Crystal and Molecular Structures of the Sulfurization and Selenation Products of Bis[bis(trimethylsilyl)amino]germanium(II). Crystal Structure of (Triphenylphosphine)gold(I) Bis(trimethylsilyl)amide

2000 ◽  
Vol 55 (5) ◽  
pp. 347-351 ◽  
Author(s):  
Gerald L. Wegner ◽  
Alexander Jockisch ◽  
Annette Schier ◽  
Hubert Schmidbaur

Treatment of bis[bis(trimethylsilyl)amino]germanium(II) with elemental sulfur or selenium affords high yields of the corresponding monosulfide [(Me3Si)2N]2GeS and selenide [(Me3Si)2N]2GeSe, respectively. The crystalline products have now been shown to be cyclic dimers with (GeS/Se)2 four-membered rings by X-ray single crystal structure analysis. The crystal structure of (triphenylphosphine)gold(I) bis(trimethylsilyl)amide (Ph3P)Au-N(SiMe3)2 has also been determined. The molecule is a monomer with a tricoordinate nitrogen atom in a planar configuration [Si2NAu]. The compound does not undergo insertion of the bis[bis(trimethylsilyl)amino]germylene.

1977 ◽  
Vol 32 (12) ◽  
pp. 1416-1420 ◽  
Author(s):  
Omar Jabay ◽  
Hans Pritzkow ◽  
Jochen Jander

The crystal and molecular structures of N-bromobenzamide (NBB), N-bromosuccinimide (NBS), and N,N-dibromobenzenesulfonamide (NBBS) were determined by X-ray structure analysis. The nitrogen atoms in NBB and NBS have a trigonal planar coordination (sp2) and the N—Br distances lie in the same range (1.82 A, 1.84 A). The N—Br distance in NBBS, where the nitrogen atom is sp3-hybridized, is somewhat longer (1.88 A). In these structures the molecules are connected by O···H—N (NBB), O···Br—N (NBS) or N···Br—N (NBBS) intermolecular bonds forming endless chains; positivated hydrogen atoms or, in case that they are absent, positivated bromine atoms act as electron acceptors with oxygen or sp3- hybridized nitrogen atoms. These results suggest, that in solid nitrogen tribromide, the crystal structure of which cannot be determined, the nitrogen atoms will be sp3-hybridized and intermolecular contacts via N—Br···N will occur.


1994 ◽  
Vol 49 (7) ◽  
pp. 939-949 ◽  
Author(s):  
Axel Fischer ◽  
Ion Neda ◽  
Thomas Kaukorat ◽  
Ralf Sonnenburg ◽  
Peter G. Jones ◽  
...  

Abstract The reaction of 4,5-benzo-2-chloro-3-methyl-1,3,2-oxazaphosphorinan-6-one 1 with 1,2-bis- (trimethylsiloxy)ethane led to the bisphosphoryl species 2a and to the isomeric bisphosphite derivative 2b. The reaction of 1 with heptamethyldisilazane furnished the expected diphos­phorus compound 3, with two λ3P(III) atoms linked by a methylamino group. Substitution of the chlorine atom of 1 by the 2-chloroethylamino and bis(2-chloroethyl)amino group led to the oxazaphosphorinanones 4 and 6. By oxidation of 4 with the hydrogen peroxide/urea 1:1-adduct, the phosphoryl compound 5 was formed. Oxidation of 4,5-benzo-2-diethyl- amino-3-methyl-1,3,2-oxazaphosphorinan-6-one 7 [1] with hydrogen peroxide, sulfur and se­lenium led to the corresponding phosphoryl, thiophosphoryl and selenophosphoryl com­pounds 8-10. Analogously, the reaction of the dimethylamino- and acetamido-substituted derivatives 11 and 13 [1] with elemental sulfur furnished the thiophosphoryl compounds 12 and 14. X-ray crystal structure determinations of 4 and 14 confirmed the molecular structures, proposed in accord with NMR spectroscopic and mass spectrometric data. The heterocyclic rings are essentially planar. In 14 a hydrogen bond N-H···O (amide) is observed.


2005 ◽  
Vol 60 (5) ◽  
pp. 569-571 ◽  
Author(s):  
Ali Ramazani ◽  
Ali Morsali ◽  
Bijan Ganjeie ◽  
Ali Reza Kazemizadeh ◽  
Ebrahim Ahmadi ◽  
...  

Selenourea reacts with dialkyl acetylenedicarboxylates under solvent-free conditions to form 1:1 adducts, which undergo a cyclization reaction to produce alkyl Z-2-(2-amino-4-oxo-1,3-selenazol- 5(4H)-ylidene)acetates, in good yields. The stereochemistry of the ethyl Z-2-(2-amino-4-oxo-1,3- selenazol-5(4H)-ylidene)acetate was established by X-ray single crystal structure analysis. The reaction is completely stereoselective.


1998 ◽  
Vol 53 (12) ◽  
pp. 1475-1482 ◽  
Author(s):  
Prit Singh ◽  
Sudha Singh ◽  
Vishnu D. Gupta ◽  
Heinrich Nöth

Abstract Tris-thiobenzoates, Arsenic, Antimony, Bismuth Tris-thiobenzoates of arsenic, antimony and bismuth, M(SOCR)3 have been obtained from their oxides and characterized. In the X-ray crystal structure determinations of these, the group 15 atom and the three covalently bonded sulfur atoms are found to constitute a trigonal pyramid, the central atoms lie at a C3 axis. In the bismuth complex the thiobenzoate ligand tends to chelate. However, three comparatively short intermolecular M···S interactions are significant features for these molecules resulting in stacking of trigonal prisms providing an essentially six coordinate environment around arsenic and antimony and a nine-coordinate one for bismuth. The structure of PhSb(SOCPh)2 can be considered


Author(s):  
H. J. Berthold ◽  
E. Vonholdt ◽  
R. Wartchow ◽  
T. Vogt

AbstractNHA single crystal structure analysis of NThe deuterated compound NThe structures of the ordered low temperature phases will be reported separately.


Synlett ◽  
2021 ◽  
Author(s):  
Hong-Wu Zhao ◽  
Xiao-Fan Bi ◽  
Hai-Liang Pang ◽  
Zhe Tang ◽  
Heng Zhang ◽  
...  

In the presence of Na2CO3, the conjugate addition between α-halogeno hydrazones and nitroso compounds proceeded readily, thus delivering multifunctionalized nitrones in the reasonable chemical yields with excellent strereoselectivities. The chemical structure and stereochemical configuration of title chemical entities were unambiguously identified by an X-ray single crystal structure analysis.


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