den oligomeren Teilchen ein Gemisch niedermolekularer Kationen. Die polymeren Spezies unterliegen dabei einer Veränderung im Sinne einer zunehmenden Kondensation bzw. Polymerisation.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885670116
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    Über Chalkogenolate. 188. Darstellung und Eigenschaften von Estern der Dithiopropionsäure (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 47-53 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 188. Preparation and Properties of Esters of Dithiopropionic AcidThe orange colored title compounds C2H5—CS—SR with R = CH3, C2H5, C(CH3)3, and CH2—C6H5 have been prepared in one-pot synthesis by reaction of ethyl bromide with magnesium followed by CS2 insertion and alkylation with the corresponding alkyl halide. Their electron absorption, infrared, nuclear magnetic resonance, and mass spectra are communicated.
    Notes: Die orangefarbene Titelverbindungen C2H5—CS—SR mit R = CH3, C2H5, C(CH3)3 und CH2—C6H5 wurden im Eintopfverfahren durch Umsetzung von Ethylbromid mit Magnesium, anschließender CS2-Insertion und Alkylierung mit dem entsprechenden Alkylhalogenid hergestellt. Ihre Elektronenabsorptions-, Infrarot-, Kernresonanz- und Massenspektren werden mitgeteilt.
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19885650106
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    Ein ungewöhnliches H-Brückenbindungssystem in Rubidium-hydroxiddihydrat, RbOH · 2 H2O (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 34-40 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: An Unusual System of Hydrogen Bonds in Rubidium Hydroxide Dihydrate, RbOH · 2 H2ORbOH · 2H2O was obtained by the reaction of Rb with H2O and dehydration of the resulting solution by concentrated sulfuric acid. The compound melts at 310 K. The structure was determined by X-ray single crystal methods: The H positions of H2O were found. The structure consists of a threedimensional H-bonded network of H2O molecules and OH-ions. Hydroxide ions are acceptors for four protons of four adjacent water molecules with d(O—O) = 2×2.59 Å and 2×2.82 Å. Oxygen of OH-ions is disordered over a distance of 1.27 Å. Rb has 8 H2O molecules as nearest neighbours, d(Rb—O) = 3.03 Å to 3.07 Å, OH-ions are further removed with d(Rb—O) ≥ 3.45 Å.
    Notes: RbOH · 2H2O wird durch Umsetzung von Rb mit H2O und Entwässern der entstehenden Lösung über konzentrierter H2SO4 erhalten. Die Verbindung schmilzt bei 310 K. An Einkristallen wurde ihre Struktur röntgenographisch bestimmt: Die H-Lagen an den H2O-Molekülen konnten ermittelt werden. Die Struktur zeigt ein brückengebundenes Gerüst von H2O-Molekülen und OH--Ionen. Die Hydroxidionen dienen als Akzeptoren für je ein Proton von vier benachbarten H2O-Molekülen mit d(O—O) = 2×2,59 Å und 2×2,82 Å. Der Sauerstoff des OH--Ions ist fehlgeordnet mit einem Abstand von 1,27 Å. Rb hat 8 H2O-Moleküle als nächste Nachbarn, d(Rb—O) = 3,03 bis 3,07 Å, OH--Ionen sind weiter entfernt mit d(Rb—O) ≥ 3,45 Å.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885650104
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    Zur Darstellung und Struktur von M1—LnTa3O9 (Ln = Pr, Nd) Röntgenographische und elektronenmikroskopische Untersuchungen (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 54-66 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of M1—LnTa3O9 (Ln = Pr, Nd), X-Ray and Electronmicroscopical InvestigationsNew ternary compounds M1—LnTa3O9 (Ln = Pr, Nd) could be prepared by chemical transport reaction in a temperature gradient T2 → T1 (T2 = 1100°C; T1 = 1000°C; CI2 as transport agent). M1 NdTa3O9 crystallizes in the monoclinic space group P 21/m with a = 5.3840(9) Å, b = 7.550(1) Å, c = 8.1911(9) Å and β = 92.46(1)°. The structure was refined to give R = 6.29% and Rw = 6.20%. It is built of double and single chains of corner-sharing TaO6 octahedra extended along the b-axis. Tunnels running along [010] are created by the framework of TaO6 octahedra. Ln (Ln = Pr, Nd) is located in these tunnels to levels of y = 1/4 and 3/4. A structure refinement for isostructural M1—PrTa3O9 led to a = 5.4051(7) Å, b = 7.5680(2) Å, c = 8.1964(9) Å, β = 92.38(2)° and R = 7.72%, Rw = 7.57%. By grinding in an agate mortar M1—LnTa3O9 transforms into M2—LnTa3O9, a new modification with a higher density.High resolution transmission electron microscopy images of the M1—PrTa3O9 structure were made along the [010] direction. They could be interpreted by comparing them with images calculated on the basis of the multi-slice method.
    Notes: Durch chemischen Transport im Temperaturgefälle T2 → T1 (T2 = 1100°C; T1 = 1000°C) mit dem Transportmittel Chlor (p(Cl2; 20°C) = 1 atm) wurden die neuen Verbindungen M1—LnTa3O9 (Ln = Pr, Nd) erhalten. Die Strukturbestimmung über Einkristalldaten ergab für M1—NdTa3O9: RG P21/m;a = 5,3840(9) Å, b = 7,550(1) Å, c = 8,1911(9) Å, β = 92,46(1)°; Z = 2; R = 6,29%, Rw = 6,20%. Es liegen TaO6-Oktaeder vor, die allseitig über Ecken miteinander verknüpft und zum Teil auch über Kanten zu Oktaederpaaren verbunden sind. In Richtung [010] wechseln sich Oktaeder und Oktaederpaare ab. In den längs b verlaufenden Kanälen zwischen den Oktaederpaaren befinden sich die Nd-Teilchen. Die Strukturverfeinerung am isotypen M1—PrTa3O9 führte zu den Gitterkonstanten a = 5,4051(7) Å, b = 7,5680(2) Å, c = 8,1964(9) Å, β = 92,38(2)° und R = 7,72%, Rw = 7,57%.Beim Zerreiben der Kristalle von M1—LnTa3O9 (Ln = Pr, Nd) erfolgt eine tribochemische Umwandlung in eine weitere neue Modifikation M2—LnTa3O9 mit signifikant höherer Dichte.Von M1—PrTa3O9 konnten hochaufgelöste elektronenmikroskopische Durchstrahlungsaufnahmen längs [010] erhalten werden. In Übereinstimmung mit der rechnerischen Kontrastsimulation sind die unbesetzten Kanäle bei einem Defokus von -1150 Å deutlich als heller Kontrast erkennbar.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885650107
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    Zur Darstellung und Struktur neuer Modifikationen von CeTa3O9 (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 67-80 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of New CeTa3O9 ModificationsThe modifications M—, O— and P—CeTa3O9 could be prepared by chemical transport reactions (T2 → T1; T2 = 1100°C; T1 = 1000°C) with chlorine as transport agent.M—CeTa3O9 crystallizes in the monoclinic space group C 2/m with a = 12.415(1) Å, b = 7.6317(8) Å, c = 6.5976(8) Å, β = 93.31(1)°; Z = 4; R = 4.88%, Rw = 3.67%. The structure consists of two types of Ta—O-polyhedra. Especially remarkable are chains of edge sharing pentagonal TaO7-bipyramids which are connected by TaO6-octahedra at opposite sides. Tunnels running along [010] are created by the framework of Ta—O-polyhedra and are filled with Ce in levels of y = 1/2 and y = 0.O—CeTa3O9 crystallizes orthorhombically with a = 6.5429(7) Å, b = 7.6491(7) Å, c = 12.583(1) Å and is isostructural to O—LaTa3O9 (space group: Pnma). O—CeTa3O9 contains the same characteristic structural units namely pentagonal TaO7-bipyramides and TaO6-octahedra. The difference between O— and M—CeTa3O9 is based on the orientation of the tunnels: in the orthorhombic modification they are arranged zigzag-like, in the latter parallel.Both modifications of CeTa3O9 can be irreversibly converted into the well-known perovskite-related P—CeTa3O9 structure with a lower density by heating in air to 1200°C.
    Notes: Durch chemischen Transport (T2 → T1; T2 = 1100°C; T1 = 1000°C) mit dem Transportmittel Chlor (p(Cl2; 298 K) = 1 atm) wurden Kristalle der neuen Modifikationen M— und O—CeTa3O9 sowie von der Perowskitvariante P—CeTa3O9 erhalten. Nach der Strukturbestimmung über Einkristalldaten ist M—CeTa3O9 monoklin (C 2/m) mit a = 12,415(1) Å, b = 7,6317(8) Å, c = 6,5976(8) Å, β = 93,31(1)°; Z = 4; R = 4,88%, Rw = 3,67%. Man erkennt aus kantenverknüpften pentagonalen TaO7-Bipyramiden bestehende Bänder längs c, die miteinander durch TaO6-Oktaeder verbunden sind. In den so gebildeten Kanälen sind die Cer-Teilchen lokalisiert.O—CeTa3O9 kristallisiert orthorhombisch mit a = 6,5429(7) Å, b = 7,6491(7) Å, c = 12,583(1) Å und ist nach Pulveraufnahmen isotyp mit der bereits näher untersuchten Verbindung O—LaTa3O9. Beide orthorhombischen Oxide sind wie M—CeTa3O9 durch ein Netzwerk kantenverknüpfter TaO7- und TaO6-Polyedern gekennzeichnet; in [010]-Richtung liegen nur Eckenverknüpfungen vor. Die TaO6-Oktaeder sind in der a—c-Ebene jeweils so angeordnet, daß die mit Ce (La) besetzten Kanäle bei O—CeTa3O9 zick-zack-förmig, bei M—CeTa3O9 parallel zueinander orientiert erscheinen.O— und M—CeTa3O9 zeigen beim Erhitzen (1200°C; an Luft) eine nicht reversible Umwandlung in die bekannte Perowskitmodifikation P—CeTa3O9 (Ce1/3TaO3) mit deutlich geringerer röntgenographischer Dichte.
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    URL: http://dx.doi.org/10.1002/zaac.19885650108
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    Zum Aufbau von NaRhO2 (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 106-110 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Structure of NaRhO2For the first time black single crystals of NaRhO2 (from Li2O, NAO0,50 α-Rh2O3, Li: Na: Rh = 1,15:2.18:1, Pd-cylinder, 950°C, 18 d, in 18 d cooled down) have been prepared and investigated by X-ray. NaRhO2 crystallizes in the α-NaFeO2-type: a = 309.71(4), c = 1552,75(34) pm, c/a = 5.01, space group R3m, Z = 3; fourcircle diffractometer data (Philips PW 1100): 124 of 126 I0(hkl): AgKα; R = Rw = 3.44%). The Madelung Part of Lattice Energy, MAPLE, and peculiarities of this type of structure are discussed.
    Notes: Erstmals wurden schwarze Einkristalle von NaRhO2 (aus Li2O, NaO0,50 und α-Rh2O3, Li: Na: Rh = 1,15:2,18:1, Pd-Bömbchen, 950°C, 18 d, 18 d abgekühlt) dargestellt und röntgenographisch untersucht. NaRhO2 kristallisiert im rhomboedrischen α-NaFeO2-Typ: a = 309,71(4), c = 1552,75(34) pm, c/a = 5,01, Raumgruppe R3m, Z = 3; Vierkreisdiffraktometerdaten (Philips PW 1100): 124 von 126 I0(hkl); AgKα; R = Rw = 3,44%). Der Madelunganteil der Gitterenergie, MAPLE, und Charakteristika des Strukturtyps werden diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19885650111
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    Chlor-Fluor-Austausch an halogenierten 1,3-Disilazanen (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 81-90 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chloro-Fluro-Exchange by Halogenated 1.3-DisilazanesAminofluorosilance (1-4) are obtained in the reaction of difluorosilanes with lithiated amines. Disilazanes (5,6) are formed in the reaction of LiNH(C6H3-iPr2) with CMe3SiF3 and C6H5SiF3. Lithium salts of 1-4 are dimers in n-hexane (7-10) and LiF adducts of iminosilanes in THF (11-14). The latter react with chlorsilanes (RSiCl3, R = Cl, H, Me) to give the substituted compounds 15-21 and LiCl. An intermolecular F/Cl exchange occurs with 15-20 which depends on the temperature, the solvents and ligands. 22-27 are formed.
    Notes: Aminofluorsilance (1-4) werden durch die Reaktion der Difluorsilane mit lithiierten Aminen erhalten. CMe3SiF3 und C6H5SiF3 reagieren zu Disilazanen (5,6). Die Lithiumsalze von 1-4 bilden in n-Hexan Dimere (7-10) und in THF LiF-Addukte von Iminosilanen (11-14). Letztere reagieren mit Chlorsilanen (RSiCl3, R = Cl, H, Me) unter LiCl-Abspaltung und Substitution zu 15-21 . 15-20 unterliegen einem intermolekularen F/Cl-Austausch, der temperatur-, lösungsmittel- und substituentenabhängig ist. Es entstehen 22-27 .
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885650109
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  • 83
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    Schwefeldioxid als Ligand und Synthon. VII. Phosphan-Schwefeldioxid-Nickel(0)- und Palladium(0)-Komplexe (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 91-105 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulfur Dioxide as Ligand and Synton. VII. Phosphane Sulfur Dioxide Nickel (0) and Palladium (0) ComplexesSynthesis and properties of phosphane sulfur dioxid d10-metal complexes of the types ML2(SO2)2, ML2(SO2), and ML3(SO2) (M = Ni(0), Pd(0); L = t-phosphane) are described. In dependence on the phosphane coligands nickel(0) complexes with η1-planar, η1-pyramidal and η2-S.O. (side on) coordinated SO2 are formed. In the case of the palladium(0)-SO2 complexes hithero prepared the dominating coordination mode is the η1-pyramidal one.
    Notes: Synthese und Eigenschaften von Phosphan-Schwefeldioxid-d10-Metallkomplexen der Typen ML2(SO2)2, ML2(SO2) und ML3(SO2) (M = Ni(0), Pd(0); L = t-Phosphan) werden beschrieben. In Abhängigkeit der Phosphan-Coliganden entstehen Nickel(0)-SO2-Komplexe mit η1-planar, η1-pyramidal und η2-S.O (side on) koordiniertem SO2. Dagegen dominiert im Falle der bislang dargestellten Palladium(0)-SO2-Komplexe die η1-pyramidale Koordinationsgeometrie.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885650110
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  • 84
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    Untersuchungen zur Anionenkonstitution in Mischungen aus Diethyl-di(2-hydroxyethyl)ammonium-und Triethyl-(2-hydroxyethyl)ammoniumsilicatlösungen Bildung von Diethyl-di (2-hydroxyethyl)ammonium-/Triethyl-(2-hydroxyethyl)ammoniumsilicathydraten (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 118-126 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigations of the Anion Constitution in Mixtures of Diethyl-di(2-hydroxyethyl)ammonium and Triethyl-(2-hydroxyethyl)ammonium Silicate Solutions. Formation of Diethyl-di(2-hydroxyethyl)-/Triethyl- (2-hydroxyethyl)ammonium Silicate HydratesOrganoammonium silicate solutions with a molar ratio base to silicon dioxide of 2 to 1 (cSiO2 =.1 and 1.7 mol · kg-1) and 1 to 1 (cSiO2 = 2.5 mol · kg-1) have been investigated with various amount of diethyl-di(2-hydroxyethyl)- and triethyl-(2-hydroxyethyl)ammonium hydroxide. Double-three and double-four ring silicate ions have been found in all solutions by 29Si n.m.r. spectroscopy. The amount of double-four ring species increases with increasing amount of diethyl-di-(2-hydroxyethyl)ammonium hydroxide. The substances crystallized are organoammonium double-four ring silicate hydrates, in which both of the mentioned base cations are present.
    Notes: Untersucht werden Organoammoniumsilicatlösungen mit einem molaren Verhältnis Base zu Siliciumdioxid von 2 zu 1 (SiO2-Konzentration von 1,1 und 1,7 mol · kg-1) und 1 zu 1 (SiO2-Konzentration von 2,5 mol · kg-1), wobei als Basekomponente unterschiedliche Anteile an Diethyl-di(2-hydroxyethyl)- und Triethyl-(2-hydroxyethyl)ammoniumhydroxid vorliegen. In allen Lösungen werden 29Si-NMR-spektroskopisch Doppeldreiring- und Doppelvierringsilicationen nachgewiesen, der Gehalt an Doppelvierringspezies erhöht sich mit steigendem Anteil an Diethyl-di(2-hydroxyethyl)ammoniumhydroxid. Auskristallisierende Substanzen sind Organoammonium-Doppelvierring-Silicathydrate, in denen stets beide Basekationen nebeneinander vorliegen.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885650113
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  • 85
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    Compound Formation in the System TeO2—Ta2O5 (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 127-136 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Verbindungsbildung im System TeO2—Ta2O5Drei Verbindungen existieren im System TeO2—Ta2O5: 3TeO2 · Ta2O5 (tetragonal), 2TeO2 · Ta2O5 (tetragonal und orthorhombisch) und TeO2 · 3Ta2O5 (orthorhombisch). Es wird gezeigt, daß die bisher als 7TeO2 · 3Ta2O5 und 2TeO2 · Ta2O5 (Hochtemperaturform) bezeichneten Verbindungen die stabilen Modifikationen von 2TeO2 · Ta2O5 (orthorhombisch) bzw. TeO2 · 3Ta2O5 sind.
    Notes: Three compounds exist in the system TeO2—Ta2O5: 3TeO2 · Ta2O5 (tetragonal), 2TeO2 · Ta2O5 (tetragonal and orthorhombic), and TeO2 · 3Ta2O5 (orthorhombie). The compounds previously denoted as 7TeO2 · 3Ta2O5 and 2TeO2 · Ta2O5 (high-temperature form) are shown to be stable modifications of 2TeO2 · Ta2O5 (orthorhombie) and TeO2 · 3Ta2O5, respectively.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885650114
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  • 86
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    Cobaltchelate als Hydrierkatalysatoren. VI. Spektralphotometrische Untersuchung der Adduktbildung des [Co(dpnH)]+-Komplexes mit Pyridin (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 137-146 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cobalt Chelates as Hydrogenation Catalysts. VI. Spectrophotometric Investigation of the Adduct Formation of [Co(dpnH)]+ with PyridineThe investigation of the adduct formation of the [Co(dpnH)]+ complex with pyridine by spectrophotometric measurements causes some difficulties due to the unfavourable overlapping of the spectra of the starting complex, the mono- and the bis-adduct in the spectral range used (17000-32000 cm-1). Therefore, the adduct formation constant β2 can only be determined, if the waveleagths for the evaluation of the data are suitably selected. The thermodynamic parameters, calculated from the temperature dependence of β1 (δRH° = -9.1 ± 0.5 kJ · mol-1, δRS° = -5.6 ± 1.7 J · mol-1 · K-1), differ clearly from those which have been obtained from kinetic measurements [3]. The reason for this difference, which is quite beyond the error limit of the applied methods, is most probably the neglect of analogous adduct equilibria with the solvent.
    Notes: Die Untersuchung der Adduktbildung des [Co(dpnH)]+-Komplexes mit Pyridin durch spektralphotometrische Messungen bereitet Schwierigkeiten, da sich die Spektren des Ausgangskomplexes, des Mono- und des Bis-Addukts im untersuchten Spektralbereich (17000-32000 cm-1) ungünstig überlagern. Die Adduktbildungskonstante β2 läßt sich daher nur ermitteln, wenn die Wellenzahlen für die Auswertung der Messungen geeignet ausgewählt werden. Die aus der Temperaturabhängigkeit von β1 berechneten thermodynamischen Parameter (δRH° = -9,1 ± 0,5 kJ · mol-1, δRS° = -5,6 ± 1,7 J · mol-1 · K-1) unterscheiden sich jedoch deutlich von den Werten, die durch kinetische Messungen [3] bestimmt worden sind. Ursache für diese, weit außerhalb der Fehlergrenze der Methoden liegenden Differenzen ist sehr wahrscheinlich die Vernachlässigung von analogen Adduktgleichgewichten mit dem Lösungsmittel.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885650115
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  • 87
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    Über die Chemie der Oxydation gasförmiger Gemische von C2F3Cl3, SiCl4, GeCl4 und POCl3 bei hohen Temperaturen (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 154-162 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About the Chemistry of the Oxidation of Gaseous Mixtures of C2F3Cl3, SiCl4, GeCl4, and POCl3 at High TemperaturesThe formation of gaseous compounds during the oxidation of gaseous mixtures of C2F3Cl3, SiCl4, POCl3, and GeCl4 within a reactor of quartz glass was investigated in the temperature range from 1273 to 2223 K by infrared spectroscopy in the effluent gases. At the low temperature CO, COF2, COFCl, and CF4 are formed as intermediates, which react in contact with SiO2 at higher temperatures to the stable final products CO2, Cl2, SiF4, POF3, and GeF4. The dependence of these reactions on temperature and the velocity of the gases is discussed.
    Notes: Die bei der Oxydation von gasförmigen Gemischen von C2F3Cl3, SiCl4, POCl3 und GeCl4 im Temperaturbereich von 1273 bis 2223 K im Quarzglasreaktor entstehenden Verbindungen werden in den Abgasen IR-spektroskopisch untersucht. Danach entstehen bei der tiefen Temperatur als Zwischenprodukte CO, COF2, COFCl und CF4, die bei der hohen Temperatur unter Wechselwirkung mit SiO2 in die Endprodukte CO2, Cl2, SiF4, POF3 und GeF4 übergeführt werden. Die Abhängigkeit dieser Reaktionen von Temperatur und Strömungsgeschwindigkeit wird diskutiert.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885650117
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  • 88
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    Synthese, thermisches Verhalten und Kristallstruktur von von [Ni(NH3)6][S(O)C=C(CN)2] · 1,5, H2O, einem Salz mit Nickel(II)-hexammin-Kationen (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 147-153 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Thermal Analysis, and X-Ray Crystal Structure of [Ni(NH3)6][S(O)C=C(CN)2] · 1.5 H2O, a Salt with the Nickel (II) Hexammine CationThe compound [Ni(NH3)6][S(O)C=C(CN)2] · 1.5 H2O is obtained by reaction of solutions of nickel acetate tetrahydrate in ammonia and K2[S(O)C=C(CN)2] · H2O in water. The salt crystallizes with the monoclinic space group P 21/a. The lattice constants are a = 15.183(1), b = 13.084(1), c = 14.386(1) Å, β = 100.96(7)° and Z = 8.The X-ray structure revealed two crystallographically independent nickel hexammine cations besides pseudochalcogenolate anions. The latter are associated with water molecules and exhibit strong delocalized π-electron systems.The thermal decomposition proceeds in three different steps. The first and second step refer to evolution of ammonia while in a third step H2O is squeezed out. This results in a decomposition of the substance.
    Notes: Die Verbindung [Ni(NH3)6][S(O)C=C(CN)2] · 1,5H2O ist durch Reaktion einer ammoniakalischen Lösung von Nickelacetat-Tetrahydrat mit K2[S(O)C=C(CN)2] · H2O, gelöst in Wasser, zugänglich. Das Salz kristallisiert monoklin mit der Raumgruppe P 21/a. Die Gitterkonstanten betragen a = 15,183(1), b = 13,084(1), c = 14,3886(1) Å, β = 100,96(7)° und Z = 8.Nach der Röntgenstrukturanalyse (R = 0,07, Rw = 0,06 für 1109 beobachtete Reflexe) liegen jeweils zwei kristallographisch verschiedene Nickelhexamminkationen neben Pseudochalkogenoanionen vor. Letztere sind ausschließlich mit Hydratwassermolekülen assoziiert und weisen mit ihren Bindungslängen auf stark delokalisierte π-Elektronensysteme hin.Die thermogravimetrische Analyse zeigt einen stufenförmigen Abbau der Solvensmoleküle, wobei zunächst in zwei Schritten Ammoniak entweicht. Der Abspaltung des Hydratwassers schließt sich die Zersetzung der Substanz an.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885650116
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  • 89
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    Darstellung und IR-spektroskopische Untersuchungen von Silylaminosilanen (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 171-180 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and I.R. Spectroscopic Investigations of SilylaminosilanesThe silylaminosilanes Me3-n(Me3SiNH)nSiH (n = 1-3) and (RMe2SiNH)3SiH were prepared by coammonolysis of dimethylorganochlorosilanes RMe2SiCl with chlorohydridosilanes Me3-nClnSiH (n = 1-3). The reaction of chlorohydridosilanes Me3-nClnSiH (n = 2,3) with hexamethyldisilzane yields the resp. silylaminosilanes Me3-n(Me3SiNH)nSiH(n = 2,3).The i.r. and 1H-n.m.r. data of the compounds are given and the relative basicity were measured by means of the V(C—D) band shift of CDCl3 associated to the silylaminosilanes. A dependence of the frequency of the Si—H stretching vibration and the number of trimethylsilylamino groups in Me3-n(Me3SiNH)nSiH and the substituents R in (RMe2SiNH)3SiH was found. All the methyl(silylamino)silanes Me3-n(Me3SiNH)nSiH show the same basicity, whereas the basicity of tris(dimethyl-organosilylamino)silanes is mainly determined by the steric effect of the substituents R.
    Notes: Die Silylaminosilane Me3-n(Me3SiNH)nSiH (n = 1-3) und (RMe2SiNH)3SiH (R = Et, n-Bu, Ph, C6H5CH2) wurden durch Coammonolyse der Dimethylorgano-chlorsilane RMe2SiCl mit den Chlorhydridsilanen Me3-nClnSiH (n = 1-3) dargestellt. Die Reaktion der Chlorhydridsilane Me3-nClnSiH (n = 2,3) mit Hexamethyldisilazan ergibt die entsprechenden Silylaminosilane Me3-n(Me3SiNH)nSiH (n = 2,3).Die IR- und 1H-NMR-Daten der Verbindungen sind angegeben, und die relative Basizität wurde gemessen an der Bandenverschiebung Δ∼ der V(C—D)-Bande des CDCl3 bei Assoziation an die Silyl-aminosilane. Die Bandenlage der Si—H-Valenzschwingung zeigt eine Abhängigkeit von der Anzahl der Trimethylsilylaminogruppen in den Me3-n(Me3SiNH)nSiH und den Substituenten R in den (RMe2SiNH)3SiH. Die Basizität der Methyl-silylamino-silane Me3-n(Me3SiNH)nSiH ist gleich, die der Tris-(dimethylorganosilylamino)-silane (RMe2SiNH)3SiH wird vorwiegend durch den sterischen Effekt der Substituenten R bestimmt.
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    URL: http://dx.doi.org/10.1002/zaac.19885650119
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  • 90
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    Vorberichte (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 192-192 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstracts.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885650121
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  • 91
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    Masthead (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 566 (1988) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885660101
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  • 92
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    Preparation, Chemical, and Structural Characterization of Some Molybdenum(III) and Tungsten(III) Coordination Compounds Containing 1-(4-pyridyl)pyridinium Cation (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 163-170 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung, chemische und strukturelle Charakterisierung von Molybdän(III)- Wolfram (III)-Komplexen mit 1-(4-pyridyl)pyridinium als Kation(Py2)HMoCl5 · H2O wurde aus der salzsauren Lösung von (NH4)2MoCl5 · H2O dargestellt ((Py2)H2+ = 1-(4-pyridyl)pyridinium-Ion, C10N2H102+). Diese nichtreaktive, luftbeständige Verbindung, kristallisiert orthorombisch. Die Gitterkonstanten sind: a = 12,895(4), b = 6,914(2), c = 16,388(7) Å, Z = 4. Die Elementarzelle enthält MoCl5 · H2O2-- Oktaeder und (Py2)H2+. Die Abstände Mo—Cl betragen 2,406(3) bis 2,446(4) Å. Die Bindung Mo—O(H2O) beträgt 2,19(1) Å. Der Winkel zwischen zwei Pyridinringen des Kations ist 38°. Die Anionen bilden Schichten auf den Ebenen mit Z = 1/4 und Z = 3/4. Zwischen den Schichten be-finden sich die (Py2)H2+-Kationen.(Py2)MX4Py2-Komplexe (M = Mo, W; X = Cl, Br; Py = Pyridin) mit deprotoniertem (Py2)H2+ als Kation, wurden aus den Lösungen von (PyH)MX4Py2 in konz. Ammoniak-Lösung durch Zusatz von (Py2)HCl2 hergestellt. Alle vier Verbindungen kristallisieren triklin. Die Gitterkonstanten sind vergleichbar. Die Stabilität gegen Oxydation und Substitution kann man der geringen Löslichkeit der Substanzen zuschreiben.
    Notes: 1-(4-pyridyl)pyridinium ion (C10H10N22+, (Py2)H2+) precipitates from the hydrochloric acid solution of (NH4)2MoCl5 · H2O sparingly soluble (Py2)HMoCl5 · H2O. This unreactive, air stable compound crystallizes in the orthorhombic unit cell with a = 12.895(4), b = 6.914(2), c = 16.388(7) Å, Z = 4. The ionic structure contains octahedral MoCl5 · H2O2- and (Py2)H2+. The bond lengths Mo—Cl are between 2.406(3) to 2.446(4) Å. The bond length Mo—O(H2O) is 2.19(1) Å. Planar pyridine rings of the cation are rotated around the common axis by 38°. Anions are located in layers at Z = 1/4 and 3/4. Between the layers (Py2)H2+ cations are situated.(Py2)MX4Py2 (M = Mo, W; X = Cl, Br; Py = Pyridine) with deprotonated (Py2)H2+ are prepared from the solutions of (PyH)MoX4Py2 in aqueous ammonia to which (Py2)HCl2 was added. All four compounds crystallize in the triclinic crystal system. Unit cell dimensions are comparable. The stability of the compounds against oxidation and substitution could have its origin in the low solubility.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19885650118
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  • 93
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    Darstellung und Reaktionen von methylenverbrückten Phosphor(III)-Phosphor(V)-Verbindungen (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 566 (1988), S. 90-102 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Reactions of Methylene-bridged Phosphorus(III)-Phosphorus(V) CompoundsThe synthesis of methylene-bridged diphosphorus compounds of the type Y2PCH2P(S)X2 (with Y = F, Cl, OPri, NMe2, Ph) is reported. Reactions of these compounds with bicycloheptadiene-metaltetracarbonyls to form complexes of the type (L—L′)M(CO)4 and (L—L′)2M(CO)4, respectively, as well as some oxidation reactions and the conversion of the phosphine F2PCH2P(S)F2 to the cyclotetraphosphine [PCH2P(S)F2]4 are described.
    Notes: Über die Darstellung von methylenverbrückten Diphosphorverbindungen der Zusammensetzung Y2PCH2P(S)X2 (mit Y = F, Cl, OPri, NMe2, Ph; X = F, OPri, NMe2, Ph) wird berichtet. Umsetzungen der erhaltenen Verbindungen mit Bicycloheptadien-Metalltetracarbonylen zu Komplexen des Typs (L—L′)M(CO)4 bzw. (L—L′)2M(CO)4 (mit M = Cr, Mo, W), einige Oxidationsreaktionen und die Umwandlung des Phosphans F2PCH2P(S)F2 zum Cyclotetraphosphan [PCH2P(S)F2]4 werden beschrieben.
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    URL: http://dx.doi.org/10.1002/zaac.19885660113
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  • 94
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    Polysulfonylamine. IX. Trimethyl(dimesylamino)stannan: Festkörperstruktur und Reaktionen mit kovalenten Chloriden (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 566 (1988), S. 103-110 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonyl Amines. IX. Trimethyl(dimesylamino)stannane: Solid State Structure and Reactions with Covalent ChloridesTrimethyl(dimesylamino)stannane, (CH3)3SnN(SO2CH3)2, is prepared from (CH3)3SnOH and HN(SO2CH3)2 in aqueous solution or from (CH3)3SnCl and AgN(SO2CH3)2 in acetonitrile. It crystallizes in the monoclinic space group Ce. In the crystal structure the Sn atoms are linked by bridging (CH3SO2)2N groups to form infinite zigzag chains in the direction of the b axis. Each Sn atom is surrounded by three C atoms and two O atoms of different mesyl groups in a strongly distorted trigonal bipyramidal arrangement. The approximately linear OSnO group (O—Sn—O angle 172.9°) is not perpendicular to the equatorial plane of the Sn atom; the O—Sn—C angles are in the range from 66.4 to 116.1°. The Sn—O distances amount to 227.5 and 230.1 pm. The very short S—N distances (159.6 and 162.3 pm) and the large S—N—S angle (116.1°) are consistent with (p—d)π interactions between nitrogen and sulfur. The compound is cleaved quantitatively by methane- and ethanesulfonyl chorides, benzoyl chlorides, hydrogen chloride, and chlorine, yielding (CH3)3SnCl and trisulfonyl amines, N-benzoyl dimesylamine, dimesylamine, and N-chloro dimesylamine, respectively.
    Notes: Trimethyl(dimesylamino)stannan, (CH3)3SnN(SO2CH3)2, wird aus (CH3)3SnOH und HN(SO2CH3)2 in Wasser oder aus (CH3)3SnCl und AgN(SO2CH3)2 in Acetonitril erhalten. Es kristallisiert monoklin in der Raumgruppe Cc. In der Kristallstruktur sind die Sn-Atome über (CH3SO2)2N-Brücken zu unendlichen Zick-Zack-Ketten in Richtung der b-Achse verknüpft. Jedes Sn-Atom ist von drei C-Atomen und zwei O-Atomen verschiedener Mesylgruppen in einer stark verzerrten trigonal-bipyramidalen Anordnung umgeben. Die nahezu lineare OSnO-Gruppe (O—Sn—O-Winkel 172,9°) steht nicht senkrecht auf der Äquatorebene des Sn-Atoms; es treten O—Sn—C-Winkel von 66,4 bis 116,1° auf. Die Sn—O-Abstände betragen 227,5 und 230,1 pm. Die sehr kurzen S—N-Abstände von 159,6 und 162,3 pm sowie der große S—N—S-Winkel von 116,1° deuten auf (p-d)π-Wechselwirkungen zwischen Stickstoff und Schwefel. Die Verbindung wird durch Methan-und Ethansulfonylchlorid, Benzoylchlorid, Chlorwasserstoff bzw. Chlor quantitativ unter Bildung von (CH3)3SnCl und Trisulfonylaminen, N-Benzoyl-dimesylamin, Dimesylamin bzw. N-Chlor-dimesylamin gespalten.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885660114
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    Beiträge zur Chemie der Silicium-Schwefel-Verbindungen. 50 [1] Bis(triorganoxysilyl)polysulfide und die Struktur des Bis(tri-t-butoxysilyl)disulfids (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 561 (1988), S. 167-173 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Silicon-Sulfur Compounds. 50. Bis(triorganoxysilyl)-polysulfides and the Structure of Bis(tri-tert-butoxysilyl)disulfideDisilylated polysulfides (RO)3SiSnSi(OR)3, R = i-Pr, tert-Bu, 2,6-Me2C6H3, n = 2-5, were obtained by reaction of (RO)3SiSNa with I2 or SnCl2, respectively. The reaction of [(t-BuO)3Si]2S2 with Ph3SiH yielded the mixed sulfide (t-BuO)3SiSSiPh3 and with Ph3P or Bu3P, by extrusion of one sulfur atom, the [(t-BuO)3Si]2S. The X-ray crystal structure of [(t-BuO)3Si]2S2 was determined. The S—S bond length is 209,2 pm, Si—S 213,2 pm. The mean value of the Si—S—S angle is 100,7°, and the torsion angle Si—S—S—Si -127,6°.
    Notes: Disilylierte Polysulfide (RO)3SiSnSi(OR)3, R = i-Pr, t-Bu, 2,6-Me2C6H3, n = 2-5, wurden durch Reaktion von (RO)3SiSNa mit I2 bzw. SnCl2 dargestellt. Die Umsetzung von [(t-BuO)3Si]2S2 mit Ph3SiH liefert ein gemischtes Sulfid (t-BuO)3SiSSiPh3 und mit Ph3P oder Bu3P, durch Abbau eines S-Atoms, [(t-BuO)3Si]2S. Die Kristall-Struktur von [(t-BuO)3Si]2S2 wurde bestimmt. Die S—S-Bindungslänge beträgt 209,2 pm, Si—S 213,2 pm. Der Mittelwert für den Si—S—S-Winkel beträgt 100,7°, der Torsionswinkel Si—S—S—Si -127,6°.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885610118
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    Methylenverbindungen von Nichtmetallen. VI. Amide der Methan-bis(phosphonigsäure), -bis(phosphonsäure) und -bis(thiophosphonsäure) (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 561 (1988), S. 157-166 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Methylene Compounds of Non-Metals. VI. Amides of Methane-bis(phosphonous Acid), -bis(phosphonic Acid) and -bis(thiophosphonic Acid)Symmetrical- and asymmetrical-substituted amides of methane-bis(phosphonous acid), -bis(phosphonic acid) and -bis(thiophosphonic acid) have been obtained by stepwise aminolysis of the chlorides Cl2(Z)PCH2P(Z)Cl2 (1: Z = electron pair; 7: Z = S; 13: Z = O) and the fluoride F2(S)PCH2P(S)F2 19 with dimethylaminotrimethylsilane. Oxidation reactions of trivalent phosphonous amides with sulfur and dimethylsulfoxide have also been investigated.
    Notes: Symmetrisch- und asymmetrisch-substituierte Amide der Methan-bis-(phosphonigsäure), -bis(phosphonsäure) und -bis(thiophosphonsäure) wurden durch stufenweise Aminolyse von Chloriden der Zusammensetzung Cl2(Z)PCH2P(Z)Cl2 (1: Z = Elektronenpaar; 7: Z = S; 13: Z = O) und des Fluorids F2(S)PCH2P(S)F2 19 mit Dimethylaminotrimethylsilan erhalten. Die Oxidation von Amiden des dreibindigen Phosphors mit Schwefel und Dimethylsulfoxid wurde ebenfalls untersucht.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885610117
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    Phosphidierung von Wolframmetall (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 561 (1988), S. 185-191 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphidation of Tungsten MetalA study was undertaken concerning the phosphidation of tungsten at 800, 900, and 1000°C in phosphorus vapor at 1 atm by a sealed-tube method. X-ray diffraction patterns and an electron probe microanalysis of the products showed that all the phosphide films were composed of two layers, that is, their outer layers were composed of WP2 and their inner layers composed of WP. All the phosphidation reactions proceeded according to a parabolic rate law. The parabolic rate constant was given as a function of the absolute temperature by the following expression. Kp = 3.06X10-5 exp(-103 KJ mol-1/RT) kg2m-4s-1, (1 atm, 1073-1273 K). Tungsten metal was appreciably superior to iron, nickel, and chromium, which are the main constituent metals of stainless steel, and titanium with respect to phosphidation resistance.
    Notes: Die Reaktion von Wolframmetall bei der Phosphidierung bei 800, 900 und 1000°C in Phosphordampf (1 atm) wurde im geschlossenen Quarzrohr untersucht. Aus Röntgenbeugungsbildern und Elektronenstrahl-Mikroanalysen der Produkte folgt, daß alle Phosphidfilme aus zwei Schichten bestanden, ihre Außenschichten bestanden aus WP2 und ihre Innenschichten aus WP. Alle Phosphidierungsreaktionen verliefen nach dem parabolischen Zeitgesetz. Die parabolische Geschwindigkeitskonstante als Funktion der absoluten Temperatur lautet Kp = 3,06X10-5 exp(-103 KJ mol-1/RT) kg2m-4s-1, (1 atm, 1073-1273 K). Wolframmetall ist „phosphorfester“ als Eisen, Nickel und Chrom, welche Hauptbestandteile der nichtrostenden Stähle sind, und Titan.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885610120
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    Isolation and spectral characteristics of Ferric Iodide (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 561 (1988), S. 174-184 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Isolierung und spektrale Charakterisierung von Eisen(III)-iodidEisen(III)-iodid wurde zum ersten Mal in reiner Form als dunkelvioletter Feststoff aus einer Lösung in n-Hexan durch Bestrahlung von Fe(CO)4I2 und I2 mit Tageslicht erhalten. Seine Zusammensetzung wurde durch Elementaranalyse und quantitative Umsetzung mit n-Bu4N+I- zu dem bekannten n-Bu4N+FeI4- bestätigt. Obwohl die Verbindung im festem Zustand stabil ist, zersetzt sich FeI3 quantitativ in Lösung zu FeI2 und 0,5 mol I2.
    Notes: Ferric iodide is isolated pure for the first time as a dark purple solid when a hexane solution of diiodotetracarbonyliron(II) and diiodine is exposed to actinic radiation. Its identity is confirmed by elemental analysis and quantitative conversion to the known tetraiodoferrate(III) by treatment with tetra-n-butylammonium iodide. Although persistent in the solid state, ferric iodide is readily decomposed in solution to ferrous iodide and 0.5 mol diiodine quantitatively.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885610119
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    Zur Darstellung und Struktur neuer Modifikationen von CeTa3O9 (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 561 (1988), S. 192-192 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885610121
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    Masthead (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885620101
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