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Chemie der Isoblausäure, 9. Dreikomponenten-Cycloadditionen mit CyanokomplexenHerrn Professor Dr. Dr. mult. Hans Bock zum 65. Geburtstag gewidmet. (1993)

Fehlhammer, Wolf Peter ; Rieger, Dirk ; Lotz, Sabine ; [et al.]

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 2243-2246

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ISSN: 0009-2940

Keywords: Reactions at coordinated cyanide ; Cycloadditions, organometallic ; Carbenoid heterocycles ; Metal-ligand bond cleavage ; Oxazolinone syntheses ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Chemistry of Hydrogen Isocyanide, 9[1]. - Three-Component Cycloadditions with Cyano ComplexesA novel and obviously general reaction of the coordinated cyano ligand in [M(CN)(CO)5] - (M = Cr, W) is reported, viz. its high-yield one-step [2 + 1 + 2] cycloaddition with a great variety of isocyanides and ketones resulting in carbenoid metal complexes of five-membered N,O heterocycles. The structure of the product 1a from [W(CN)(CO)5] - , tert-butyl isocyanide, and diethyl ketone has been elucidated by X-ray diffraction and found to contain a C-bound non-aromatic 4-aminooxazoline with an unprecedented π-delocalization along the exo chain which is also evident from severe low-field shifts of the C-2 and C-4 signals in the 13C-NMR spectra. The heterocycles are cleaved off the metal by oxidative decomposition with KMnO4/Fe(NO3)3 to give the corresponding oxazolinones, e.g. 4, with a high potential for biological activity. The general validity of this reactivity pattern for metal cyanides is further demonstrated by the successful incorporation of cyanoiron(II) and -cobalt(III) species in these three-component cycloaddition reactions.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/cber.19931261012

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Die Reaktion von Imidokomplexen des Vanadiums mit NaF und Kronenethern Die Kristallstruktur von VCl3(N-t-Bu)Professor Klaus Krogmann zum 65. Geburtstage am 19. Oktober 1990 gewidmet (1990)

Massa, Werner ; Wocadlo, Sigrid ; Lotz, Sabine ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 589 (1990), S. 79-88

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ISSN: 0044-2313

Keywords: Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: The Reaction of Imido Complexes of Vanadium with NaF and Crown Ethers. The Crystal Structure of VCl3(N-t-Bu)The imido complexes of vanadium VCl3(NR) with R = Cl, Br, I react with NaF in acetonitrile in the presence of 15-crown-5 forming the complexes [Na-15-crown-5][V(NR)FCl3(CH3CN)], with R = t-Bu [Na-15-crown-5]2[V(N-t-Bu)FCl3]2, and with R = SiMe3 the nitrido complex [Na-15-crown-5][VNCl3] by cleavage of FSiMe3. The complexes are brown, moisture sensitive crystal powders, which are soluble in acetonitrile, but only sparingly in nonpolar solvents; they are characterized by IR spectroscopy.The crystal structure determination of VCl3(NCMe3) was solved with X-ray methods (Space group P21/c, Z = 4, 1048 observed unique reflexions, R = 0.073). The compound forms centrosymmetric dimeric molecules. They contain two nearly symmetric chloro bridges and are associated to chains by asymmetric VCl2V bridges (bond lengths VCl = 229.6 and 271.8 pm), the longer one being in trans-position to the V≡N—CMe3 group. The VN bond length (162 pm) corresponds with a triple bond, bond angle VNC = 170.4°.

Notes: Die Imidokomplexe des Vanadiums VCl3(NR) mit R = Cl, Br, I reagieren mit NaF in Acetonitril bei Anwesenheit von 15-Krone-5 unter Bildung von [Na-15-Krone-5][V(NR)FCl3(CH3CN)], mit R = t-Bu zu [Na-15-Krone-5]2[V(N-t-Bu)FCl3]2, und mit R = SiMe3 unter Abspaltung von FSiMe3 zu [Na-15-Krone-5][VNCl3]. Die Komplexe bilden braune, feuchtigkeitsempfindliche, in Acetonitril lösliche, in unpolaren Lösungsmitteln wenig lösliche Kristallpulver, die durch ihre IR-Spektren charakterisiert werden.Von VCl3(N—CMe3) wurde eine Kristallstrukturanalyse ausgeführt. Raumgruppe P21/c, Z = 4, 1048 unabhängige beobachtete Reflexe, R = 7,3%. Die Verbindung bildet über symmetrische VCl2V-Brücken verknüpfte zentrosymmetrische Dimere, die über weitere, asymmetrische VCl2V-Brücken zu Ketten polymerisieren (Abstände V-Cl 229,6 und 271,8 pm). Die längere V—Cl-Bindung befindet sich in trans-Position zu der V≡N—CMe3-Gruppe, deren VN-Abstand von 162 pm etwa einer Dreifachbindung entspricht (Bindungswinkel VNC = 170,4°).

Additional Material: 6 Tab.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19905890109

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Kristall- und Molekülstruktur von Bis(pyridin)bis(trifluoromethyl)zink (1993)

Behm, Joachim ; Lotz, Sabine D. ; Herrmann, Wolfgang A.

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 619 (1993), S. 849-852

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ISSN: 0044-2313

Keywords: Bis(pyridin)bis(trifluoromethyl)zinc ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Crystal and Molecular Structure of Bis(pyridine)bis(trifluoromethyl)zincBis(pyridin)bis(trifluoromethyl)zinc 1 has been isolated and characterized by means of single-crystal X-ray diffraction techniques. The title compound represents the first structure determination of a fully fluorinated alkylzinc compound (monoclinic, space group P21/c, Z = 4, a = 8.856(3), b = 18.158(3), c = 8.979(3) Å, β = 98.14(2)°, R = 0.054, Rw = 0.035). The zinc atom is in a distorted tetrahedral environment. The molecular structure of [ClZn(CCl2CF3) η2O]2 2 was solved, but is not included in a structural comparison due to crystallographic disorder.

Notes: Der Pyridin-Komplex 1 von Bis(trifluoromethyl)zink wurde durch Einkristall-Röntgenstrukturanalyse charakterisiert. Die Titelverbindung repräsentiert die erste Struktur eines vollfluorierten Zinkalkyls (monoklin, Raumgruppe P21/c, Z = 4, a = 8,856(3), b = 18,158(3), c = 8,979(3) Å, β = 98,14(2)°, R = 0,054, Rw = 0,035). Das Zinkatom ist verzerrt tetraedrisch koordiniert. Die Kristall- und Molekülstruktur der zweikernigen Zinkverbindung [ClZn(CCl2CF3) η2O]2 2 wurde bestimmt, kann aber wegen kristallographischer Fehlordnung nicht einem Strukturvergleich unterzogen werden.

Additional Material: 3 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19936190507

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