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  • 1
    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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  • 2
    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.
    Additional Material: 6 Ill.
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  • 3
    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.
    Additional Material: 5 Ill.
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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: 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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  • 5
    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.
    Additional Material: 1 Ill.
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  • 6
    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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  • 7
    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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  • 8
    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.
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  • 9
    ISSN: 0044-2313
    Keywords: γ-anti effect ; 1-phosphabicyclo 3.3.1 nonane derivatives ; pentacarbonylchromium complex ; structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: γ-Anti Effect in 1-Phosphabicyclo[3.3.1]nonane Derivatives with Substituents at Phosphorus. Synthesis and Structure of Pentacarbonyl(1-phosphabicyclo[3.3.1]nonane) ChromiumIn 1-phosphabicyclo[3.3.1]nonane derivatives of the composition C8H15P(X) the CC-conformation always dominates. Changes in the chemical shifts of the bridge-head carbon atom C(5) in the 13C-NMR spectrum are only originated by the electronic influence of the substituent X at the phosphorus centre. Based on a homogeneous interpretation of the electronic interactions and with regard to Pearsons's definition of electronegativity the electronegativities of substituents at the phosphorus atom X = Cr(CO)5, Fe(CO)4, and Ni(CO)3 are estimated. These groups are placed in antiperiplanar orientation to the carbon atom C(5).The molecular structure of (1-phosphabicyclo[3.3.1]-nonane) Cr(CO)5 3 was elucidated by X-ray diffraction analysis. The molecule features the 1-phosphabicyclononane ligand in the CC-conformation, which has a nearly undistorted Cr(CO)5 unit coordinated to the phosphorus atom (d Cr—P = 2.368(1) Å).
    Notes: Bei 1-Phosphabicyclo[3.3.1]nonan-Derivaten C8H15P(X) dominiert stets die CC-Konformation. Änderungen der chemischen Verschiebung des C(5)-Brückenkopfatoms im 13C-NMR-Spektrum werden alleine durch den elektronischen Einfluß des Substituenten X am Phosphoratom hervorgerufen. Auf der Grundlage einer einheitlichen Interpretation der elektronischen Wechselwirkungen und unter Anwendung des Elektronegativitätsbegriffs von Pearson konnte die Elektronegativität der in antiperiplanarer Position zu C(5) stehenden Phosphorsubstituenten X = Cr(CO)5, Fe(CO)4, Ni(CO)3 abgeschätzt werden.Die Molekülstruktur von (1-Phosphabicyclo[3.3.1]-nonan) Cr(CO)5 (3) wurde mittels Röntgenbeugung ermittelt. Das Molekül zeigt das Bild eines 1-Phosphabicyclo[3.3.1]nonans in der CC-Konformation, an dessen Phosphoratom eine nahezu unverzerrte Cr(CO)5 Einheit (d Cr—P = 2,368(1) Å) koordiniert ist.
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  • 10
    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).
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