Über Antimon-haltige Heterocyclen, V Antimon(III)-dithiolate mit verbrückten 5-und 8-Ringen/On Heterocyclic Systems Containing Antimony, V Antimony(III) Dithiolates with Bridged 5-and 8 -Membered Rings

1986 ◽  
Vol 41 (11) ◽  
pp. 1455-1460 ◽  
Author(s):  
Harald M. Hoffmann ◽  
Martin Dräger

Abstract For diamony(III)-trisdithiolates two constitutions (bicyclic B or two bridged monocycles C) are possible. Two synthetical paths to three examples Sb2(XS2)3 with X = CH2CH2 (1), CH2CH2- O - CH2CH2 (2), CH2CH2- S - CH2CH2 (3) are reported. 13C NMR spectra in CDCl3 solution show the constitution C for 2 and 3, and a possible equilibrium C ⇌ 4:1) for 1. This corresponds to the result of a crystal structure analysis (R = 0.027). The constitution C found in solid 1 exhibits expanded coordination polyhedra around the two antimony atoms which indicate a starting point for rearrangement into the constitution B. The two bridged 5-membered rings have different conformations: envelope and half-chair.

1999 ◽  
Vol 54 (7) ◽  
pp. 858-862 ◽  
Author(s):  
Thomas P. Braun ◽  
Paul A. Gutsch ◽  
Hans Zimmer

The synthesis, IR and 31P NMR spectra of the complexes of various N-aryltriphenylphosphinimines with some mercury dihalides as well as the corresponding phosphonium salts are reported. It is shown by an X-ray crystal structure analysis of the complex of the unsubstituted phosphinimine with HgCl2 that in the solid state these complexes form dimers via two Hg ∙∙∙ μ2- Cl ∙∙∙ Hg bridges.


1996 ◽  
Vol 51 (1) ◽  
pp. 107-111 ◽  
Author(s):  
Anton Meller ◽  
Christoph Kümmel ◽  
Mathias Noltemeyer

Abstract Monomerie diiodides of 2,4,6-tri(tert-butyl)phenyl = (s-Mes), 2,4,6-triisopropylphenyl = (Trip)-and 2,4-di-tert-butyl-6-methylphenyl = (DBMP)-gallium and -indium were prepared by the reaction of the lithiated aryls with MI3 (M = Ga, In) in hexane/Et2O. s-MesInI2 (1), s-Mes2InI (2), s-MesGaI2 (3), s-Mes2GaI (4), Trip2InI (5) and (DBMP)2InI (6) were obtained and characterized by their mass and NMR spectra (1H, 13C), and/or by elemental analyses. An X-ray crystal structure analysis was carried out for 1.


2013 ◽  
Vol 68 (9) ◽  
pp. 1031-1040 ◽  
Author(s):  
Ivo C. Ivanov ◽  
Violina T. Angelova ◽  
Nikolay Vassilev ◽  
Ioannis Tiritiris ◽  
Boyan Iliev

Reactions of 4-hydroxycoumarin (1a) and 4-chlorocoumarin-3-carbaldehyde (1b) with amino alcohols or alkylene diamines led to the formation of the corresponding N-substituted 4-aminocoumarins 3, 5 and 6. However, 4-hydroxycoumarin-3-carbaldehyde (8) reacted with 2-aminoethanol and ethylenediamine to give N-substituted 3-(aminomethylene)-chromane-2,4-diones 9a, b. The structure and the E-configuration of compound 6 were proven by X-ray crystal structure analysis. Products 9a, b displayed signals of both E- and Z-isomers in their NMR spectra. All novel products have been characterized by means of spectral (IR, NMR, MS) data and elemental analyses


1984 ◽  
Vol 39 (6) ◽  
pp. 721-726 ◽  
Author(s):  
Irene Brüdgam ◽  
Hans Hartl ◽  
Dieter Lentz

AbstractThe unstable trifluorom ethylisocyanide can be stabilized on the Fe3(CO)11 framework. Infrared data suggest that the isocyanide ligand occupies bridging positions in the solid state and in solution. This fact has been confirmed by the crystal structure analysis and by 13C NMR measurements.


1979 ◽  
Vol 34 (2) ◽  
pp. 217-223 ◽  
Author(s):  
Volker Küllmer ◽  
Erika Röttinger ◽  
Heinrich Vahrenkamp

Abstract The selenium bridged complexes [(CO)4M-SeX]2 (M = Mn, Re; X = H, SnMe3) were converted by trimethylphosphine to the dimers [Me3P(CO)3M-SeX]2 and/or the monomers (Me3P)2(CO)3M-SeX. The obtained Se-SnMe3 compounds reacted with HCl to form the SeH compounds. The structures of the new complexes were deduced from their IR and NMR spectra. [(Me3P)2(CO)3Re]2Se, the first monobridged bis-carbonylmetal chalcogenide, was obtained as a byproduct and confirmed by a crystal structure analysis.


1995 ◽  
Vol 50 (12) ◽  
pp. 1833-1838 ◽  
Author(s):  
Ion Neda ◽  
Michael Farkens ◽  
Holger Thönnessen ◽  
Peter G. Jones ◽  
Reinhard Schmutzler

The reactions o f 2-hydro-1,3,5-trim ethyl-1,3,5-triaza-2-oxo-2λ4 -phosphorinan-4,6-dione 1 with the triazine derivatives, 1,3,5-trimethyl- and 1,3,5-tribenzyl-hexahydro-1,3,5-triazine, are described. The reaction of three equivalents of 1 with one equivalent of the triazine derivative gave 2 and 3. Both compounds were characterized via their 1H, 13C, and 31P NMR spectra, mass spectra and, in the case of 2, by an X-ray crystal structure analysis, which showed an almost planar six-membered ring; hydrogen bonds of the form N-H···O link the molecules in centrosymmetric pairs. The reactions of 1 with the aldehydes glyoxylic acid, 2-hydroxybenzaldehyde and 3,4,5-trimethoxybenzaldehyde gave addition products. The C (:O) group o f the aldehyde is inserted into the P -H bond o f 1. The resulting compounds 4 ,5 and 6 were characterized through their 1H, 13C, and 31P NMR spectra, and mass spectra.


1987 ◽  
Vol 42 (6) ◽  
pp. 739-745 ◽  
Author(s):  
Max Herberhold ◽  
Bertram Schmidkonz ◽  
Manfred L. Ziegler ◽  
Orhan Serhadle

Abstract Reaction of the tetrahydrofuran-stabilized 16-electron complex fragment [Cp*Re(CO)2] with dimethyl disulfide, MeSSMe, leads to the diamagnetic title compound, Cp*Re(CO)(SMe)2 , which was characterized by mass, IR and NMR spectra and by an X-ray crystal structure analysis**. The two methylsulfido ligands are bent (angles Re-S-CH3 114.1(3)°) and turned away from the Cp* ring. The Re - S-bond distances are 227.0(2) pm.


2000 ◽  
Vol 55 (12) ◽  
pp. 1188-1194 ◽  
Author(s):  
Max Herberhold ◽  
Gudrun Frohmader ◽  
Jürgen Peukert ◽  
Wolfgang Milius

The photo-induced substitution of a CO ligand in Cp*Ta(CO)4 (1) has been used to prepare a series of Cp*Ta(CO)3L (2) complexes, in which the two-electron ligand L includes, e.g., isonitriles, sulfanes, cyclic ethers, phosphanes and pyridines. The complexes (2a-y) were characterized by their v(CO) frequencies and their 1H and 13C NMR spectra, and were compared - if possible - with the corresponding vanadium complex, Cp*V(CO)4 (3) and its derivatives, Cp*V(CO)3L (4). The molecular structure of the 4-picoline complex Cp*V(CO)3(NC5H4-Me(4)) (4r) has been determined by X-ray crystal structure analysis.


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