scholarly journals 2.2.5.5-Tetraorganyl-1.4-dioxa-2.5-disilacyclohexane/2,2,5,5-Tetraorganyl-1,4-dioxa-2,5-disilacyclohexanes

1983 ◽  
Vol 38 (2) ◽  
pp. 190-193 ◽  
Author(s):  
Reinhold Tacke ◽  
Hartwig Lange ◽  
Anke Bentlage ◽  
William S. Sheldrick ◽  
Ludger Ernst

Abstract The 2,2,5,5-tetraorganyl-1,4-dioxa-2,5-disilacyclohexanes 2a-2c were prepared by condensation of the corresponding (hydroxymethyl)diorganylsilanes 1 a-1 c. The constitution of the heterocycles was confirmed by elemental analyses, cryoscopic measurements, mass spectrometry, and NMR-spectroscopic (1H, 13C) investigations. The molecular structure of 2 b was determined by X-ray diffraction analysis.

Author(s):  
Süheyla Özbey ◽  
Nilgün Karalı ◽  
Aysel Gürsoy

AbstractIn this study 4-(3-coumarinyl)-3-benzyl-4-thi azolin-2-one 4-methylbenzylidenehydrazone 3 was synthesised. An independent proof of the thiazolylhydrazone structure of 3 was achieved by single crystal X-ray diffraction analysis. Elemental analyses and spectral data (IR,


1985 ◽  
Vol 40 (3) ◽  
pp. 363-367 ◽  
Author(s):  
Fritz Preuss ◽  
Edith Fuchslocher ◽  
William S. Sheldrick

tC4H9N = VCl2(NHtC4H9) and the tert-butylamine complex [tC4H9N=VCl2(NHtC4H9)(NH2tC4H9)] have been prepared by reaction of tC4H9N=VCl3 with NH2tC4H9. 1H and 51V NMR data of these compounds are reported. The complex was investigated by X-ray diffraction analysis; the structure has been found to be a binuclear vanadium complex bridged by two Cl-atoms with a distorted octahedral arrangement of the ligands.


Synthesis ◽  
2017 ◽  
Vol 49 (11) ◽  
pp. 2389-2393 ◽  
Author(s):  
Stefanie Pelzer ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Nikolai Ignat’ev ◽  
Reint Eujen ◽  
...  

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.


2002 ◽  
Vol 2002 (12) ◽  
pp. 644-646 ◽  
Author(s):  
Michael T.M. Choi ◽  
Qingchuan Yang ◽  
Thomas C.W. Mak ◽  
Dennis K.P. Ng

Two hexa-substituted anthracenes have been synthesised; the molecular structure of a [4+4] head-to-tail anthracene dimer has also been determined by X-ray diffraction analysis.


1980 ◽  
Vol 58 (8) ◽  
pp. 777-779 ◽  
Author(s):  
T. Stanley Cameron ◽  
Christine Chan ◽  
David G. Morris ◽  
Alistair G. Shepherd

The crystals belong to the orthorhombic space group C222, with a = 9.226, b = 12.092, c = 16.513 Å, Z = 4. A single crystal X-ray diffraction analysis has shown that the title compound, in which all carbon atoms are sp2 hybridized, exists with the ten membered ring in a slightly twisted tub conformation. The 13C nmr spectrum is also reported.


2001 ◽  
Vol 56 (11) ◽  
pp. 1100-1108 ◽  
Author(s):  
Fritz Preuss ◽  
Monika Vogel ◽  
Uwe Fischbeck ◽  
Jens Pemer ◽  
Gerhard Overhoff ◽  
...  

The reactions of tBuN = VCl2 · DME with LiX (X = NHtBu, NR2, OSiPh3, SR, Alkyl, Cp) have been studied. LiNHtBu and LiCH3 furnish the binuclear diamagnetic tert-butylimido-vanadium( IV) compounds [(μ-NtBu)2V2X4]; in all other cases only the vanadium(V) compounds tBuN=VX3 and tBuN=VCpCl2 formed by disproportionation reactions of vanadium(IV) can be isolated. The syntheses of various mononuclear amido tert-butylimido-vanadium(V) complexes as well as of the binuclear complexes [μ-NtBu)2V2(NtBu)2Cl2] and [(μ-0)V2(NtBu)2Cp2Cl2] are also described. All compounds obtained have been characterized by 51V NMR spectroscopy. tBuN=V(OMe)3 was investigated by X-ray diffraction analysis; the molecular structure has been found to be that of a binuclear vanadium(V) complex with two bridging methoxo ligands.


Synthesis ◽  
2020 ◽  
Vol 52 (07) ◽  
pp. 1025-1034 ◽  
Author(s):  
Marvin Linnemannstöns ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Norbert W. Mitzel

Starting from trichloro(phenylethyl)silane, six differently fluorinated triaryl(phenylethyl)silanes were synthesized by salt elimination reactions and their structures were determined by X-ray diffraction analysis. Tris(pentafluorophenyl)(phenylethyl)silane reveals a folded structure due to intramolecular π-stacking interactions, while those with a lower degree of fluorination show either intermolecular π-stacking or no interplay between the aryl groups. A similar folded structure was observed for (4-methylphenethyl)tris(pentafluorophenyl)silane and [2-(naphth-2-yl)ethyl]tris(pentafluorophenyl)silane, both generated from the corresponding trichlorosilanes. In contrast, the inversely fluorinated [2-(pentafluorophenyl)ethyl]triphenylsilane only revealed intermolecular π-stacking interactions. Compounds with tetrafluoropyridyl substituents behave differently; with these compounds, π-stacking is only observed between the fluorinated units. All compounds were analyzed by NMR and IR spectroscopy, elemental analyses and single-crystal X-ray diffraction, and found to have strong H/C/N/F···F and N···C contacts.


2003 ◽  
Vol 58 (5) ◽  
pp. 389-394 ◽  
Author(s):  
Alexander A. Trifonov ◽  
Mikhail N. Bochkarev ◽  
Herbert Schumann ◽  
Sebastian Dechert

Racemic trans-2-(9(H)-fluoren-9-yl)cyclohexanol, C13H9-cyclo-C6H10-OH (1), reacts with two equivalents of potassium naphthalenide in THF to give the dipotassium salt [C13H8-cyclo-C6H10-O]- K2(THF) (2). Recrystallization of 2 from pyridine affords the solvent free salt [C13H8-cyclo-C6H10- O]K2 (3). The reactions of LaI3(THF)4 with one equivalent of 2 or of YbI2(THF)2 with equimolar amounts of 2 produce the alkoxolanthanum diiodide (C13H9-cyclo-C6H10-O)LaI2(DME)2 (4) and the ytterbium dialkoxide (C13H9-cyclo-C6H10-O)2Yb(THF)0.5(5), respectively. [(Me3Si)2N]3Y reacts with three equivalents of 1 with elimination of hexamethyldisilazane and formation of the yttrium trialkoxide (C13H9-cyclo-C6H10-O)3Y (6). The compounds 2 to 5 were characterized by elemental analyses, 1H NMR, 13C NMR and IR spectra. The molecular structure of 4 was determined by single crystal X-ray diffraction.


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