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  • 1
    Electronic Resource
    Electronic Resource
    Phosphinsubstituierte Chelatliganden. XVIII. Penta- und Tetracarbonylmetall-Komplexe des Chroms, Molybdäns und Wolframs mit sekundären und tertiären Phosphinothioformamid-LigandenProfessor Gerhard Gattow zum 60. Geburtstage am 6. Februar 1986 gewidmet (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 532 (1986), S. 107-117 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphine Substituted Chelate Ligands. XVIII. Penta- and Tetracarbonylmetal Complexes of Chromium, Molybdenum, and Tungsten with Secondary and Tertiary Phosphinothioformamide LigandsMono- and bidentately coordinated phosphinothioformamide complexes are obtained by photochemical substitution of the metal hexacarbonyls M(CO)6 (M = Cr (a), Mo (b), W (c)). The M(CO)5 · THF adducts react with secondary thioamides under exclusion of light to give the P-coordinate pentacarbonyl complexes [(CO)5MPPh2C(S)NHR1] (R1 = Ph (1a-c), Me (2a)). The photoreaction of M(CO)5 · THF with secondary and tertiary thioamides at low temperatures leads to the formation of the P, S-chelate complexes . The corresponding N-silylated complexes 6a-c (R1 = Me3Si, R2 = Ph) are obtained by direct photosubstitution of M(CO)6 in cyclohexane solution. The labile bis(thioformamide) complexes [(CO)4M(PPh2C(S)NHMe)2] (7a-c, cis-trans isomers) are synthesized in low yields according to the same procedure. The attempted alkylation of the chelate complexes 3a-c remains unsuccessful, whereas the secondary thioformamides react with n-BuLi/CH2Br2 to give the methylene bis(thioformirnidoesters) [Ph2PC(NR1)S]2CH2 (R1 = Ph (8), Me (9)) in quantitative yields.
    Notes: Ein- und zweizähnig koordinierte Phosphinothioformamid-Komplexe lassen sich durch photochemische Substitution der Metallhexacarbonyle M(CO)6 (M = Cr (a), Mo (b), W (c)) darstellen. Durch Dunkelreaktion der M(CO)5 · THF-Addukte mit sekundären Thioamiden entstehen die P-koordinierten Pentacarbonyl-Komplexe [(CO)5MPPh2C(S)NHR1] (R1 = Ph (1a-c), Me (2a)). Die Tieftemperatur-Photoreaktion von M(CO)5 · THF mit sekundären und tertiären Thioamiden führt zur Bildung der P, S-Chelatkomplexe . Die entsprechenden N-silylierten Komplexe 6a - c (R1 = Me3Si, R2 = Ph) erhält man durch direkte Photosubstitution von M(CO)6 in Cyclohexan-Lösung. Nach der gleichen Methode lassen sich die labilen Bis(thioformamid)-Komplexe [(CO)4M(PPh2C(S)NHMe)2] (7a-c, cis-trans-Isomere) in geringer Ausbeute darstellen. Während die Alkylierung der Chelatkomplexe 3a-c nicht gelingt, reagieren die sekundären Thioformamide mit n-BuLi/CH2Br2 quantitativ zu den Methylen-bis(thioformimidoestern) [Ph2PC(NR1)S]2CH2 (R1 = Ph (8), Me (9)).
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19865320116
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  • 2
    Electronic Resource
    Electronic Resource
    IR- und RAMAN-spektroskopische Untersuchungen an der Trifluordithioessigsäure und einigen ihrer Derivate (1971)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 383 (1971), S. 255-262 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The infrared and RAMAN spectra of trifluorothioacetamide, trifluorodithioacetic acid, and silver and lead trifluorodithioacetate are reported. By combination of infrared and RAMAN spectroscopy, we especially succeeded in assigning definitely the asymmetric CS2 stretching vibration of CF3CSSH which is situated in the CF3 stretching range. In the case of CF3CSNH2, a nearly complete assignment of the vibrational spectrum is possible.
    Notes: Es wird über die IR- und RAMAN-Spektren des Trifluorthioacetamids, der Trifluordithioessigsäure und der Silber- und Bleitrifluordithioacetate berichtet. Durch Kombination von IR- und RAMAN-Spektroskopie ist es insbesondere gelungen, die im Bereich der CF3-Valenzschwingungen liegende asymmetrische CS2-Valenzschwingung von CF3CSSH eindeutig zuzuordnen. Im Falle des CF3CSNH2 ist eine nahezu vollständige Zuordnung des Schwingungsspektrums möglich.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19713830305
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  • 3
    Electronic Resource
    Electronic Resource
    Die Kristallstruktur des Trimethylzinn-methansulfinats, (CH3)3Sn02SCH3 (1976)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 423 (1976), S. 35-39 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Trimethyltin Methanesulfinate, (CH3)3SnO2SCH3Trimethyltin methanesulfinate, (CH3)3SnO2SCH3 crystallizes orthorhombie in the space group A2122. The lattice constants are: a = 7.98 ± 0.01, b = 12.59 ± 0.02 and c = 17.83 ± 0.02 Å Within the crystal structure the Sn atoms are linked together via bridging RSO2 groups to form a helical chain along [l00]. Each Sn atom is surrounded by three C and two 0 atoms in a trigonal bipyramidal arrangement. The Sn—C distances are in the range from 2.09 to 2.18 Å the Sn—0 distance amounts to 2.23 Å.
    Notes: Trimethýlzinn-methansulfinat, (CH3)3SnO2SCH3 kristallisiert orthorhombisch in der Raumgruppe A2122 mit den Gitterkonstanten a = 7,98 ± 0,01, b = 12,59 ± 0,02 und c = 17,83 ± 0,02 Å. In der Kristallstruktur sind die Sn-Atome über RS02-Brücken zu schraubenförmigen Ketten längs [100] verknüpft. Jedes Sn-Atom ist von drei C- und zwei 0-Atomen trigonalbipyramidal umgeben. Die Sn—C-Abstände liegen zwischen 2,09 und 2,18 Å, der Sn—0-Abstand beträgt 2,23 Å.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19764230106
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  • 4
    Electronic Resource
    Electronic Resource
    Nucleophile Addition von Triorganozinn-Anionen an Kohlenstoffdisulfid. III. Koordinationschemie der Triorganostannandithiocarbonsäurealkylester (1983)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 498 (1983), S. 41-49 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nucleophilic Addition of Triorganotin Anions to Carbon Disulfide. III. Coordination Chemistry of the Alkyl Esters of Triorganostannanedithiocarboxylic AcidsAs the first trialkyltin dithiocarboxylic ester, methyl tricyclohexylstannanedithiocarboxylate (L1) was synthesized which forms with (η5-C5H5)Mn(CO)2 · THF the complex CpMn(CO)2L1. In the same way, the triarylstannanedithiocarboxylic esters, L2 = Ar3SnCS2R (Ar = phenyl, R = methyl, ethyl, allyl, isopropyl; Ar = o-, p-tolyl, R = methyl), react with irradiated metal carbonyls to give the neutral complexes W(CO)5L2 and CpMn(CO)2L2 in which L2 is coordinated monodentately via the thiocarbonyl group. The methylester, L3 = Ph3SnCS2Me, forms with Re2(CO)9 · THF the dimetalcarbonyl complex Re2(CO)9L3 in which the ligand probably occupies the axial position.
    Notes: Als erster Trialkylzinndithiocarbonsäureester wurde Methyl-tricyclohexylstannandithiocarboxylat (L1) dargestellt, das mit (η5-C5H5)Mn(CO)2 · THF den Komplex CpMn(CO)2L1 bildet. Entsprechend reagieren die Triarylstannandithiocarbonsäure-alkylester, L2 = Ar3SnCS2R (Ar = Phenyl, R = Methyl, Ethyl, Allyl, Isopropyl; Ar = o-, p-Tolyl, R = Methyl), mit photochemisch aktivierten Metallcarbonylen zu den Neutralkomplexen W(CO)5L2 und CpMn(CO)2L2, in denen L2 einzähnig über die Thiocarbonylgruppe koordiniert ist. Der Methylester, L3 = Ph3SnCS2Me, liefert mit Re2(CO)9 · THF den Dimetallcarbonyl-Komplex Re2(CO)9L3, in dem der Ligand wahrscheinlich die axiale Position einnimmt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19834980306
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  • 5
    Electronic Resource
    Electronic Resource
    Nucleophile Addition von Triorganozinn-Anionen an Kohlenstoffdisulfid. IV. Darstellung und Komplexbildung von 1,n-Bis(triphenylstannandithiocarbonsäure)alkylenestern (1983)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 498 (1983), S. 50-56 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nucleophilic Addition of Triorganotin Anions to Carbon Disulfide. IV. Synthesis and Complex Formation of 1,n-Bis(triphenylstannanedithiocarboxylic) Alkylene EstersThe reaction of lithium triphenylstannanedithiocarboxylate with 1,n-dibromo-alkanes in THF solution yields for 3 ≤ n ≤ 6 stable 1,n-bis(triphenylstannanedithiocarboxylic) alkylene esters I-IV whereas for n = 1,2 elimination takes place. Only the propylene and butylene esters I, II (L) form with irradiated metal carbonyls neutral dinuclear complexes of the type M—L—M (M = W(CO)5, CpMn(CO)2) with monodentate coordination of the thiocarbonyl group on each side. Since the esters I-IV preferably adopt the open n-alkane conformation, no formation of a chelate ring occurs from steric reasons.
    Notes: Die Umsetzung von Lithium-triphenylstannandithiocarboxylat mit 1,n-Dibromalkanen in THF-Lösung liefert für 3 ≤ n ≤ 6 stabile 1,n-Bis(triphenylstannandithiocarbonsäure)alkylenester I-IV, während für n = 1,2 Eliminierungsreaktionen ablaufen. Nur die Propylen- und Butylenester I, II (L) bilden mit photochemisch aktivierten Metallcarbonylen neutrale Zweikern-Komplexe des Typs M—L—M (M = W(CO)5, CpMn(CO)2) mit jeweils einzähniger Koordination der Thiocarbonylgruppe. Da die Ester I-IV bevorzugt in der offenen n-Alkan-Konformation vorliegen, erfolgt aus sterischen Gründen keine Chelatring-Bildung.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19834980307
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  • 6
    Electronic Resource
    Electronic Resource
    Koordinationschemie funktioneller Phosphorylide. VII. Pentacarbonylmetall-Komplexe des Cyanmethylen-triphenyl-phosphorans, [Ph3P=CH(CN)] · M(CO)5 (M = Cr, Mo, W)Professor Walter Rüdorff zum 75. Geburtstage am 3. Oktober 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 516 (1984), S. 93-101 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Coordination Chemistry of Functional Phosphorus Ylides. VII. Pentacarbonylmetal Complexes of Cyanomethylene Triphenylphosphorane, [Ph3P=CH(CN)] · M(CO)5 (M = Cr, Mo, W)The pentacarbonyl complexes [Ph3P=CH(CN)] · M(CO)5 (1a-c) are obtained by reaction of the irradiated metal hexacarbonyls M(CO)6 (M = Cr, Mo, W) with cyanomethylene triphenylphosphorane under exclusion of light. The IR and NMR spectra indicate N-coordination of the ligand, that means a nitrile complex. The chromium complex 1a crystallizes triclinic (space group P1, Z = 2) with the lattice constant a = 1126.5(2), b = 1153.6(3), c = 951.4(3) pm; α = 103.47(3), β = 102.04(3), γ = 84.00(2)°. The linear array of the ligand atoms C7, C6, N forms an angle of 168.1(5)° with the metal-nitrogen bond. Significant bond distances are Cr—N = 206.2(6), N—C6 = 115.3(7), C6—C7 = 137.2(8) and P—C7 = 170.9(5) pm.
    Notes: Durch Umsetzung der photochemisch aktivierten Metallhexacarbonyle M(CO)6 (M = Cr, Mo, W) mit Cyanmethylen-triphenylphosphoran unter Lichtausschluß erhält man die Pentacarbonyl-Komplexe [Ph3P=CH(CN)] · M(CO)5 (1a-c). Die IR- und NMR-Spektren weisen auf N-Koordination des Liganden, d. h. auf einen Nitrilkomplex hin. Der Chromkomplex 1a kristallisiert triklin (Raumgruppe P1, Z = 2) mit den Gitterkonstanten a = 1126,5(2), b = 1153,6(3), c = 951,4(3) pm; α = 103,47(3), β = 102,04(3), γ = 84,00(2)°. Die linear angeordneten Ligandatome C7, C6, N bilden mit der Metall-Stickstoff-Bindung einen Winkel von 168,1(5)°. Die wichtigsten Bindungsabstände betragen Cr—N = 206,2(6), N—C6 = 115,3(7), C6—C7 = 137,2(8) und P—C7 = 170,9(5) pm.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845160913
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  • 7
    Electronic Resource
    Electronic Resource
    Insertion von Heteroallenen in Trimethylsilyl-diphenylphosphinProfessor Walter Rüdorff zum 70. Geburtstage am 3. Oktober 1979 gewidmet (1979)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 456 (1979), S. 155-162 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Insertion of Heteroallenes into Trimethylsilyl DiphenylphosphineThe Si—P bond in Me3SiPPh2 is easily attacked by the electrophilic heteroallenes CS2, RNCS(R = Ph, Me) and RNCO (R = Ph, Me). Normally, air- and water-sensitive 1:1 insertion products containing a Si—S (CS2) or Si—N bond (RNCS, RNCO) and small amounts of hydrolysis products are obtained. The IR, 1H NMR and mass spectra are discussed.
    Notes: Die Si—P-Bindung in Me3SiPPh2 wird von den Heteroallenen CS2, RNCS (R = Ph, Me) und RNCO (R = Ph, Me) leicht elektrophil angegriffen. Es entstehen die in der Regel luft- und feuchtigkeitsempfindlichen 1:1-Insertionsprodukte mit Si—S- (CS2) bzw. Si—N-Bindung (RNCS, RNCO) neben geringen Mengen Hydrolyseprodukten. Die IR-, 1H-NMR- und Massenspektren werden diskutiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19794560116
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