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1Author    Kristallstruktur Neuer, Kai Landskron, Wolfgang SchnickRequires cookie*
 Title    Synthese und  
 Abstract    -diphosphazenium bromide [(NH->)3PNP(NHi)3]Br, nitrate 1(NH2)3PNP(NH2)3][N03], and toluene-4-sulfonate [(NH2)3PNP(NH2)3][CH3C6H4S0 3] have been prepared by anion exchange in aqueous solution. Single crystals were obtained from acetonitrile solutions in a temperature gradient between 60 °C and room temperature. The crystal structures were determined by single crystal X-ray methods at room temperature. ([(NH2)3PNP(NH2)3]Br: P i, Z = 2, a = 596.2(1),b = 744.5(1), c = 1114.4(1) pm, a = 108.78(1), ß = 104.18(1), 7 = 90.64(1)°, R 1 = 0.048, wR2 = 0.104; [(NH2)3PNP(NH2)3][N03]: Pi, Z = 2, a = 550.9(1), b = 796.3(1), c = 1115.7(1) pm, a = 94.45(1), ß = 99.55(1), 7 = 101,53(1)°, R l = 0.033, wR2 = 0.095; [(NH2)3PNP(NH2)3][CH3C6H4S 0 3]: P2,/c, Z = 4, a = 804.1(1), b = 596.1(1), c = 3218.7(3) pm, ß = 94.59(1)°, /?1 = 0.052, wR2 = 0.136). In the solid the three salts consist of discrete [(NHi)3PNP(NH2)3]+ cations and their corresponding anions. The PN4 tetrahedra in [(NH2)3PNP(NH2j3]Br are staggered, while in [(NH2)3PNP(NH2)3][N03] the eclipsed conformation is preferred. The PN4 tetrahedra of [(NH2)3PNP(NH2)3][CH3C 6H4S 0 3] show gauche conformation. 
  Reference    Z. Naturforsch. 54b, 1363—1370 (1999); eingegangen am 13. Juli 1999 
  Published    1999 
  Keywords    3, 3, 3-Hexaamino-lA5, 3A5-diphosphazenium-Salze Synthesis and Crystal Structure of Novel l, l, l, 3, 3, 3-Hexaamino-lA5, 3A5-diphosphazenium Salts Phosphazenes, Ion Exchange, Crystal Structure 1, 1, 1, 3, 3, 3-Hexaamino-lA\3A5 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1363.pdf 
 Identifier    ZNB-1999-54b-1363 
 Volume    54 
2Author    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 
3Author    G. Ernot, Heckm Ann3, Stefan Planka, Ekke­ Hard Fluckb, Dashti-M Anahita, Bernhard Ommertzc, NeumüllercRequires cookie*
 Title    6-Pyridyl-l-aza-2A5,4/.5-diphosphinin - ein 2,2'-Bipyridin-Analogon 6-Pyridyl-l-aza-2/l5,4/l5-diphosphinine - a 2,2'-Bipyridine Analogue  
 Abstract    -Tetrakis(dimethylamino)-lA5,3A5-diphos-phete, (1), reacts with 2-cyano-pyridine to yield 6-pyridyl-l-aza-2/l5,4A5-diphosphinine (3). 3 is cha­ racterized by its 'H , 31P, and 13C NMR, mass, and IR spectra as well as the results of the X-ray struc­ ture analysis. 
  Reference    Z. Naturforsch. 54b, 1478—1481 (1999); eingegangen am 23. August 1999 
  Published    1999 
  Keywords    A5-Diphosphete, l-Aza-2A5, 4A5-diphosphinine, NMR D ata, Crystal Structure l, l, 3, 3 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1478_n.pdf 
 Identifier    ZNB-1999-54b-1478_n 
 Volume    54