Wilhelm Kuchen

Heinrich-Heine-Universität Düsseldorf, Düsseldorf, North Rhine-Westphalia, Germany

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Publications (188)478.26 Total impact

  • K. DIEMERT · T. HAHN · W. KUCHEN
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    ABSTRACT: ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.
    No preview · Article · Sep 2010 · ChemInform
  • [Show abstract] [Hide abstract]
    ABSTRACT: ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.
    No preview · Article · May 2010 · ChemInform
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    ABSTRACT: The dissociative ionization by electron impact (70 eV) of tetraphosphorus trisulfide, P4S3, yields [P3S]+ and [PZS]+0 ions whose structures have been investigated by means of Coliisionai Activation (CA) mass spectra. Using the technique of Neutralization-Reionization mass spectrometry (NRMS) it is shown that both ions can be reduced to the corresponding neutral molecules. Thus, triphosphorus sulfide and diphosphorus sulfide are viable molecules in the rarefied gas phase. The results of ab initio MO calculations were used to interpret the experimental findings. Tetrahedral (C3v) and triangular (C2v) structures are proposed for the [P,S]+ and [PZS]+0 ions respectively.
    No preview · Article · Mar 2010 · ChemInform
  • T. Wong · J. K. Terlouw · H. Keck · W. Kuchen · P. Tommes
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    ABSTRACT: Using the technique of neutralization-reionization mass spectrometry (NRMS) we have shown that the elusive thioxophosphane H - P=S and its tautomer H - S - P, (thiohydroxy)phosphinidene, are stable molecules in the gas phase. H - S - P•+ radical cations, generated by electron impact ionization of diethylphosphine sulfide, (C2H5)2HP=S, are cleanly reduced to H - S - P; whereas H - P=S•-anions, generated in a negative chemical ionization (NCI) experiment with the diethylphosphine sulfide, are readily oxidized to H - P=S. Double collision experiments on the 34S isotopomers of the two tautomeric species were used to confirm the connectivity of the atoms. H - S - P is the first example of a molecule of the composition "XPS" (e.g., X = F, Cl, or Br) in which P does not take the central position.
    No preview · Article · Feb 2010 · ChemInform
  • K. DIEMERT · W. KUCHEN · P. STANIEK · H. WUNDERLICH
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    ABSTRACT: ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.
    No preview · Article · Jan 2010 · ChemInform
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    ABSTRACT: On mixing organic solutions of [Et2PS2]M/n and [Prop2PS2]M/n [M=Pd(II), Pt(II), Rh(III), lr(III), Cr(III)] an equilibrium is obtained containing statistical amounts of the corresponding mixed ligand complexes as can be shown by 31P{1H}-NMR, HPLC and FD-MS. With Pt(II)- and Pd(II)-chelates the kinetics of ligand exchange was determined by HPLC. Mixed complexes ML2L′ and MLL′2 were isolated from the equilibrium solutions in case of the more inert Cr(III)-, Rh(III)- and lr(III)-chelates by preparative HPLC. Pd(II), Pt(II) and Rh(III) can be determined quickly and simultaneously in aqueous solutions at nanogramm level by complexation with Et2PS2 in a modified sample loop followed by reversed phase HPLC.
    No preview · Article · Jan 2007
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    ABSTRACT: Tris(Diethylphosphinodithioato)-Tris-μ-Disulfido-μ3-Thio-Triangulo-Trimolybdenum(IV)Diethylphosphinodithioate μ-Diethylposphinodithioato-Tris(Diethylphosphinodithioato)Tri-μ-Thio-μ3-Thio-Triangulo-Trimolybdenum(IV)
    No preview · Article · Jan 2007
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    ABSTRACT: Das vollständige Manuskript dieser Zuschrift erscheint in: Angew. Chem. Suppl. 1982, 1962. DOI: 10.1002/ange.198219620
    No preview · Article · Dec 2006 · Angewandte Chemie
  • K. Diemert · W. Kuchen · D. Mootz · W. Poll · F. Sandt
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    ABSTRACT: Phosphonic acid anhydrides are useful condensation reagents in the peptide and polyamide synthesis [1,2]. A new method for the preparation of well defined anhydrides is now described and intermediates of the peptide synthesis are elucidated. Cryoscopic and mass spectrometric data confirm the suggested cyclic trimeric molecular structure and the 31P{1H}- as well as 1H-NMR spectra can be explained with the structures: Reaction of t-BuP(O)(SiMe3)2 and PhBCl2 yields the mixed anhydride of t-butylphos-phonic and phenylboronic acid C40H57B4O12P4. The compound forms colourless crystals and the obtained data are in agreement with a 16 membered P-0-B- ring.
    No preview · Article · Oct 2006 · Phosphorus Sulfur and Silicon and the Related Elements
  • Helmut Keck · Wilhelm Kuchen · Johan K. Terlouw · Peter Tommes
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    ABSTRACT: Dissociative electron impact ionization (70 eV) of PhPBr2 yields [C6,H5,P]*+ ions with the PhP connectivity, as inferred from its collisional activation mass spectrum. Neutralization-Reionization experiments on this ion indicate that its neutral counterpart, phenylphosphinidene, Ph-P, is a stable species in the dilute gas phase.
    No preview · Article · Sep 2006 · Phosphorus Sulfur and Silicon and the Related Elements
  • W Kuchen · H Wunderlich
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    ABSTRACT: The crystal structure of the title compound, [(t)Bu(2)P(S)N(i)Pr](2)Ni or [Ni(C(11)H(25)NPS)(2)], shows a dihedral angle of 82.27 (6) degrees between the two Ni/S/N planes and thus a distorted tetrahedral arrangement of the NiN(2)S(2) chromophore. The structure is in accordance with the observed paramagnetism and is contrasted with the oxo analogue, which is planar but also paramagnetic.
    No preview · Article · Dec 2000 · Acta Crystallographica Section C Crystal Structure Communications
  • Wilhelm Kuchen · Hartmut Wunderlich
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    ABSTRACT: The crystal structure of the title compound, [tBu2P(S)NiPr]2Ni or [Ni(C11H25NPS)2], shows a dihedral angle of 82.27 (6)° between the two Ni/S/N planes and thus a distorted tetrahedral arrangement of the NiN2S2 chromophore. The structure is in accordance with the observed paramagnetism and is contrasted with the oxo analogue, which is planar but also paramagnetic.
    No preview · Article · Nov 2000 · Acta Crystallographica Section C Crystal Structure Communications
  • Wilhelm Kuchen · Hartmut Wunderlich
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    ABSTRACT: The title paramagnetic compound, chloro-2κCl-[di-tert-butyl­phos­phinic ethylamide-1κO]­bis­[μ-di-tert-butyl­phos­phin­ic ethyl­amidato(1−)-1:2κ4O:N]­lithium(I)­nickel(II), [NiLiCl(C10H23NOP)2(C10H24NOP)], revealed an incomplete bischelation of Ni2+ by L− {L = [tBu2P(O)NEt]−}, with the formation of a pseudo-tetrahedral NiON2Cl chromophore. The Ni atom is coordinated by Cl−, bidentate L− and mono­dentate LLi (via N).
    No preview · Article · Oct 2000 · Acta Crystallographica Section C Crystal Structure Communications
  • W. Kuchen · W. Peters · M. Sünkeler
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    ABSTRACT: N,N′-Bis(P,P-dialkylthiophosphinyl)diamines 1a-e were obtained from Et2P(S)Br and H2NR′NH2 with elimination of HBr. Compounds 2a-e were prepared by sulfuration of R2PNHR′NHPR2 that were generated without isolation from NH2-R′-NH2 and t-Bu2PCl.
    No preview · Article · Feb 1999 · Journal für praktische Chemie
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    ABSTRACT: Metathese von [NiCl2(PPh3)2] mit Li-Salzen potentiell vierzähniger Liganden [R2P(S)N–R'–NP · (S)R2]2– (= L) ergibt monomere Komplexe NiL, die den Chromophor NiN2S2 enthalten (1: R = Et; a, b: R' = Me2C–(CH2)2–CMe2, o-Phenylen; 2: R = t-Bu, R' = (CH2)n; a–c: n = 2, 3, 4). Aufgrund der Ergebnisse magnetischer Messungen sowie von VIS- und NMR-Untersuchungen (1H, 31P) sind diese Komplexe planar mit Ausnahme der tetraedrischen Verbindung 1 a. Im Falle von 1 a und 2 c wurden diese Befunde durch Kristallstrukturanalysen bestätigt. In Lösungen von 1 a bzw. 2 c in Toluol liegt ein Gleichgewicht planarer (diamagnetischer) und tetraedrischer (paramagnetischer) Konformeren vor. VT-1H-NMR Messungen in Kombination mit 1H,1H-COSY lassen bei 1 a eine verlangsamte Δ,Λ-Inversion unterhalb 330 K erkennen. Nur 1 b bildet mit Triphenylphosphan ein kristallines Addukt 1 b · PPh3 mit pentakoordiniertem Nickel(II), das in Lösung weitgehend dissoziiert. 1 a und 2 c kristallisieren in der monoklinen Raumgruppe P21/c mit Z = 4 Molekülen pro Elementarzelle der Abmessungen 1 a: a = 8.774(1), b = 12.335(2), c = 21.339(3) Å, β = 92.33(1)° und 2 c: a = 13.374(8), b = 16.197(8), c = 12.814(6) Å, β = 109.20(4)°. Bei 1 a beträgt der Diederwinkel ϵ im Chromophor 41.7(1)° entsprechend einem stark verzerrten Tetraeder. 2 c ist hingegen mit einem Winkel von 4.5(1)° nahezu planar.Monomeric Complexes NiL with Tetradentate Ligands [R2P(S)N–R'–NP(S)R2]2– (= L)Metathesis of [NiCl2(PPh3)2] with Li salts of the potentially tetradentate ligands [R2P(S)N–R'–NP(S)R2]2– (= L) affords monomeric complexes NiL containing the chromophore NiN2S2 (1: R = Et; a, b: R' = Me2C–(CH2)2–CMe2, o-Phenylen; 2: R = t-Bu, R' = (CH2)n; a–c: n = 2, 3, 4). According to the results of magnetic measurements and VIS as well as NMR spectroscopy (1H, 31P) these complexes are planar except 1 a that is tetrahedral. In case of 1 a and 2 c this was confirmed by the results of crystal structure analyses. In toluene, however, 1 a and 2 c form an equilibrium of planar (diamagnetic) and tetrahedral (paramagnetic) conformers. VT-1H-NMR including 1H,1H-COSY showed a hindered Δ,Λ-inversion of 1 a below 330 K. Only with 1 b a pentacoordinate adduct 1 b · PPh3 was obtained that completely dissociates in its components on dissolving in benzene. 1 a and 2 c crystallize in the monoclinic space group P21/c containing 4 molecules in the unit cell of the dimensions 1 a: a = 8.774(1), b = 12.335(2), c = 21.339(3) Å, β = 92.33(1)° and 2 c: a = 13.374(8), b = 16.197(8), c = 12.814(6) Å, β = 109.20(4)°. The coordination of the Ni atom yields in 1 a a dihedral angle ϵ of 41.7(1)° and thus a geometry intermediate between planar and tetrahedral while in 2 c the angle of 4.5(1)° reveals a nearly planar chromophore NiN2S2.
    No preview · Article · Dec 1998 · Zeitschrift für anorganische Chemie
  • R. Boese · M. Düppmann · W. Kuchen · W. Peters
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    ABSTRACT: Die Umsetzung von LLi mit Metallhalogeniden oder Metallhalogenidkomplexen ergibt Chelatkomplexe LM/n (L = R2P(NR′)2–; M = Cr+++, Co++, Ni++, Zn++). Mit dem sperrigen Liganden t-Bu2P(NSiMe3)2– und Ni(PPh3)2Cl2 oder Ni(dme)Br2 (dme = Dimethoxyethan) konnten lediglich die halogenoverbrückten Komplexe [LNiHal]2 (Hal = Cl, Br) mit tetraedrischen NiN2Hal2-Chromophoren erhalten werden. Hauptsächlich untersucht wurden die Bischelate L2Ni 2. 2 a (R = i-Pr, R′ = Me) und 2 c (R = Ph, R′ = Et) sind planar, 2 b (R = i-Pr, R′ = Et) und 2 d–g (R, R′ = i-Pr, i-Pr; Ph, i-Pr; Et, SiMe3; Ph, SiMe3) hingegen tetraedrisch. In Lösungen von 2 b und 2 c liegt ein Konformerengleichgewicht planar (diamagnetisch)  tetraedrisch (paramagnetisch) vor, das sich mit steigender Temperatur nach rechts verschiebt und in dem bei Raumtemperatur das tetraedrische (2 b) bzw. das planare Konformer (2 c) bei weitem überwiegt. Wie im Falle der isovalenzelektronischen Verbindungen [R2P(S)NR′]2Ni begünstigen offensichtlich auch hier kleine Substituenten R′ den planaren Zustand und im Gegensatz zu einigen Komplexen [R2P(O)NR′]2Ni beobachtet man bei 2 keine paramagnetischen planaren Spezies. Diese Befunde, die sich aus magnetischen Messungen und UV/VIS- sowie NMR spektroskopischen Untersuchungen ergaben, konnten durch Röntgenstrukturuntersuchungen erhärtet werden. Dabei erwies sich 2 a als planar (orthorhombisch; a = 3382.8(11), b = 1124.0(4), c = 8874(3); P21212; Z = 6), 2 g als tetraedrisch (monoklin; a = 1268.4(2), b = 1806.8(2), c = 1971.6(2), P21/n; Z = 4). Der Bißwinkel NNiN des Chelatliganden in 2 a (ca. 77.0°) ist von ähnlicher Größe wie in den paramagnetischen planaren Komplexen [R2P(O)NR′]2Ni (NNiO 74–77°) und zeigt somit, daß ein kleiner „Biß” des Chelatliganden bei planaren Ni(II)-Komplexen nicht notwendigerweise Paramagnetismus zur Folge hat.Chelate Complexes LM/n of Transition Metals with Phosphinoimidic Amidato Ligands R2P(NR′)2– (= L)Reaction of LLi with metal halides or metal halide complexes affords chelate complexes LM/n (L = R2P(NR′)2–; M = Cr+++, Co++, Ni++, Zn++). With the bulky ligand t-Bu2P(NSiMe3)2– and Ni(PPh3)2Cl2 or Ni(dme)Br2 (dme = dimethoxyethane) only halide bridged chelates [LNiHal]2 (Hal = Cl, Br) containing tetrahedral chromophors NiN2Hal2 were obtained. Main objects of investigation were the bischelates L2Ni 2. 2 a (R = i-Pr, R′ = Me) and 2 c (R = Ph, R′ = Et) are planar, 2 b (R = i-Pr, R′ = Et) and 2 d–g (R, R′ = i-Pr, i-Pr; Ph, i-Pr; Et, SiMe3; Ph, SiMe3) tetrahedral. In solutions of 2 b and 2 c a conformational equilibrium planar (diamagnetic)  tetrahedral (paramagnetic) exists that is shifted to the right with increasing temperature and is dominated by the tetrahedral (2 b) or planar conformer (2 c) at room temperature. As is the case with the isovalence electronic compounds [R2P(S)NR′]2Ni small substituents R′ apparently favour the planar state and in contrast to some complexes [R2P(O)NR′]2Ni no paramagnetic planar species 2 have yet been observed. These findings that are derived from the results of magnetic measurements and of UV/VIS as well as NMR spectroscopy are confirmed by crystal structure determinations: 2 a was found to be planar (orthorhombic; a = 3382.8(11), b = 1124.0(4), c = 8874(3); P21212; Z = 6), and 2 g to be tetrahedral (monocline; a = 1268.4(2), b = 1806.8(2), c = 1971.6(2), P21/n; Z = 4). The bite angle NNiN of the chelate ligand in 2 a (ca. 77°) is similar to those in paramagnetic planar complexes [R2P(O)NR′]2Ni (NNiO 74–77°) and shows that a small chelate bite does not necessarily imply paramagnetism of planar Ni(II) complexes.
    No preview · Article · May 1998 · Zeitschrift für anorganische Chemie
  • R. Boese · M. Düppmann · W. Kuchen · W. Peters
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    ABSTRACT: Reaction of LLi with metal halides or metal halide complexes affords chelate complexes LM/n (L = R2P(NR′)2-; M = Cr+++, Co++, Ni++, Zn++). With the bulky ligand t-Bu2P(NSiMe3)2- and Ni(PPh3)2Cl2 or Ni(dme)Br2 (dme = dimethoxyethane) only halide bridged chelates [LNiHal]2 (Hal = Cl, Br) containing tetrahedral chromophors NiN2Hal2 were obtained. Main objects of investigation were the bischelates L2Ni 2. 2a (R = i-Pr, R′ = Me) and 2c (R = Ph, R′ = Et) are planar, 2b (R = i-Pr, R′ = Et) and 2d-g (R, R′ = i-Pr, i-Pr; Ph, i-Pr; Et, SiMe3; Ph, SiMe3) tetrahedral. In solutions of 2b and 2c a conformational equilibrium planar (diamagnetic) ⇌ tetrahedral (paramagnetic) exists that is shifted to the right with increasing temperature and is dominated by the tetrahedral (2b) or planar conformer (2c) at room temperature. As is the case with the isovalence electronic compounds [R2P(S)NR′]2Ni small substituents R′ apparently favour the planar state and in contrast to some complexes [R2P(O)NR′]2Ni no paramagnetic planar species 2 have yet been observed. These findings that are derived from the results of magnetic measurements and of UV/VIS as well as NMR spectroscopy are confirmed by crystal structure determinations: 2a was found to be planar (orthorhombic; a = 3382.8(11), b = 1124.0(4), c = 8874(3); P21212; Z = 6), and 2g to be tetrahedral (monocline; a =1268.4(2), b = 1806.8(2), c =1971.6(2), P21/n; Z = 4). The bite angle NNiN of the chelate ligand in 2a (ca. 77°) is similar to those in paramagnetic planar complexes [R2P(O)NR′]2Ni (NNiO 74-77°) and shows that a small chelate bite does not necessarily imply paramagnetism of planar Ni(II) complexes.
    No preview · Article · May 1998 · Zeitschrift für anorganische und allgemeine Chemie
  • Klaus Diemert · Wilhelm Kuchen · Wolfgang Poll · Frank Sandt
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    ABSTRACT: By reaction of RP(O)Cl2 with RP(O)(OSiMe3)2, phosphonic anhydrides (RPO2)3 (R = tBu, 2-methylphenyl, 2,4,6-trimethylphenyl) 1a−c are conveniently obtained. In contrast to 1b and 1c, compound 1a is remarkably stable against protolysis. Intermediates of hydrolysis of 1a, namely tris(tert-butyl)triphosphonic acid (2) and bis(tert-butyl)diphosphonic acid (3), can also be isolated in good yield. The structures of 1−3 were determined mainly by NMR spectroscopy (1 H, 13C, 31P). Assuming an energetic preference for the chair conformations in solution, and considering the steric requirements of the bulky substituents R, configurations Ia (point group Cs, two R in equatorial positions) for 1a and b, and IIa (point group C3v, all R equatorial) for 1c are suggested. − Reaction of 1a with N-benzyloxycarbonylglycine (4) in methanol affords strong evidence that in the first step of peptide synthesis with (RPO2)3, a mixed anhydride of triphosphonic acid and the N-protected amino acid is formed. − The crystal structure of 1a (monoclinic, space group P21/n) widely corresponds to the suggested configuration Ia, but reveals an envelope conformation for the six-membered ring with a P3O2 plane in the crystal. In the crystal structure of the octahydrate of the disodium salt of 2 (monoclinic, space group P21/c), it can be seen that the polar end groups of the anions [tBu3P3O7]2− together with the water molecules and the Na+ cations, form hydrogen-bonded double-layers, strictly separated from each other by the non-polar tert-butyl groups of the anions.
    No preview · Article · Mar 1998 · Berichte der deutschen chemischen Gesellschaft
  • Klaus Diemert · Wilhelm Kuchen · Wolfgang Poll · Frank Sandt
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    ABSTRACT: By reaction of RP(O)Cl2 with RP(O)(OSiMe3)2, phosphonic anhydrides (RPO2)3 (R = tBu, 2-methylphenyl, 2,4,6-trimethylphenyl) 1a-c are conveniently obtained. In contrast to 1b and 1c, compound 1a is remarkably stable against protolysis. Intermediates of hydrolysis of 1a, namely tris(tert-butyl)triphosphonic acid (2) and bis(tert-butyl)diphosphonic acid (3), can also be isolated in good yield. The structures of 1-3 were determined mainly by NMR spectroscopy (1H, 13C, 31P). Assuming an energetic preference for the chair conformations in solution, and considering the steric requirements of the bulky substituents R, configurations Ia (point group Cs, two R in equatorial positions) for 1a and b, and IIa (point group C3vi all R equatorial) for 1c are suggested. - Reaction of 1a with N-benzyloxycarbonylglycine (4) in methanol affords strong evidence that in the first step of peptide synthesis with (RPO2)3, a mixed anhydride of triphosphonic acid and the N-protected amino acid is formed. - The crystal structure of 1a (monoclinic, space group P21/n) widely corresponds to the suggested configuration Ia, but reveals an envelope conformation for the six-membered ring with a P3O2 plane in the crystal. In the crystal structure of the octahydrate of the disodium salt of 2 (monoclinic, space group P21/c), it can be seen that the polar end groups of the anions [tBu3P3O7]2- together with the water molecules and the Na+ cations form hydrogen-bonded double-layers, strictly separated from each other by the non-polar tert-butyl groups of the anions.
    No preview · Article · Mar 1998 · European Journal of Inorganic Chemistry
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    ABSTRACT: Metathesis of [NiCl2(PPh3)2] with Li salts of the potentially tetradentate ligands [R2P(S)N-R′-NP(S)R2]2- (= L) affords monomeric complexes NiL containing the chromophore NiN2S2 (1: R = Et; a, b: R′ = Me2C-(CH2)2-CMe2, o-Phenylen; 2: R = t-Bu, R′ = (CH2)n; a-c: n = 2, 3, 4). According to the results of magnetic measurements and VIS as well as NMR spectroscopy (1H, 31P) these complexes are planar except 1 a that is tetrahedral. In case of 1 a and 2 c this was confirmed by the results of crystal structure analyses. In toluene, however, 1 a and 2 c form an equilibrium of planar (diamagnetic) and tetrahedral (paramagnetic) conformers. VT-1H-NMR including 1H,1H-COSY showed a hindered Δ,Λ-inversion of 1 a below 330 K. Only with 1 b a pentacoordinate adduct 1 b · PPh3 was obtained that completely dissociates in its components on dissolving in benzene. 1 a and 2 c crystallize in the monoclinic space group P21/c containing 4 molecules in the unit cell of the dimensions 1 a: a = 8.774(1), b = 12.335(2), c = 21.339(3) Å, β = 92.33(1)° and 2 c: a = 13.374(8), b = 16.197(8), c = 12.814(6) Å, β = 109.20(4)°. The coordination of the Ni atom yields in 1 a a dihedral angle ε of 41.7(1)° and thus a geometry intermediate between planar and tetrahedral while in 2 c the angle of 4.5(1)° reveals a nearly planar chromophore NiN2S2.
    No preview · Article · Jan 1998

Publication Stats

2k Citations
478.26 Total Impact Points

Institutions

  • 1968-2010
    • Heinrich-Heine-Universität Düsseldorf
      • Institute of Inorganic Chemistry and Structural Chemistry
      Düsseldorf, North Rhine-Westphalia, Germany
  • 1992
    • McMaster University
      Hamilton, Ontario, Canada
  • 1965-1967
    • RWTH Aachen University
      • Institute of Inorganic Chemistry
      Aachen, North Rhine-Westphalia, Germany
    • Fachhochschule Aachen
      Aachen, North Rhine-Westphalia, Germany