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1Author    Gerhard Müller, Hans-Joachim Matheus3, Martin WinklerbRequires cookie*
 Title    Donor-Acceptor Complexes between Simple Phosphines. First Structural Data for an Almost Forgotten Class of Compounds  
 Abstract    Lewis acid-base adducts between simple phosphines have been structurally characterized for the first time in the form of (Me3 P)PBr3 (1) and (MeiPjPB^Bz' (2; Bz' = 3,5-dimethyl-benzyl). On the basis of its solid-state structure the bonding situation in 1 may be described as intermediate between a neutral donor-acceptor complex containing hypervalent phosphorus(III) and an ion pair, according to the resonance formulae Me3 P —► PBn — [Me3 P-PBr2 ]+Br_ . The weak (incomplete) bond formation to the third bromine atom clearly reflects the reluctance of trivalent phosphorus to accommodate more than four electron pairs in its valence shell. (Crystal data for 1: monoclinic P2\ln, a = 7.142(3), b = 16.844(2), c = 8.139(4) A, ß = 106.24(2)°, Z = 4). As a result of the inferior acceptor properties of PB^Bz' as compared to PBr3 , 2 has more ion pair character [MeiP-PBrBz] Br"othan 1. (Crystal data for 2: orthorhombic P 2j 2i2 i, a = 7.063(2), b = 8.578(2)rf c = 25.158(4) A, Z = 4). Both compounds have short P-P bonds (1: 2.264(2); 2: 2.236(2) A). The results are compared with previous IR/Raman and NMR investigations on 1 : 1 and 2 : 1 adducts between organophosphines (as donors) and phosphorus trihalides (as acceptors). 
  Reference    Z. Naturforsch. 56b, 1155—1162 (2001); received July 17 2001 
  Published    2001 
  Keywords    Hypervalence, Phosphines, Lewis Acid-Base Adducts 
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 TEI-XML for    default:Reihe_B/56/ZNB-2001-56b-1155.pdf 
 Identifier    ZNB-2001-56b-1155 
 Volume    56 
2Author    Gerhard Müller, Jörg Brand, SimoneElisabeth JetterRequires cookie*
 Title    Donor-Acceptor Complexes between Organoamines and Phosphorus Tribromide  
 Abstract    Lewis acid-base adducts between NMe3, tmeda (A^A^Af'-tetramethylethylenediamine), and 1.4-dimethylpiperazine as donors and PBr3 as acceptor have been prepared and structurally characterized. NMe3 and tmeda form 1:1 adducts (Me3 N)PBr3 (1) and (tmeda)PBr3 (2), re­ spectively, while 1,4-dimethylpiperazine adds 2 molecules of PBr3 leading to [(1,4-dimethyl-piperazine)(PBr3):] (3). Adduct 2 is found in two modifications 2a and 2b with different crystal and molecular structures. (Crystal data of 1: monoclinic P2\/n, a = 5.983(3), b = 10.821(2), c = 13.877(5) Ä, ß = 99.70(2)°, Z = 4. 2a: monoclinic P2i/c, a = 7.891(1), b = 12.826(1), c = 12.218(2) A ,ß = 102.162(6)°, Z = 4. 2b: monoclinic P2]/n, a = 11.687(2), b = 8.375(1), c = 12.668(1) A, ß = 102.74(1)°, Z = 4. 3: monoclinic P2Jc, a = 6.383(3), b = 16.36(3), c = 8.407(3) A,ß= 101.49(2)°, Z= 2). The molecular structures of 1 and 2 indicate a partially ionic character with a strongly bonded amine and one (1) or two (2) weakly bonded bromine atoms. In 2 the donor tmeda is bonded through both nitrogen atoms to one phosphorus atom. In 3 the 1.4-dimethylpiperazine ring is in chair conformation, the methyl and PBr3 substituents being in equatorial and axial positions, respectively. Due to axial-axial repulsion the N-P donor-acceptor bonds are long while the P-Br bonds are rather uniform in length. 
  Reference    Z. Naturforsch. 56b, 1163—1171 (2001); received July 17 2001 
  Published    2001 
  Keywords    Hypervalence, Phosphines, Lewis Acid-Base Adducts 
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 TEI-XML for    default:Reihe_B/56/ZNB-2001-56b-1163.pdf 
 Identifier    ZNB-2001-56b-1163 
 Volume    56 
3Author    Markus Häp, TheoG. Illes, Thomas Kruck, Karl-Friedrich TebbeRequires cookie*
 Title    Dichloro  
 Abstract    [bis(775-2,4-cyclopentadien-l-yl)aIkylphosphan]zirconium: PR(C5H4)2 ZrCl2 ; R = Me, Et, 'Pr, 'Bu Dichloro[bis(/7r'-2 ,4 -cyclopentadien-l-yl)alkylphosphine]zirconium: PR(C5H4)7ZrCL; R = Me, Et, 'Pr, ?Bu A series of new ansa-zirconocene dichloride compounds [PR(C5H4)2ZrCl2: R = Me (5), Et (6), 'Pr (7), ?Bu (8)] with phosphorus as bridging atom between the cyclopentadienyl rings have been prepared, isolated, and characterised by 'H, i3C, 31P NMR spectroscopy, mass spectrometry and elemental analysis. The X-ray structure of 5 is reported. 
  Reference    Z. Naturforsch. 54b, 482—486 (1999); eingegangen am 22. Dezember 1998 
  Published    1999 
  Keywords    Zirconium Ansa-Metallocene, Cyclopentadienyl, Phosphine, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0482.pdf 
 Identifier    ZNB-1999-54b-0482 
 Volume    54 
4Author    Joachim Bruckmann, Carl Krüger, Frank LutzRequires cookie*
 Title    Systematic Structural Investigations on Phosphines  
 Abstract    This work contributes to the systematic investigation of phosphines. In an attem pt to deter­ mine the nature, shape, volume and direction of the lone pairs at the phosphorus atoms in phosphines, high resolution X-ray structure analyses of triphenylphosphine, tris(p-methoxy-phenyl)phosphine, bis(2,4,6-triisopropylphenyl)phosphine, 1,1 -bis(diphenylphosphino)ethene and 4,5,6-triphenyl-4-phosphaspiro[2.4]hept-5-en have been carried out. New valence force field param eters (TRIPOS force field) are presented which were developed on the basis of the molecular structures of the free phosphines. The results of crystal growing experiments using zone melting techniques are summarized. 
  Reference    Z. Naturforsch. 50b, 351—360 (1995); received Septem ber 20 1994 
  Published    1995 
  Keywords    Phosphines, Molecular Modeling, Crystal Growing, High Resolution X-Ray Analysis 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-0351.pdf 
 Identifier    ZNB-1995-50b-0351 
 Volume    50 
5Author    ViktorP. Balema, Steffen Blaurock, Evamarie Hey-HawkinsRequires cookie*
 Title    Synthesis and Molecular Structure of a Superbulky Tertiary Phosphine: Bis[2-phenyl-l,2-dicarba-c/oso-dodecaboran-l-yl(12)]phenylphosphine  
 Abstract    Bis[2-phenyl-l,2-dicarba-c/oso-dodecaboran-l-yl(12)]phenylphosphine (2) was obtained in 91% yield from phenyldichlorophosphine and two equivalents of l-lithium-2-phenyl-l ,2-dicarba-c/o5o-dodecaborane(12) in ether and characterized by spectroscopy (3IP, 1 B, 'H, l3C NMR; IR) and by X-ray structure determination. 
  Reference    Z. Naturforsch. 53b, 1273—1276 (1998); received May 20 1998 
  Published    1998 
  Keywords    Synthesis, Molecular Structure, X-Ray Data, NMR Data, Phosphine 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1273.pdf 
 Identifier    ZNB-1998-53b-1273 
 Volume    53 
6Author    G. Ünter Schmid, AbdelK. Boutrid, Eva-M Aria KreuzerRequires cookie*
 Title    Azaborolyl-Komplexe, 25 Das (l-terf-Butyl-2-methyl-l H-l,2-azaborolyl)cobalt-Fragment (AbCo) als Synthesebaustein Azaborolyl Complexes, 25 The (l-/ej7-Butyl-2-methyl-l H -l,2-azaborolyl)cobalt Fragm ent (AbCo) as Building Block in Synthesis  
  Reference    Z. Naturforsch. 45b, 1235—1242 (1990); eingegangen am 19. März 1990 
  Published    1990 
  Keywords    1 H -l, 2-A zaborolyl-cobalt, Ethene, Phosphine, Carbonyl Derivatives, Cobalt Clusters (di-, tri-, and tetranuclear) 
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 TEI-XML for    default:Reihe_B/45/ZNB-1990-45b-1235.pdf 
 Identifier    ZNB-1990-45b-1235 
 Volume    45