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1994 (1)
1987 (1)
1982 (2)
1Author    Peter Schreiber, Karl Wieghardt, Ulrich Flörke, Hans-Jürgen HauptRequires cookie*
 Title    Synthese von Wolframkomplexen  
 Abstract    des Typs [ L W (C O) 3X ] + (X = H , F, Br; L = 1,4,7-Triazacyclononan). Die Kristallstrukturen von [L W (C O) 3B r]B F 4 und [L W (C O) 3H ] 2[W O C l5] • h 2o Synthesis o f Tungsten Complexes o f the Type [L W (C O)3X ] + (X = H, F, Br; L = 1.4,7-triazacyclononane). The Crystal Structures o f [L W (C O)3Br]BF4 and [L W (C O)3H ]2[W O C l5] • H 20 The reaction of LW (C O), (L = 1,4,7-triazacyclononane) with Br2 in CHCl, yields orange [L W (C O)3Br](Br3) which was converted to its BF4~ salt. [L W (C O)3Br]BF4 crystallizes in the triclinic space group P 1 (a = 8.273(3), b = 8.628(2), c = 13.034(3) Ä , a = 80.10(2), ß = 72.69(2). y = 61.14(2)°, Z = 2); it consists of cations [L W (C O)3Br] + , with seven-coordinate W atoms, and BF4 -anions. The corresponding salt [L W (C O)3F](PFft) was obtained from L W (C O)3 with 20% aqueous HF in the presence of air and addition of NaPF6. The analogous reaction with 37% aqueous HC1 affords green crystals of [L W (C O)3H ]2[W OCl5] • H 20 which crystallize in the mono­ clinic space group P2,/c (a = 12.234(4), b = 18.853(7), c = 14.609(5) Ä . ß = 105.65(3)°, Z — 4). The W atoms in the [L W (C O)3H ]+ cations are seven-coordinate; the six-coordinate [W OCl5]: anions are not disordered. The W = 0 distance is short (1.72(1) Ä), the mean equatorial W —Cl distance is 2.390 Ä whereas the W —Cl bond distance trans to the W = 0 group is 2.562(5) Ä. 
  Reference    Z. Naturforsch. 42b, 1391 (1987); eingegangen am 2. Juli 1987 
  Published    1987 
  Keywords    Tungsten Complexes, X-Ray, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1391.pdf 
 Identifier    ZNB-1987-42b-1391 
 Volume    42 
2Author    Albini, H. KischRequires cookie*
 Abstract    Chromium and tungsten carbonyls react with 3,3,4,4-tetramethyl-l,2-diazetine (1) or its mono-N-oxide (2) to form complexes (l)M(CO)5, (l)2M(CO)4, (l)M2(CO)io, (l)2M2(CO)8, (l)3M2(CO)6 or (2)M(CO)5 and (2)2M(CO)4, resp. In the reactions of 2 some deoxygenation affords complexes of 1 as by-products. The stability of these and other complexes of the N=N group is related to the ring size of the cyclic diazene ligand. 
  Reference    Z. Naturforsch. 37b, 468—472 (1982); received November 13 1981 
  Published    1982 
  Keywords    I, 2-Diazetines, 1, 2-Diazetine-N-oxide, Chromium Complexes, Tungsten Complexes 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0468.pdf 
 Identifier    ZNB-1982-37b-0468 
 Volume    37 
3Author    Marianne Baudler, Franz Salzer, Josef HahnRequires cookie*
 Title    Beiträge zur Chemie des Phosphors, 120 [1] Carbonyl-Triorganylcyclotriphosphan-Komplexe von Chrom und Wolfram Contributions to the Chemistry of Phosphorus, 120 [1] Carbonyl-Triorganylcyclotriphosphane Complexes of Chromium and Tungsten  
 Abstract    The reaction of triorganylcyclotriphosphanes, (RP)3 (R = i-Pr, £-Bu), with metal carbonyl-tetrahydrofuran complexes, M(CO)sTHF (M = Cr, W), yields the novel mono-nuclear and binuclear cyclotriphosphane-carbonylmetal complexes (RP)3M(CO)5 (R = i-Pr, *-Bu; M = Cr, W) 1-4 and (RP)3[M(CO)5]2 (R = t-Pr, M = Cr) 5, respectively. They are remarkably stable both thermally and to oxidation. Their structures have been elucidated by 31 P NMR spectroscopic investigations. The cyclotriphosphane functions as a 2-or a 4-electron donor, respectively, and behaves as a Ti-acceptor comparable to PI13P. Bei unseren Untersuchungen über Triorganyl-cyclotriphosphane (RP)3 [2, 3] konnten in den letz-ten Jahren bemerkenswert beständige Vertreter dieser Substanzklasse in reiner Form dargestellt werden [4-6, 1]. In diesem Zusammenhang interes-sierte die Frage, inwieweit diese Verbindungen in der Lage sind, an ein Übergangsmetall zu koor-dinieren [7]. Der einzige bislang bekannte Cy-clotriphosphan-Komplex, das Triphenylcyclotri-phosphan-tris(cyclopentadienyldicarbonylmangan), (C6H5P)3[Mn(CO)2CöH5]3, wurde unerwartet beim Versuch der Darstellung eines Phosphiniden-Kom-plexes erhalten [10]. Im folgenden wird über Syn-these und Eigenschaften der ersten ein-und zwei-kernigen Übergangsmetall-Komplexe mit Triorga-nylcyclotriphosphan-Liganden berichtet. Präparative Ergebnisse 
  Reference    Z. Naturforsch. 37b, 1529—1533 (1982); eingegangen am 26. Juli 1982 
  Published    1982 
  Keywords    Tri-isopropylcyclotriphosphane, Tri-£er£-butylcyclotriphosphane, Cyclotriphosphane Complexes, Chromium Complexes, Tungsten Complexes 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-1529.pdf 
 Identifier    ZNB-1982-37b-1529 
 Volume    37 
4Author    Hans-Jürgen Plinta, Ion Neda, Reinhard SchmutzlerRequires cookie*
 Title    .3-Dimethyl-l,3-diaza-2-R-5,6-benzo-2 A3-phosphorinan-4-one (R = F, Me2N, 2-Methylpiperidino, MeC(: 0 ) N H -) als Liganden in Übergangsmetallkomplexen; Synthese und Struktur von Dichloro-Platin(II)-und Tetracarbonyl-Metall(O)- Koordinationsverbindungen (Metall = Cr, Mo und W) 1.3-Dimethyl-l,3-diaza-2-R-5,6-benzo-2/l3-phosphorinan-4-ones (R = F, Me2N, 2-Methylpiperidino, MeC(: 0 ) N H -) as Ligands in Transition-Metal Complexes; Synthesis and Structure o f Dichloro-Platinum(II)-and Tetracarbonyl-Metal(O) Coordination Compounds (Metal = Cr, Mo and W)  
 Abstract    -2-fluoro-5,6-benzo-l,3,2-phosphorinane-4-one (1) reacted with (COD)PtCl2 (COD = 1,5-cyclooctadiene) or K2PtCl4 to give the c/s-dichloro-platinum(II) complex (2). The reactions of 1 with the tetracarbonyl norbornadiene derivatives of Cr, Mo and W furnished the complexes 3 -6 . In the case of the chromium and tungsten complexes the trans-isomers 3 and 6 were formed, due to a c/s-?ra«s-isomerization. Room temperature and low temperature 3IP NMR spectra of a mixture of 5 and 6 show no significant temperature dependence of the cis-trans equilibrium. The reaction of 1 with the pentacarbonyl tetrahydro-furan derivative of W led to the product 7. The spirophosphoranes 8 and 9 were obtained in low yields. The analogous reactions of 10, 15 and 20 with (COD)PtCl2 and the tetracarbonyl norbornadiene derivatives of Cr and Mo furnished the coordination compounds 1 1 -1 4 , 16-18, 21 and 23. In the case of all chromium complexes only the /rarcs-isomers 11,16 and 21 were formed, whereas in the case of molybdenum m-fraH.s'-isomer mixtures 12 and 13, as well as 17 and 18 were obtained. An attempt to obtain the cis-isomer of the molybdenum complex 22 failed. In the case of platinum the expected m-complexes 14 and 23 were formed, while the attempted synthesis of 19 was unsuccessful. All these results are interpreted in terms of both steric and electronic factors. The ligands 1, 10, 15 and 20 coordinate via phosphorus. The va­ lidity of the concept of hard and soft acids and bases (HSAB) was confirmed. The characteri­ zation of 2 -7 , 1 1-14, 16-18, 21 and 23 rests, especially, on their 'H, 13C and 3IP NMR spec­ tra, and their mass and infrared spectra. 31p -3,p coupling constants 2/(PP) for the cis-coordi­ nated complexes 4, 5 and 14 involving two equivalent phosphorus ligands are also reported. 
  Reference    (Z. Naturforsch. 49b, 100—110 [1994]; eingegangen am 17. Mai 1993) 
  Published    1994 
  Keywords    Platinum Complexes, Chromium Complexes, Molybdenum Complexes, Tungsten Complexes, NMR Spectra 1, 3-Dimethyl-l, 3-diaza 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0100.pdf 
 Identifier    ZNB-1994-49b-0100 
 Volume    49