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1999[X]
1Author    BemdW. Rackm, SergeiV. PonomarevbRequires cookie*
 Title    Decomposition of Ethoxyethynyl(trimethyl)tin -Studied by 119Sn and 13 C NMR Spectroscopy  
 Abstract    A The thermally induced decomposition o f ethoxyethynyl(trimethyl)tin (1) was studied by ll9Sn NM R which revealed the formation o f bis(trimethylstannyl) ketene (2) as the major product, bis(trimethylstannyl) acetic acid ethyl ester (3) as a minor product, and a small amount o f tetramethyltin (4). Full NM R data sets, including coupling constants and isotope induced chemical shifts 1 _ \ 12 13C(1 l9Sn) are provided for 1 -3 . The first example o f ultra-high resolution " 9Sn NM R is shown. 
  Reference    Z. Naturforsch. 54b, 705 (1999); received February 23 1999 
  Published    1999 
  Keywords    lkynes, Ketenes, Tin, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0705.pdf 
 Identifier    ZNB-1999-54b-0705 
 Volume    54 
2Author    Nils Wiberg, Hans-Wolfram Lemer, Susanne Wagner, Heinrich Nöth+, Thomas Seifert+Requires cookie*
 Title    On an Octastannanediide R*6Sn8[Na(THF)2]2 and the Possible Existence of an Octastannane R*6Sn8 [ 1 ]  
 Abstract    The black, air and moisture sensitive octastannanediide R*6Sn8[Na(THF)2]2 (4) (R* = Si/Bu3) is prepared by reaction of Sn[N(SiM e3)2]2 with R*Na in rBuOMe at -78°C . Red brown octa­ stannane R*6Sn8 (5) is formed by thermolysis of the tristannacyclopropene R*4Sn3 in benzene at 100 °C. According to the result of the X-ray structural analysis, 4 contains a Sn8 cubane with six Sn atoms each connected with R* and two at the end o f a space diagonal connected with Na(THF)2. A preliminary X-ray structure analysis shows 5 to adopt the same Sn8 cubane structure as 4 with two bare Sn atoms at the end of a space diagonal. 
  Reference    Z. Naturforsch. 54b, 877—880 (1999); eingegangen am 1. April 1999 
  Published    1999 
  Keywords    Silicon, Tin, Sodium, Tincluster, X-Ray Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0877.pdf 
 Identifier    ZNB-1999-54b-0877 
 Volume    54 
3Author    BerndW. Rackmeyer1 ', Saqib Alib, Wolfgang Storch0, Martina VosteencRequires cookie*
 Title    2-[N,N-Bis(trimethylstannyl)amino]pyridine and Bis[N-(N-trimethyIsiIyI- 2-aminopyridyI)]dimethyltin -Intramolecular N-Sn Co-ordination  
 Abstract    2-[N,N-Bis(trimethylstannyl)amino]pyridine (1), bis[N-(N-trimethylsilyl-2-aminopyridyl)]-dimethyltin (2) and bis[N-(N-trimethylsilyl-2-amino-3-methyl-pyridyl)]dimethyltin (3) were prepared and characterized by 'H, i3C, l5N, 29Si and ll9Sn NMR spectroscopy. In the case of 1, intramolecular pyridine-N-Sn co-ordination was established by the low temperature ll9Sn NMR spectra which show two resonance signals, one for a penta-co-ordinate and one for a tetra-co-ordinate tin site. In the cases of 2 and 3, intramolecular pyridine-N-Sn co-ordination follows conclusively from l3C, l5N and ll9Sn NMR parameters. In contrast with the known behaviour of the corresponding trimethyltin derivative, the methyl group in 3-position of the pyridine ring does not prevent this type of co-ordination in 3. 
  Reference    Z. Naturforsch. 54b, 1165—1169 (1999); received June 17 1999 
  Published    1999 
  Keywords    Tin, Amines, Pyridine, Co-ordination, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1165.pdf 
 Identifier    ZNB-1999-54b-1165 
 Volume    54 
4Author    KurtO. Klepp, Ferdinand Fabian, *. Sonderdruckanforderungen, Prof Kurt, O. KleppRequires cookie*
 Title    Darstellung und Kristallstruktur von Rb6Sn2S7 New Chalcogenometallates with Binuclear Anions, I: Preparation and Crystal Structure of Rb6Sn2S7  
 Abstract    Colorless crystals of the new thiostannate Rb6Sn2S7 were obtained by reacting a stoichio­ metric melt of Rb2S, Sn and S at 700°C. The compound is orthorhombic, oP60, s.g. f '2,2,2, (No. 19) with a = 9.982(4), b = 13.45(1), c = 15.20(1) A; Z = 4. The crystal structure was determined from diffractometer data and refined to a conventional R of 0.043 (1380 Fo's, 137 variables). The crystal structure contains dimeric anions, [Sn2S7]2 -, which are built up by slightly distorted SnS4 tetrahedra sharing a common sulfur atom. The mean Sn-S bond length calculates as 2.384 Ä, the bond angle on the bridging S is 110.4°. The structure contains six independent Rb-cations which are coordinated to 5-6 sulfur atoms in irregular configurations. Neue Chalkogenometallate mit binuklearen Anionen, I: 
  Reference    Z. Naturforsch. 54b, 1505—1509 (1999); eingegangen am 13. September 1999 
  Published    1999 
  Keywords    Crystal Structure, Chalcogenides, Thiostannates, Rubidium, Tin, Sulfur 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1505.pdf 
 Identifier    ZNB-1999-54b-1505 
 Volume    54 
5Author    M. Ax Herberhold, U. Do Steffl, BerndW. RackmeyerRequires cookie*
 Title    l,3-Distanna-2-phospha-[3]ferrocenophanes -Synthesis, Reactivity and NMR Spectroscopic Properties  
 Abstract    -organo(R)-l,3-distanna-2-phospha-[3]ferrocenophanes [R = Me (2a), rBu (2b), CöH i i (2c), Ph (2d)] and one arsa-analogue 2d(As) were obtained from the reaction of l,l'-bis(chlorodim ethylstannyl)ferrocene 1 with either bis(trimethylsilyl)methylphosphane or the dilithio derivatives, Li2PR and Li^AsPh, respectively. All compounds 2 react with chalco-gens (oxygen, sulfur, selenium) by cleavage of the Sn-P bonds and formation of the known l,3-distanna-2-chalcogena-[3]ferrocenophanes. In contrast, 2d traps pentacarbonylmetal frag­ ments [M(CO)5] to give the stable phosphane complexes [M = Cr (4d), Mo (5d), W (6d)]. The l,l'-bis(diorganophosphanostannyl)ferrocenes [R = fBu (3b), Ph (3d)] were prepared for comparison of NMR data. The ferrocenophanes 2 are fluxional with respect to fast movement of the cyclopentadienyl rings which induces inversion at the pyramidal phosphorus atom. This dynamic process is slow in the cases of 2d(As) and of the pentacarbonyl complexes 4d -6d. All new compounds were characterised by 'H , i3C, 31P and 1 l9Sn NMR spectroscopy. Various 2D heteronuclear shift correlations {e.g. 11P /1H and ll9Sn/'H) were carried out for the com ­ pounds 2 and also for non-cyclic derivatives such as bis(trimethylstannyl)phenvlphosphane and -arsane in order to determine absolute signs of coupling constants [e.g. 7(n S n,''P) > 0 and 2J(] l9Sn,' l7Sn) < 0]. The NM R data suggest that the molecular frameworks of the ferroceno­ phanes 2 are not particularly strained. 
  Reference    (Z. Naturforsch. 54b, 57—62 [1999]; received July 28 1998) 
  Published    1999 
  Keywords    Ferrocene, Tin, Phosphorus, NMR Data, Coupling Signs l, l, 3, 3-Tetramethyl-2 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0057.pdf 
 Identifier    ZNB-1999-54b-0057 
 Volume    54