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  • Chemistry  (14)
  • bis(phosphane) sulphur dioxide nickel(0) complexes  (1)
  • structure  (1)
  • 1
    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.
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  • 2
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,4,6-Trimethyl-5,5-dialkyldiptychdiazastannolidone - Intramolecular Pentacoordinated Stannyl Derivatives of N,N′,N″-Trimethyliminodiacetic Acid AmideThe title compounds were obtained by the reaction of dialkyltin dialkoxides with N,N′,N″-trimethyl iminodiacetic acid diamide in boiling toluene. The compounds are monomeric in benzene. Their structure was investigated by 1H, 13C and 119Sn n.m.r. measurements.
    Notes: Die Titelverbindungen werden durch die Reaktion von Dialkylzinndialkoxiden mit N,N′,N″-Trimethyliminodiessigsäurediamid in siedendem Toluen erhalten. Die Verbindungen sind monomer in Benzen. Ihre Struktur wird 1H-, 13C- und 119Sn-NMR-spektroskopisch aufgeklärt.
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  • 3
    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.
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  • 4
    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.
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  • 5
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The analysis of the 1H NMR spectra of 2,8-dithia-1,5-diphosphabicyclo[3.3.0]octane, 2,8-dithia-1-phospha-5-azabicyclo[3.3.0]octane and 2,8-dithia-1-arsa-5-phosphabicyclo[3.3.0]octane is supported by means of 2D- J-resolved NMR measurements. The spectra suggest a preferred conformer with strong puckering of the fused five membered rings.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 463 (1980), S. 123-131 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Association Behaviour of Strannatranes1-Alkylstannatranes (R = Me, Et, Bu, Phenyl) associate in unpolar solvents to relatively stable trimeric units. In aqueous solution 1-methylstannatran displays no autoassociation. 1-t-Butylstannatran, 1-o-tolylstannatran, and 1-alkylthiostannatranes are monomeric in all kinds of solvents. The association behaviour is characterized by molecular mass estimation and 1H-, 13C-, and 119Sn-NMR measurements.
    Notes: Es wird über einige neue Stannatrane und Thiostannatrane berichtet und gezeigt, daß die 1-Alkylstannatrane in unpolaren Lösungsmitteln zu relativ stabilen trimeren Einheiten assoziieren. In wäßriger Lösung zeigt 1-Methylstannatran keine Selbstassoziation. 1-t-Butylstannatran, 1-o-Tolylstannatran und 1-Alkylthiostannatrane sind in allen Lösungsmitteln monomer. Das Assoziationsverhalten wird durch Molekulargewichtsbestimmung und 1H-, 13C- und 119Sn-NMR-Messungen charakterisiert.
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  • 7
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1-Organo-5,5-di-t-butyl-diptych-benzoxaphospha-stannolins  -  Diorganotin Compounds with Transannular Sn—P InteractionDi-t-butyltindimethoxid react with organo-bis-o-hydroxyphenyl-phosphines in benzene under elemination of methanol to the title compounds. The phosphorus-tin coordination is proved by 31 and 119Sn n.m.r. measurements.
    Notes: Di-t-butylzinndimethoxid reagiert mit Organo-bis-o-hydroxy-phenyl-phosphinen RP(o-C6H4OH)2 in Benzen unter Austritt von Methanol zu den Titelverbindungen. Die Verbindungen sind monomer löslich, die Phosphor-Zinnkoordination wird 31P- und 119Sn-NMR-spektroskopisch nachgewiesen.
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  • 8
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Bis(2-mercaptoethyl)phosphines with Organotin Compounds. Molecular Structure of a Tin Containing Sixteen-membered RingThe reaction of bis(2-mercaptoethyl)phosphine with di-t-butyltin dimethoxide yields mixture of oligomers of the type [t-Bu2Sn(SCH2CH2)2Pr]n (R = Me, Ph) from which the trans-configurated dimers (n = 2) have been isolated. By the reaction with sulphur and selenium, respectively, these dimers were transformed to the corresponding thioxo and selenoxo derivatives.The sixteen-membered ring trans-[t-Bu2Sn(SCH2CH2)2P(S)Ph]2 crystallizes in the space group P21/n with the unit cell dimensions a 1350.9, b 1310.2, c 1500.3 pm, β 96.36° and does not exhibit any intramolecular Sn—P interaction: The 1,5-diorgano-1-chloro-5-elementa-1-stanna(IV)-bicyclo-[3.3.01,5]octanes R(Cl)Sn(SCH2CH2)2E (6, R = Ph, E = PPh; 7, R = Ph, E = NMe) have been prepared from the corresponding sodium dithiolates and phenyltrichlorostannane. The transannulare Sn—P and Sn—N interactions in 6 and 7 are confirmed by 31P and 119Sn NMR investigations.
    Notes: Die Reaktion von Bis(2-mercaptoethyl)phosphinen mit Di-t-butylzinndimethoxid liefert Mischungen von Oligomeren des Typs [t-Bu2Sn(SCH2CH2)2PR]n (R = Me, Ph), von denen die trans-konfigurierten Dimere (n = 2) isoliert wurden. Durch Reaktion mit Schwefel bzw. Selen wurden diese in die entsprechenden Thio- bzw. Selenoderivate überführt. Der Sechzehnring trans-[t-Bu2Sn(SCH2CH2)2P(S)Ph]2 4 kristallisiert in der Raumgruppe P21/n mit den Gitterkonstanten a 1350,9, b 1310,2, c 1500,3 pm und β 96,36°, er enthält keine intramolekularen Sn—P.-Wechselwirkungen. Die 1,5-Diorgano-1-chloro-5-element-1-stanna(IV)-bicyclo[3.3.01,5]-octaneR(Cl)Sn(SCH2CH2)2E (6, R = Ph, E = PPh; 7, R = Ph, E = NMe) wurden aus den entsprechenden Natriumdithiolaten und Phenyltrichlorstannan erhalten. Die transannularen Sn—P- und Sn—N- Wechselwirkungen in 6 und 7 werden durch 31P- und 119Sn-NMR-Untersuchungen bestätigt.
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  • 9
    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.
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  • 10
    ISSN: 0044-2313
    Keywords: I. r. and 31P n. m. r. spectroscopy ; bis(phosphane) sulphur dioxide nickel(0) complexes ; X-ray structure of Ni(PCy3)2(SO2) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulphur Dioxide as Ligand and Synthon. X. The Coordination Geometry of SO2 in Bis(phosphane)-Sulphur Dioxide-Nickel(0) Complexes. Structure of Ni(PCy3)2(SO2)The SO2 coordination geometry in Ni(PR3)2(SO2) complexes with steric parameters of the coligands Θ ≫ 141° was investigated by means of IR and 31P-NMR spectroscopy. The X-ray structure of Ni(PCy3)2(SO2) is described. The hitherto discussed n2-S.O-SO2 coordination mode for this type of complexes couldn't be confirmed.
    Notes: Zur Ermittlung der SO2-Koordinationsgeometrie in Ni(PR3)2(SO2)-Komplexen deren Coliganden Kegelöffnungswinkel von Θ ≫ 141° aufweisen, wurden die IR-und 31P-NMR-Spektroskopie herangezogen. Die Einkristallröntgenstrukturanalyse von Ni(PCy3)2(SO2) wird beschrieben. Eine für diesen Komplextyp bislang diskutierte n2-S.O-Koordination des Schwefeldioxids ließ sich nicht bestätigen.
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