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  • 1975-1979  (5)
  • 1978  (5)
Material
Years
  • 1975-1979  (5)
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  • 1
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Behavior of Mono- and Diorganylphosphine Sulfides towards Metal Carbonyl Systems, XIX: The Stabilization of Dithiobis(dimethylphosphine), [(CH3)2PS—]2. Crystal and Molecular Structure of [η5-C5H5(OC)2MnP(CH2)2S—]2 and [η5-C5H5(OC)2MnP(CH3)2]2SDithiobis(dimethylphosphine), [(CH3)2PS—]2, could be stabilized for the first time by complexing it with η5-C5H5Mn(CO)2. Crystals of the title compounds 1 and 2 are orthorhombic and monoclinic, space groups Iba 2 and C2/c, respectively, with Z = 8. With 218 pm the Mn — P bonds in 1 and 2 have considerable π-character. The dihedral angle in 1 is 120°.
    Notes: Dithiobis(dimethylphosphin), [(CH3)2PS—]2, konnte durch Komplexierung mit η5-C5H5Mn(CO)2 erstmals stabilisiert werden. Die Titelverbindungen 1 und 2 kristallisieren orthorhombisch bzw. monoklin in den Raumgruppen Iba 2 bzw. C 2/c mit Z = 8. Die Mn — P-Bindungen in 1 und 2 besitzen mit 218 pm beachtlichen π-Bindungscharakter. Der Torsionswinkel in 1 beträgt 120°.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Behavior of Mono- and Diorganylphosphine Sulfides towards Metal Carbonyl Systems, XV: Reactions at the Functional SH Group of Complex-stabilized Dimethylthiophosphinous AcidThe thiophosphinous acid complex LnMnPR2SH (1) (LnMn = π-C5H5Mn(CO)2: R = CH3) is obtained from R2HPS and LnMnTHF 1 can be oxidized with oxygen to the disulfide[LnMnPR2S—]2 (2) The acidic character of the SH proton in 1 is proved with CH2N2, sodium, or N(C2H5)3 whereby the methyl ester 3 and the salts Kat[LnMnPR2S] (4a,b) are formed. Acylation of 4a leads to the acyl derivatives LnMnPR2SCOR (5a-c), which on warming eliminate CO with the formation of the alkyl compounds LnMnPR2SR (7b,c). The monosulfide [LnMnPR2]2S (6) is obtained from 4a and LnMnPR2Cl. The properties of the newly prepared compounds and their structures are discussed on the basis of IR, 1H and 31P NMR spectra.
    Notes: Den Thiophosphinig-Säure-Komplex LnMnPR2SH (1) (LnMn = π-C5H5Mn(CO)2: R = CH3) erhält man aus R2HPS und LnMnTHF. 1 läßt sich mit Sauerstoff zum Disulfid [LnMnPR2S—]2 (2) oxidieren. Der acide Charakter des SH-Protons in 1 wird durch Umsetzung mit CH2N2. Natrium oder N(C2H5)3 nachgewiesen, wobei der Methylester 3 und die Salze Kat[LnMnPR2S] (4a,b) entstehen. Acylierung von 4a führt zu den Acylderivaten LnMnPR2SCOR (5a-c), welche beim Erwärmen unter Bildung der Alkylverbindungen LnMnPR2SR (7b,c) CO abspalten. Das Monosulfid [LnMnPR2]2S (6) erhält man aus 4a und LnMnPR2Cl. Die Eigenschaften der neu dargestellten Verbindungen und ihre Konstitutionen werden mit Hilfe von IR-, 1H- und 31P- NMR-Spektren diskutiert.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 111 (1978), S. 2067-2076 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Properties and Structure of Phosphinato Complexes of RheniumThe solvent adducts [R2PO2Re(CO)3L]n (1a, b) [R = CH3 (a); C6H5 (b)] are obtained by photolysis of R2PO2H with [Re(CO)5]2 in THF or 1,4-dioxane. Whereas substitution of L by CO forms the dimeric complexes [R2PO2Re(CO)4]2 (2a, b), elimination of L yields the tricarbonyl compounds [R2PO2Re(CO)3]n (3a, b). 2b and 3b between which exists a reversible equilibrium are also obtained by the reaction of BrRe(CO)5 with (C6H5)2PO2Ag. 2b crystallizes triclinic in the space group P¯1 with Z = 2. The IR and Raman spectra are discussed, the 31P NMR data reported.
    Notes: Durch Photolyse von R2PO2H mit [Re(CO)5]2 in THF oder 1.4-Dioxan erhält man die Solvens-Addukte [R2PO2Re(CO)3L]n (1a, b) [R = CH3 (a); C6H5 (b)]. Während der Austausch von L durch CO zu den dimeren Komplexen [R2PO2Re(CO)4]2 (2a, b) führt. bilden sich bei der Abspaltung von L die Tricarbonyl-Verbindungen [R2PO2Re(CO)3]n (3a, b). Zu 2b und 3b, zwischen denen ein reversibles Gleichgewicht besteht, gelangt man auch bei der Einwirkung von BrRe(CO)5 auf (C6H5)2PO2Ag. 2b kristallisiert triklin in der Raumgruppe P¯1 mit Z = 2. Die IR- und Raman-Spektren werden diskutiert, die 31P-NMR-Daten mitgeteilt.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 111 (1978), S. 2455-2457 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Selenium Dioxide Insertion into Tin-Oxygen BondsThe monomeric selenites [R3SnO]2SeO (1) [R = CH3 (a), n-C4H9 (b), C6H5 (c)] are obtained by insertion of SeO2 into the Sn—O bonds of bis(triorganyltin) oxides [R3Sn]2O. 1c is also formed from [(C6H5)3Sn]2E (E = S, Se) and SeO2. Depending on the stoichiometric ratio the reaction of (CH3)3SnOH with SeO2 yields 1a or (CH3)3SnOSe(O)OH (2a).
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 111 (1978), S. 3048-3057 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparative, Spectroscopic, and Structural Investigations on Organyl IVb-Element Seleninic Acid DerivativesThe seleninic acid derivatives R3EO2SeR′ [E = Pb (1), Sn (2), Ge (3), Si (4), C (5); R = CH3, C6H5:R′ = CH3 (a, d), C2H5 (b, e), C6H5 (c, f)] are obtained by reaction of triorganyl IVb-element halides R3EX (X = Cl, Br) with sodium or silver seleninates R′SeO2M. The lead and tin compounds 1 and 2 exist as polymeric seleninato-O, O′ complexes with the coordination number 5. While the germanium and silicium derivatives 3 and 4 are esters, in which the Ge and Si atoms are linked by only one O-atom to the R′SeO2- ligands, (C6H5)3CSe(O)2C6H5 (5f) is a selenone. The IR, Raman, 1H, 77Se, 13C NMR, and Mößbauer spectra are discussed. (CH3)3SnO2SeCH3 (2a) crystallizes in the monoclinic system, space group P21/c with Z = 8.
    Notes: Durch Umsetzung verschiedener Triorganyl-IVb-Elementhalogenide R3EX (X = Cl, Br) mit Natrium- oder Silberseleninaten R′SeO2M erhält man die Seleninsäurederivate R3EO2SeR′ [E = Pb (1), Sn (2), Ge (3), Si (4), C (5); R = CH3, C6H5: R′ = CH3 (a, d), C2H5 (b, e), C6H5 (c, f)]. Die Blei- und Zinnverbindungen 1 und 2 liegen als polymere Seleninato-O, O′-Komplexe mit der Koordinationszahl 5 vor. Während es sich bei den Germanium- und Silicium-Derivaten 3 und 4 um Ester handelt, in denen die Ge- und Si-Atome über nur ein O-Atom an die R′SeO2-Liganden gebunden sind, ist (C6H5)3CSe(O)2C6H5 (5f) ein Selenon. Die IR-, Raman-, 1H-. 77Se-, 13C-NMR- und Mößbauer-Spektren werden diskutiert. (CH3)3SnO2SeCH3 (2a) kristallisiert monoklin in der Raumgruppe P21/c mit Z = 8.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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