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  • 1
    Electronic Resource
    Electronic Resource
    Molecular structure of and restricted internal rotation about the tin-tin bond in [ClSn(CH2CH2CH2)2NCH3]2 and solution isomerism and isomerizations in [CH3Sn(CH2CH2CH2)2NCH3]2, two compounds with five-coordinate tin centers bound to each other (1988)
    s.l. : American Chemical Society
    Organometallics 7 (1988), S. 593-603 
    Details
    ISSN: 1520-6041
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1021/om00093a004
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  • 2
    Electronic Resource
    Electronic Resource
    Determination of the pore widths of highly porous materials with NMR microscopy (1997)
    Springer
    Fresenius' journal of analytical chemistry 357 (1997), S. 508-513 
    Details
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The quantitative characterization of macro-porous materials with regard to pore width and pore width distribution was accomplished for the first time by using 1H-NMR microscopy in combination with suitable methods of digital image analysis. Here we present the newly developed algorithm and discuss the first experimental results. Large-pored glass filter systems filled with silicon oil as intrusion fluid were used as references. Silicates of unknown pore width were analyzed both with the new method and with Hg intrusion. NMR image data were recorded using a 3D spin echo sequence, which gave 128 slice images with a spatial resolution of 14.5 μm × 14.5 μm within each slice, with a slice-thickness of 37 μm or 48 μm. A quantitative evaluation of the 3D NMR data, with regard to pore width and pore width distribution, was done using the appropriate image processing function of the HORUS program. Individual slice evaluation was performed first, followed by an analysis of the binding elements between the slices. Pore widths of the glass filters determined using this analytical algorithm were in accordance with the manufacturer’s values, and silicate pore widths were in good agreement with the values determined by Hg intrusion.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002160050203
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  • 3
    Electronic Resource
    Electronic Resource
    1,3,2,5-Dioxadiphosphorinanes. Six-membered ring compounds containing two different phosphorus atoms (1985)
    Springer
    Journal of chemical crystallography 15 (1985), S. 423-431 
    Details
    ISSN: 1572-8854
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The reaction of bis(hydroxymethyl)phenylphosphane withtert-butyldichlorophosphane leads to the formation ofcis-2-tert-butyl-5-phenyl-1,3,2,5-dioxadiphosphorinane (1). Thecis configuration was definitively proven by the X-ray diffraction study of the 2, 5-dithioxo derivative (2), which was obtained from (1) by a stereoselective reaction. The diselenoxo compound (3) was also prepared. These three new compounds were subjected to a complete NMR study (1H,13C,31P, and77Se).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01171046
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  • 4
    Electronic Resource
    Electronic Resource
    The structure of 5-aza-2,8-dioxa-1-stanna(II)bicyclo[3.3.0]octane (1983)
    Springer
    Journal of chemical crystallography 13 (1983), S. 201-210 
    Details
    ISSN: 1572-8854
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract From the1H,13C, and119Sn NMR spectra at different temperatures, it is concluded that the 5-alkyl-5-aza-2,8-dioxa-1-stanna(II)bicyclo[3.3.0]octanes dimerize in nonpolar solvents. The barrier for dimerization is lower (ΔG
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01161514
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  • 5
    Electronic Resource
    Electronic Resource
    Lanthanid-Komplexe mit schneller Z/E-Isomerisierung des 3-AcetyltetramsäureligandenHerrn Prof. Dr. Rolf Borsdorf zum 60. Geburtstag gewidmet (1992)
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 334 (1992), S. 179-180 
    Details
    ISSN: 0941-1216
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Lanthanide-Complexes with Rapid Z/E-Isomerisation of the 3-Acetyltetramic Acid Ligand
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prac.19923340215
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  • 6
    Electronic Resource
    Electronic Resource
    Synthese, Struktur und Molekülbeweglichkeit von [(o-Diorganophosphinylmethyl)-phenyl]-diorganozinn-halogeniden (1980)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 467 (1980), S. 203-210 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Molecular Mobility of [(o-Diorganophosphinylmethyl)phenyl]-diorganotin HalidesThe oxidation and halogenation of (o-triorganostannylbenzyl)diorganophosphines, prepared from o-lithiobenzyl-diorganophosphines and triorganotin halides yields the [(o-diorganophosphinylmethyl)phenyl]diorganotin halides 6-10. IR, 1H- and 31P-NMR data confirm for 6-10 a complexcyclic structure with pentacoordinated tin. From the temperature dependence of the 1H-NMR spectra follows a configuration inversion at the tin atom in these compounds.
    Notes: Die Oxidation und Halogenierung von (o-Triorganostannylbenzyl)-diorganophosphinen, dargestellt aus o-Lithiobenzyl-diorganophosphinen und Triorganozinnhalogeniden, liefert die [(o-Diorganophosphinylmethyl)-phenyl]-diorganozinnhalogenide 6-10. IR-, 1H-und 31P-NMR-Daten bestätigen für 6-10 eine komplexcyclische struktur mit pentakoordiniertem Zinn. Aus der Temperaturabhängigkeit der 1H-NMR-Spektren folgt ein Konfigurationswechsel am Zinn. Atom in diesen Verbindungen.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19804670123
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  • 7
    Electronic Resource
    Electronic Resource
    5-Alkyltriptychoxazastannolidone und 4,5,6,11-Tetramethyltriptychdiazastannolidon - Atranartige Organostannylderivate der Nitrilotriessigsäure und des Nitrilotriessigsäure-N,N′, N″-trimethyltriamids (1982)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 492 (1982), S. 135-138 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 5-Alkyltriptychoxazastannolidones and 4,5,6,11-Tetramethyltriptychdiazastannolidone  -  Atrane-like Organotin Derivatives of the Nitrilotriacetic Acid and the Nitrilotriacetic Acid TriamideAlkylphenyltin oxides react with nitrilotriacetic acid in dimethylformamide/toluene under elemination of water and benzene to the 5-alkyltriptychoxazastannolidones. The reaction of methyltin triethoxide with nitrilotriacetic-N,N′,N″-trimethyltriamide leads to the 4,5,6,11-tetramethyltriptychdiazastannolidone. The structure of these compounds is investigated by 1H-, 13C- and 119Sn-n.m.r. measurements.
    Notes: Alkylphenylzinnoxide reagieren mit Nitrilotriessigsäure in DMF/Toluen unter Eliminierung von Wasser und Abspaltung von Benzen zu den 5-Alkyltriptychoxazastannolidonen. Die Reaktion von Methylzinntriethoxid mit Nitrilotriessigsäure-N,N′,N′-trimethyltriamid führt zum 4,5,6,11-Tetramethyltriptychdiazastannolidon. Die Struktur der Verbindungen wird 1H-, 13C- und 119Sn-NMR-spektroskopisch aufgeklärt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19824920115
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  • 8
    Electronic Resource
    Electronic Resource
    5-Aza(Oxa, Thia)-2,8-dithia-1-stanna(II)-bicyclo[3.3.01,5]octane Intramolekular basenstabilisierte Stannylene (1983)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 502 (1983), S. 158-164 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 5-Aza(oxa, thia)-2, 8-dithia-1-stanna(II)-bicyclo[3.3.01,5]octanes  -  Intramolecular Stabilized StannylenesBy the reaction of tin(II) butoxide with mercaptanes of the general type E(CH2—CH2SH)2 (E = N-t-Bu, NMe, O, S) at temperatures up to 50°C the 5-aza(oxa, thia)-2, 8-dithia-1-stanna(II)-bicyclo[3.3.01,5]octanes I - IV are obtained in high yields. The compounds are monomeric in solution. Contrary at higher reaction temperatures (80°C) the spiro-compounds of the type [E(CH2CH2S)2]2Sn (V - VIII) are formed. Some typical stannylene reactions of I - IV with BF3, Cr(CO)6, Br2, and PhS—SPh show the high reactivity of the compounds. Their structure is investigated by 1H, 13C, and 119Sn n.m.r., i.r., and Mössbauer spectroscopy.
    Notes: Durch Umsetzung von Zinn(II)-butoxid mit Mercaptanen des allgemeinen Typs E(CH2CH2SH)2 (E = N-t-Bu, NMe, O, S) werden bei Temperaturen bis 50°C die 5-Aza(Oxa, Thia)-2, 8-dithia-1-stanna(II)-bicyclo[3.3.01,5]octane in hohen Ausbeuten erhalten. Die Verbindungen sind monomer in Lösung. Bei höheren Reaktionstemperaturen (80°C) resultieren dagegen vorzugsweise die Spiroverbindungen des Typs [E(CH2CH2S)2]2Sn (V - VIII). Einige typische Stannylenreaktionen von I - IV mit BF3, Cr(CO)6, Br2 und PhS—SPh belegen die hohe Reaktivität der Verbindungen. Ihre Struktur wird durch 1H-, 13C-, 119Sn-NMR, IR- und Mößbauer-Spektren bewiesen.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19835020720
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  • 9
    Electronic Resource
    Electronic Resource
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885670114
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  • 10
    Electronic Resource
    Electronic Resource
    1,5-Diphosphabicyclo[3.3.1]nonanFrau Professor Marianne Baudler zum 70. Geburtstage am 27. April 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 594 (1991), S. 66-76 
    Details
    ISSN: 0044-2313
    Keywords: Organophosphorus compounds, bicyclic hydrophosphorylation, intramolecular ; methylenebisphosphines ; 1,3-diphosphorinances ; 1,5-diphosphabicyclo[3.3.1]nonanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,5-Diphosphabicyclo [3.3.1]nonane1,5-Diphosphabicyclo[3.3.1]nonane 8 has been obtained by free-radical cyclization of CH2=CHCH2(H)PCH2P(H)CH2CH=CH2 6 and 1-allyl-1,3-diphosphorinane 7. For the synthesis of 6 and 7 the chlorophosphine Cl2PCH2PCl2 1 is used as a starting material, which can be converted into Me2N(Cl)PCH2P(Cl)NMe2 3 by reaction with (Me2N)2PCH2P(NMe2)2 2. Treatment of 3 with two equivalents of allyl lithium and cleavage of the PN bonds in CH2=CHCH2(Me2N)PCH2P(NMe2)CH2CH=CH2 4 with diluted HCl affords CH2=CHCH2(H)(O)PCH2P(O)(H)CH2CH=CH2 5. Phenylsilane is used for the first time as a reducing agent to obtain a secundary phosphine like 6 from the secundary phosphine oxide (5). Prolonged heating increases the yield of the byproduct 7 in the mixture of 6 and 7. Reactions of the trivalent phosphorus in 8 with CS2, CH3I, POCl3, NO, sulfur, and KSeCN, respectively, delivers the corresponding derivatives 9-17. The compounds decribed are characterized by 1H, 13C, 31P, 77Se n.m.r., i.r., and m.s. data.
    Notes: 1,5-Diphosphabicyclo[3.3.1]nonan 8 wird durch radikalische Cyclisierung von CH2=CHCH2(H)PCH2P(H)CH2CH=CH2 6 und 1-Allyl-1,3-diphosphorinan 7 erhalten. Ausgangsmaterial für die Synthese von 6 und 7 ist Cl2PCH2PCl2 1, das mit (Me2N)2PCH2P(NMe2)22 quantitativ zu Me2N(Cl)PCH2P(Cl)NMe2 3 reagiert. Die Umsetzung von 3 mit zwei Äquivalenten Allyllithium zu CH2=CHCH2(Me2N)PCH2P(NMe2)CH2CH=CH2 4 und Abspaltung der Me2N-Schutzgruppen mit verdünnter Salzsäure liefert CH2=CHCH2(H)(O)PCH2P(O)(H)CH2CH=CH2 5. Dessen Reduktion zu 6 gelingt mit C6H5SiH3. Daneben entsteht 7, das durch längeres Erhitzen angereichert werden kann. Reaktionen des dreibindigen Phosphors in 8 mit CS2, CH3I, POCl3, NO, Schwefel und KSeCN führen zu den Derivaten 9-17. Die Verbindungen werden durch 1H-, 13C-, 31P- und 77Se-NMR-sowie IR- und MS-Daten charakterisiert.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915940108
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