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1998[X]
1Author    Max Herberhold, Silke Gerstmann, Bernd WrackmeyerRequires cookie*
 Title    Tetrakis(sulfurdiimido)silane, -germane and -stannane  
 Abstract    Two tetrakis(sulfurdiimido)silanes [Si(NSNR)4 (R = rBu la, SiMe3 lb)], two germanes [Ge(NSNR)4 (R = rBu 2a, SiMe3 2b)] and one stannane [Sn(NSN?Bu)4Sn 3a] were prepared and characterised by 'H, l3C, i5N, 29Si and ll9Sn NMR spectroscopy in solution, and 3a was also studied in the solid state by 1 l9Sn CP/MAS NMR. Whereas la,b and 2a,b are monomeric in solution, the 119Sn NMR data suggest that 3a is associated both in solution and in the solid state, and that the tin atoms are hexa-coordinated. The attempted stepwise synthesis of la by using one, two, three or four equivalents of K[(NSN)rBu] led to mixtures of la with Cl3Si(NSNrBu) 4a, Cl2Si(NSN/Bu)2 5a, and ClSi(NSNfBu)3 6a. Only one sulfurdiimido ligand of the silane la reacted with hexachlorodisilane by oxidative addition and cleavage of the Si-Si bond to give the new heterobicyclic derivative 7a which is held together by two different coordinative N-Si bonds. 
  Reference    Z. Naturforsch. 53b, 573—580 (1998); received March 30 1998 
  Published    1998 
  Keywords    Silicon, Germanium, Tin, Sulfur Diimides, Heterocycles, NMR Data 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0573.pdf 
 Identifier    ZNB-1998-53b-0573 
 Volume    53 
2Author    Matthias Westerhausena, Mathias Kroftaa, Nils Wiberga, Jörg Knizeka, Heinrich Nötha, Arno PfitznerbRequires cookie*
 Title    Tetrazinn(II)-und Bariumtrizinn(II)-tetrakis[/i3 -tri-ter/-butyIsilylphosphan- diid]-Verbindungen mit einem Tetrametallatetraphosphacuban-Gerüst Tetratin(II) and Barium Tritin(II) Tetrakis[//3-tri-rm-butylsilylphosphandiide] Compounds with a Tetrametallatetraphosphacubane Core  
 Abstract    The metalation o f tri-terr-butylsilylphosphane with bis[bis(trimethylsilyl)amino]stannylen yields nearly quantitatively the tetrameric tin(II) tri-terf-butylsilylphosphandiide with a central Sn4 P4 cubane moiety. Barium bis[tri-/£Tf -butylsilylphosphanide] is accessible via the reaction o f tri-?£T/-butylsilylphosphane with barium bis[bis(trimethylsilyl)amide] in the molar ratio 2 : 1 . This phosphanide reacts with bis[bis(trimethylsilyl)amino]stannylen to give barium tritin(II) tetrakis[/i3-tri-ter?-butylsilylphosphandiide]. Crystallographic data of 1: P 21212), T = 193 K, a = 1532.6(3), b = 2120.2(4), c = 2194.0(5) pm, V = 7.129(3) nm3, Z = 4, R, = 0.0360 (9132 observed data [I > 2a(f)]), wR2 = 0.1064 (all data); crystallographic data of 3: P 2,/c, T= 193 K, a = 1927.35(1), b = 1799.27(2), c = 2201.35(2) pm, ß = 93.010(1)°, V= 7.6234(1) nm3, Z = 4, R, = 0.0321 (11993 observed data [I > 2cr(/)]), wR2 = 0.0772 (all data). 
  Reference    Z. Naturforsch. 53b, 1489—1493 (1998); eingegangen am 3. Juli 1998 
  Published    1998 
  Keywords    Arene Complexes, Barium, Heterocubanes, Phosphorus, Tin 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1489.pdf 
 Identifier    ZNB-1998-53b-1489 
 Volume    53 
3Author    Anja Loose, WilliamS. SheldrickRequires cookie*
 Title    Solventothermal Synthesis of the Lamellar Selenidostannates(IV) A2Sn4Se9*H20 (A = Rb, Cs) and Cs2Sn2Se6  
 Abstract    Reaction of A 2C O 3 with Sn and Se in an H 2O /CH 3OH mixture at 115 -130°C affords the isotypic lamellar selenidostannates A2Sn4Se9-H20 1 (A = Rb) and 2 (A = Cs). The polyanions ^ [Sn4Se92~] exhibit S ^ S e s molecular building units, in which two adjacent Sn(IV) atoms of an Sn4Se4 8-membered ring are bridged by an additional Se atom. These units connect through (SnSe)2 4-mem bered rings to afford a 44 anionic net with 16-membered cavities. Cs2Sn2Se6 (3) may be prepared by methanolothermal reaction of CstCO^ with SnSe and Se at 130°C and contains porous 2 [SnTSeö2 -] sheets in which [SnSes--] ribbons are linked through Se-Se bonds. The resulting 4 net displays 14-membered pores in which the Cs cations reside. 
  Reference    Z. Naturforsch. 53b, 349—354 (1998); received December 29 1997 
  Published    1998 
  Keywords    Tin, Selenium, Selenidostannates(IV), Lamellar Structures, Solventothermal Synthesis 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0349.pdf 
 Identifier    ZNB-1998-53b-0349 
 Volume    53 
4Author    Bernd Wrackmeyer3, Jürgen Weidinger3, Heinrich Nöthb, Wolfgang Storchb, Thomas Seifertb, Martina VosteenbRequires cookie*
 Title    Determination of Coupling Signs 17 (119Sn, 15N ) and 2/ ( 119Sn, 117Sn) in Trimethylstannylamines  
 Abstract    The l5N-labelled trimethylstannylamines 1 -3 [(M e3Sn)3N, (M e3Sn)2NPh, (M e3Sn)2N-BCgHi4 (BCgHi4 = 9-borabicyclo[3.3.0]nonyn and the non-labelled 4, Me3 Sn-N(BC8Hi4)2 , were prepared and studied by 1H, 1 C, l5N and l9Sn NMR. The l5N ultrahigh resolution NMR spectra of 1 revealed otherwise unobserved parameters such as 2/ (15N ,S n ,'C) and the isotope induced chemical shift 2 zAl2/l3C (l5N). ll9Sn NM R spectra of 1, recorded under similar con­ ditions, also show new parameters such as V (' |ySn,N,Sn,l3C) which are not resolved in the non-labelled derivative. By using various types o f two-dimensional heteronuclear shift corre­ lations, absolute coupling signs o f l7 (l l9 Sn,15N) (all < 0) in 1 -3 were determined. By the same techniques it proved possible to confirm the negative sign o f :7(Sn,Sn) (-195.4 Hz) in 1. In contrast, the coupling constants 27(Sn,Sn) for 2 (+71.7) and 3 (+62.0) possess a positive sign. This sign inversion, observed here for the first time for apparently similar compounds, demonstrates the enormous influence o f substituents on the nature o f the lone pair o f electrons at the nitrogen atom. It also shows that these experiments for sign determinations o f coupling constants are necessary in order to interpret these data correctly. 
  Reference    Z. Naturforsch. 53b, 1494—1500 (1998); received July 30 1998 
  Published    1998 
  Keywords    Tin, Amines, NM R Data, Ultrahigh Resolution, Coupling Sign Determination 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1494.pdf 
 Identifier    ZNB-1998-53b-1494 
 Volume    53