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Digitale Medien

Synthesis, characterization, and structures of 1-(9-Fluorenyl)-germatrane and 1-(Phenylacetylenyl)germatrane (1997)

Zaitseva, Galina S. ; Karlov, Sergei S. ; Churakov, Andrei V. ; [weitere]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 623 (1997), S. 1144-1150

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ISSN: 0044-2313

Schlagwort(e): Trihalogenogermane ; Germatrane ; Transmetalation ; Crystal structure ; Chemistry ; Inorganic Chemistry

Quelle: Wiley InterScience Backfile Collection 1832-2000

Thema: Chemie und Pharmazie

Beschreibung / Inhaltsverzeichnis: Darstellung, Charakterisierung und Strukturen von 1-(9-Fluorenyl)germatran and 1-(Phenylacetylenyl)germatranÜber die Synthesen der Titelverbindungen, nämlich N(CH2CH2O)3GeY (2 Y=Fluorenyl; 4 Y=PhC≡C) durch Reaktion von X3GeY (1 Y=Fluorenyl, X=Br; 5 Y=PhC≡C, X=Cl) mit N(CH2CH2OSnR3)3 (3 R=Et; 6 R=Bu) wird berichtet und die Darstellung der neuen Verbindung 1 wird beschrieben. Die Strukturen der Verbindungen wurden durch Elementaranalysen sowie mittels 1H and 13C NMR-Spektroskopie bestimmt, 2 und 4 massenspektrometrisch charakterisiert. 1, 2 und 4 wurden mit Röntgenbeugungsmethoden analysiert.

Notizen: Syntheses of the title compounds, viz. N(CH2CH2O)3GeY (2 Y=Fluorenyl; 4 Y=PhC≡C) by the reaction of X3GeY (1 Y=Fluorenyl, X=Br; 5 Y=PhC≡C, X=Cl) with N(CH2CH2OSnR3)3 (3 R=Et; 6 R=Bu) are reported including the preparation of the new compound 1. Identity and structures were established by elemental analyses, 1H and 13C NMR spectroscopy. 2 and 4 were characterized by mass spectrometry. Single crystal structures of 1, 2 and 4 were determined by X-ray diffraction methods.

Zusätzliches Material: 3 Ill.

Materialart: Digitale Medien

URL: http://dx.doi.org/10.1002/zaac.19976230723

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Digitale Medien

Synthesis of Germatranyl Derivatives of Esters of Carboxylic Acids via Organometallic (Si, Ge, Sn) Reagents (1997)

Zaitseva, Galina S. ; Livantsova, Ljudmila I. ; Nasim, Mohammed ; [weitere]

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 739-746

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ISSN: 0009-2940

Schlagwort(e): Germatranes ; Organotrihalogenogermanes ; Organometallic (Si, Ge, Sn) reagents ; Transmetallation ; Chemistry ; Inorganic Chemistry

Quelle: Wiley InterScience Backfile Collection 1832-2000

Thema: Chemie und Pharmazie

Notizen: Trialkylstannyl esters of tris(2-hydroxyalkyl)amines, N(CH2CHROSnAlk3)3 (9-11 (R = H, Me; Alk = Et, Bu), react with X3GeC(R1)(R2)COOR3 (12-17) (X = Cl or Br; R1, R2=H, Me, Ph, SiMe3, COOEt; R3=Me, Et) to give esters of α-germatranylcarboxylic acids, N(CH2CHRO)3GeC(R1)(R2)-COOR3 (1-8), in high yields. The synthesis of esters 12-17 is reported. Esters of α-germatranyldiphenylacetic acid 24 and 25 can be obtained by treatment of diphenylketene with Et3SnOMe to give in situ Et3SnC(Ph2)COOMe (23), followed by reaction with GeCl4 to give in situ Cl3GeC(Ph2)COOMe (22 and further reactions with 9 or 11, respectively. Reduction of germatrane 6 with LiAlH4 in diethyl ether leads to cleavage of the germanium-carbon bond with subsequent formation of (2-hydroxyethyl)trimethylsilane. The crystal structures of 3, 6 and 7 are reported. 1-Acyloxygermatranes 26 and 27 are obtained by treatment of 1-methoxygermatrane (28) with diphenyl- and dichloroacetic acid, respectively.

Zusätzliches Material: 4 Ill.

Materialart: Digitale Medien

URL: http://dx.doi.org/10.1002/cber.19971300611

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Digitale Medien

1H NMR T1(min) data and structure in a series of rhenium polyhydride complexes and the contribution of M-H dipole-dipole relaxation (1991)

Luo, Xiao-Liang ; Howard, Judith A. K. ; Crabtree, Robert H.

Chichester : Wiley-Blackwell

Organic Magnetic Resonance 29 (1991), S. S89

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ISSN: 0749-1581

Schlagwort(e): T1 method ; Dihydrogen complexes ; Dipole-dipole relaxation ; Chemistry ; Analytical Chemistry and Spectroscopy

Quelle: Wiley InterScience Backfile Collection 1832-2000

Thema: Chemie und Pharmazie

Notizen: The unusual species [ReH5(H2){P(p-tolyl)3}2], for which a neutron diffraction study shows an intermediate H—H bond distance of 1.357 Å, is studied by variable-temperature 1H NMR spin-lattice (T1) relaxation time measurements. The T1 relaxation rate goes through a maximum at low temperature and the resulting T1 (min) value is 66 ms. This is within the range of T1(min) values found for classical ReH7L2 complexes, so H2 complexes with such long H—H bond distances are undetectable by the T1 method. The observed T1(min) value is compared with that calculated from the neutron diffraction data. We consider not only the usual proton-proton dipole-dipole (HHDD) contributions to the relaxation but also the metal-hydride dipole-dipole (MHDD) contributions. The latter are shown to be negligible for most transition metals, but not for Nb, V, Re, Mn, Co and Ta. Inclusion of the MHDD contributions leads to better agreement between the calculated and observed T1(min) values for a series of rhenium polyhydride complexes. The MHDD relaxation also accounts for most of the disparity previously noted between the calculated and observed T1(min) values for Re2H8(PEt2Ph)4.

Zusätzliches Material: 1 Ill.

Materialart: Digitale Medien

URL: http://dx.doi.org/10.1002/mrc.1260291317

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