| | 1 | Author
| Gerhard Müller, Hans-Joachim Matheus3, Martin Winklerb | Requires 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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| default:Reihe_B/56/ZNB-2001-56b-1155.pdf | | | | Identifier
| ZNB-2001-56b-1155 | | | | Volume
| 56 | |
| 2 | Author
| Gerhard Müller, Jörg Brand, SimoneElisabeth Jetter | Requires 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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| default:Reihe_B/56/ZNB-2001-56b-1163.pdf | | | | Identifier
| ZNB-2001-56b-1163 | | | | Volume
| 56 | |
| 3 | Author
| Markus Häp, TheoG. Illes, Thomas Kruck, Karl-Friedrich Tebbe | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-0482.pdf | | | | Identifier
| ZNB-1999-54b-0482 | | | | Volume
| 54 | |
| 4 | Author
| Joachim Bruckmann, Carl Krüger, Frank Lutz | Requires 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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| default:Reihe_B/50/ZNB-1995-50b-0351.pdf | | | | Identifier
| ZNB-1995-50b-0351 | | | | Volume
| 50 | |
| 5 | Author
| ViktorP. Balema, Steffen Blaurock, Evamarie Hey-Hawkins | Requires 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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| default:Reihe_B/53/ZNB-1998-53b-1273.pdf | | | | Identifier
| ZNB-1998-53b-1273 | | | | Volume
| 53 | |
| 6 | Author
| G. Ünter Schmid, AbdelK. Boutrid, Eva-M Aria Kreuzer | Requires 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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| default:Reihe_B/45/ZNB-1990-45b-1235.pdf | | | | Identifier
| ZNB-1990-45b-1235 | | | | Volume
| 45 | |
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