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  • Phosphaalkyne, amino-  (3)
  • imidazole  (2)
  • 1,2,3-Diazaphospholes  (1)
  • 1,2-Dihydro-1,3,2λ5,4λ5-diazadiphosphete  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Reaktive E = C(p-p)π-Systeme, XXXIII. Side-on-Koordination des Phosphaalkins P ≡ C  -  N(iPr)2 im 16e-Nickel(0)-Komplex Ni(CO)PCy3[PCN(iPr)2] (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 63-65 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkyne, amino- ; Nickel carbonyl phosphane complex ; π Coordination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactive E = C(p-p)π Systems, XXXIII.  -  Side-on Coordination of the Phosphaalkyne P ≡ C  -  N(iPr)2 in the 16e Nickel(0) Complex Ni(CO)PCy3[PCN(iPr)2]The reaction of (diisopropylamino)phosphaethyne P ≡ C  -  N(iPr)2 with the nickel complex [Ni(CO)3PCy3] - in contrast to the analogous reactions with Ni(CO)4 or Ni(CO)3PR3 (R = Me, Ph) - leads to the novel 16e nickel(0) system [Ni{η2-P ≡ C  -  N(iPr2)}(CO)PCy3] with a planar geometry of all skeleton atoms besides the methyl and cyclohexyl groups. Side-on coordination of the P ≡ C triple bond results in an increase of the PC distance to 1.665 Ȧ typical for phosphaalkenes.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260111
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  • 2
    Electronic Resource
    Electronic Resource
    Reaktive E = C(p - p)π-Systeme, XXXI Erste Vertreter aminosubstituierter 1,2,4-Diazaphosphole (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 411-414 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkyne, amino- ; [3 + 2] Cycloaddition ; 1,2,4-Diazaphospholes ; 1,2,3-Diazaphospholes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactive E = C(p - p)π Systems, XXXII[1].  -  First Representatives of Amino-Substituted 1,2,4-Diazaphospholes(Diisopropylamino)phosphaethyne iPr2N - C≡P reacts at 20° C in a [3 + 2] cycloaddition with (trifluoromethyl)diazomethane (2a) or methyl diazoacetate (2b) to yield a mixture of the corresponding regioisomers 1H-1,2,4-diazaphospholes (5a or 5b) and 1H-1,2,3-diazaphospholes (6a or 6b) in quantitative yields (isomer ratio: 5a/6a = 2:1; 5b/6b = 4:1). X-ray diffraction studies on 5a and 5b indicate a delicate charge balance in the bonding system of 1H-1,2,4,σ2-diazaphospholes under the influence of the exocyclic push/pull substituents iPr2N and CF3 or CO2Me, respectively.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250219
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  • 3
    Electronic Resource
    Electronic Resource
    1,2-Dihydro-1,3,2λ5,4λ5-diazadiphosphet - Synthese, Struktur und Isomerisierung zum „inneren Salz“ von 1,3,2,4λ5-Diazadiphosphetan-2-iumhydroxid* (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 2631-2634 
    Details
    ISSN: 0009-2940
    Keywords: 1,2-Dihydro-1,3,2λ5,4λ5-diazadiphosphete ; Isomerization ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,2-Dihydro-1,3,2λ5,4λ5-diazadiphosphete - Synthesis, Structure and Isomerization to the „Inner Salt“ of 1,3,2,4λ5-Diazadiphosphetan-2-ium HydroxideThe photochemical reaction of the azidophosphane (iPr2N)2PN3 (1) with the tetraazaphospholene (3) and the bis(imino)phosphorane (Me3Si)2NP(=NSiMe3)2 (6) proceeds by elimination of N2 to yield (5) and by 1,3-silyl group shift to furnish (8) the structures of which were determined by means of NMR data and, in the case of 5, additionally by X-ray structure analysis.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921251202
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  • 4
    Electronic Resource
    Electronic Resource
    Zink-Koordinationsverbindungen mit Imidazolin- und Imidazol-DonorligandenProfessor Dietrich Mootz zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1183-1195 
    Details
    ISSN: 0044-2313
    Keywords: Zinc complexes ; imidazole ; imidazoline ; bisimidazoline complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zinc Coordination Compounds with Imidazoline and Imidazole Donor Ligands.By reaction of the two bidentate bisimidazoline ligands 1,2-bis(2-imidazoline-2-yl)ethan (BIE) and 1,2-bis(2-imidazoline-2-yl)benzene (BIB) with zinc bromide under various reaction conditions the complexes [ZnBr2(BIE)] (1), [ZnBr2(BIB)] (2), [Zn(BIE)2]Br2 (3) and [Zn(BIB)2](BPh4)2 (4) were synthesized and characterized. In all compounds the zinc atom is tetrahedrally coordinated, either by a bidentate ligand and two bromine ligands, or by two of the chelate ligands. Zn—N—bond distances for 1-4 range from 1.966(2) to 2.013(3) Å, and the Zn—Br distances from 2.372(1) to 2.403(1) Å. [3-(imidazole-1-yl)-1-oxopropyl]benzene (IOB) was prepared as a novel imidazole ligand which carries a keto-O atom in 1,5-position to the pyridine-N atom. The zinc in [ZnCl2(IOB)2] (5) is coordinated by two ligands and two Cl atoms forming a distorted tetrahedral ZnN2Cl2 unit (Zn—N: 2.013(3) and 2.029(2) Å; Zn—Cl: 2.226(1) and 2.242(1) Å).The colourless compounds 1-5 were characterized by IR, 1H-NMR, X-ray absorption spectra and single-crystal X-ray structure analysis. Space groups and structural data: 1: P21/c, a = 7.717(2), b = 22.814(5), c = 8.026(2) Å, β = 117.58(2)° (140 K), R = 0.0283; 2: Cc, a = 11.831(3), b = 11.677(1), c = 11.846(1) Å, β = 114.55(2)°, R = 0.0237; 3: P42/n, a = 7.931(1), c = 16.945(1) Å, R = 0.0312; 4: P21/c, a = 18.666(2), b = 16.615(2), c = 19.786(2) Å, β = 99.17(1)°, R = 0.0472; 5: P21/c, a = 9.173(2), b = 9.230(1), c = 28.357(3) Å, β = 96.63(1)°, R = 0.0317.
    Notes: Durch Umsetzungen der zweizähnigen Bisimidazolin-Liganden 1,2-Bis(2-imidazolin-2-yl)ethan (BIE) und 1,2-Bis(2-imidazolin-2-yl)benzol (BIB) mit Zinkbromid unter verschiedenen Reaktionsbedingungen konnten die Komplexverbindungen [ZnBr2(BIE)] (1), [ZnBr2(BIB)] (2), [Zn(BIE)2]Br2 (3) und [Zn(BIB)2](BPh4)2 (4) synthetisiert und charakterisiert werden. Das Zinkatom ist jeweils tetraedrisch von einem zweizähnigen Chelatliganden und zwei Bromatomen oder von zwei dieser Liganden koordiniert. Die Zn—N-Bindungslängen in 1-4 variieren zwischen 1,966(2) und 2,013(3) Å, für die Zn—Br-Abstände wurden Werte zwischen 2,372(1) und 2,403(1) Å beobachtet. Mit dem neuen Liganden [3-(Imidazol-1-yl)-1-oxopropyl]benzol (IOB) gelang die Synthese des Komplexes [ZnCl2(IOB)2] (5), in dem eine tetraedrische ZnN2Cl2-Koordinationseinheit vorliegt (Zn—N: 2,013(3) und 2,029(2) Å; Zn—Cl: 2,226(1) und 2,242(1) Å).Die farblosen Verbindungen 1-5 wurden durch IR-, 1H-NMR- und Röntgenabsorptionsspektren sowie durch vollständige Röntgenstrukturanalysen charakterisiert. Raumgruppen und Gitterkonstanten: 1: P21/c, a = 7,717(2), b = 22,814(5), c = 8,026(2) Å, β = 117,58(2)° (140 K), R = 0,0283; 2: Cc, a = 11,831(3), b = 11,677(1), c = 11,846(1) Å, β = 114,55(2)°, R = 0,0237; 3: P42/n, a = 7,931(1), c = 16,945(1) Å, R = 0,0312; 4: P21/c, a = 18,666(2), b = 16,615(2), c = 19,786(2) Å, β = 99,17(1)°, R = 0,0472; 5: P21/c, a = 9,173(2), b = 9,230(1), c = 28,357(3) Å, β = 96,63(1)°, R = 0,0317.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190707
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  • 5
    Electronic Resource
    Electronic Resource
    Reaktive E = C(p-p)π-Systeme. XLII [1]. Neue Koordinationsverbindungen des 2-(Diisopropylamino)-1-phosphaethins: [{η4-(iPr2NCP)2}Ni{η2-(iPr2NCP)}], [(Ph3P)2Pt{η2-(iPr2NCP)}] und [Co2(CO)6{η2-η2-(iPr2NCP)}]In memoriam Wilhelm Klemm (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 24-34 
    Details
    ISSN: 0044-2313
    Keywords: Phosphaalkyne, amino- ; nickel, platinum, cobalt complexes ; 1 λ3, 3 λ5-diphosphetene ; 1H, 13C{1H} and 31P{1H} NMR spectra ; X-ray structure determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactive E = C(pp)π-Systems. XLII [1]. Novel Coordination Compounds of 2-(Diisopropylamino)-1-phosphaethyne: [{η4-(iPr2NCP)2}Ni{η2-(iPr2NCP)}], [(Ph3P)2Pt{η2-(iPr2NCP)}], and [Co2(CO)6{η2-μ2-(iPr2NCP)}]2-(Diisopropylamino)-phosphaethyne iPr2N—C≡P (2) reacts with the Ni(0)-complexes [Ni(1,5-cyclooctadiene)2] and [Ni(CO)3(1-azabicyclo[2.2.2]octane)], respectively, to give the novel complex [{η4-(iPr2NCP)2}Ni{η2-(iPr2NCP)}] (5), with the 1,3-diphosphacyclobutadiene derivative and 2 (side-on) as π-ligands. The molecular structure of 5 determined by X-ray diffraction on single crystals proves the spin systems and rotational barriers deduced from NMR-data (1H, 13C-, 31P). The PC distances of the four-membered ring of 1.817(2) and 1.818(2) Å - as expected - are considerably longer than the PC bond of the η2-coordinated phosphaalkyne 2 [1.671(2) Å]. - In the reactions of 2 with [(Ph3P)2Pt(C2H4)] or [Co2(CO)8] the ligand properties of 2 resemble those of alkynes affording the complexes [(Ph3P)2Pt{η2-(iPr2NCP)}] (7) with side-on coordinated 2 and [Co2(CO)6{η2-μ2-(iPr2NCP)}] with 2 acting as a 4e donor bridge in quantitative yield.In attempts to prepare copper(I) complexes of the aminophosphaalkyne 2 by reaction with CuCl or CuI the only isolable product formed in reasonable amounts under the influence of air and moisture is the 1 λ3, 3 λ5-diphosphetene (iPr2N) (10) (isolated yield: ca. 20%). The crystal structure analysis of 10 indicates a strong structural relationship to the diamino-2-phosphaallyl cation [Me(iPr2N)]+ (12), the 1,3-diphosphacyclobutadiene ligand (iPr2NCP)2 in the binuclear complex [{η1, μ2-(iPr2NCP)2}Ni2(CO)6] (3a) as well as to the heterocycles (dme)2LiOE2′ (E′ = S, 11a; E′ = Se, 11b) prepared by Becker et al. [11b, 35].
    Notes: 2-(Diisopropylamino)-phosphaethin iPr2N-C≡P (2) reagiert mit den Ni(0)-Komplexen [Ni(1,5-Cyclooctadien)2] bzw. [Ni(CO)3(1-Azabicyclo[2.2.2]octan)] zu dem neuen Komplex [{η4-(iPr2NCP)2}Ni{η2-(iPr2NCP)}] (5), der zwei Moleküle 2 in Form des 1,3-Diphosphacyclobutadiensystems und ein Molekül 2 „side-on“ koordiniert als π-Liganden enthält. Die Molekülstruktur von 5, ermittelt durch Röntgenbeugung an Einkristallen, bestätigt die aus den NMR-Daten (1H-, 13C-, 31P) abgeleiteten Spinsysteme und Rotationsbarrieren. Die PC-Abstände des Vierrings sind mit 1,817(2) bzw. 1,818(2) Å erwartungsgemäß erheblich länger als die PC-Bindung des η2-koordinierten Phosphaalkins 2 [1,671(2) Å]. Bei den Umsetzungen von 2 mit [(Ph3P)2Pt(C2H4)] bzw. [Co2(CO)8] entspricht das koordinative Verhalten dem von Alkinen; sie liefern die Komplexe [(Ph3P)2Pt{η2-(iPr2NCP)}] (7) mit side-on gebundenem 2 bzw. [Co2(CO)6{η2-η2-(iPr2NCP)}] mit 2 als 4e-Donorbrücke in quantitativer Ausbeute.Bei dem Versuch, aus 2 und CuCl bzw. CuI Kupfer(I)-Komplexe des Aminophosphaalkins darzustellen, bildet sich unter Einwirkung von Luft und Feuchtigkeit als einziges isolierbares Produkt das 1λ3, 3λ5-Diphospheten (iPr2N) (10) in beträchtlicher Menge (Reinausbeute: ca. 20%). Für 10 ergibt sich aus der Kristallstrukturanalyse eine enge Beziehung zu dem Diamino-2-phosphaallyl-Kation [Me(iPr2N)]+ (12), dem 1,3-Diphosphacyclobutadien-Liganden (iPr2NCP)2 im Zweikernkomplex [{η1-μ2-(iPr2NCP)2}Ni2(CO)6] (3a) sowie zu den von Becker et al. [11 b, 35] dargestellten Heterocyclen (dme)2LiOE2′ (E′ = S, 11a; E′ = Se, 11b).
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220106
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  • 6
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    Electronic Resource
    Tripodal Ligands: Design of Distorted Coordination Polyhedra in Biomimetic Metal Complexes. Crystal structures of [Zn(SCN)(ntb)](SCN) · iPrpOH and [Fe(acac)(ntb)](ClO4)2 · 2CH2Cl2 · iPrpOH, ntb = N-tris(2-benzimidazolylmethyl)amineProfessor Gerhard Thiele zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 329-336 
    Details
    ISSN: 0044-2313
    Keywords: Zinc complex ; iron complex ; tripodal ligand ; benzimidazole ; imidazole ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tripodliganden: Darstellung verzerrter Koordinationspolyeder in biomimetischen Metallkomplexen. Kristallstrukturen von [Zn(SCN)(ntb)](SCN) · iPrpOH und [Fe(acac)(ntb)](ClO4)2 · 2 CH2Cl2 · iPrpOH, ntb = N-Tris(2-benzimidazolylmethyl)aminDer Tripodligand N-Tris(2-benzimidazolylmethyl)amin (ntb) wurde zur Synthese eines Zink(II)- und eines Eisen(III)-Komplexes, [Zn(SCN)(ntb)](SCN) · iPrpOH (1) und [Fe(acac)(ntb)](ClO4)2 · 2 CH2Cl2 · iPrpOH (2), eingesetzt. Der Zinkkomplex hat eine stark verzerrte trigonal-bipyramidale Koordinationssphäre. Die koordinierenden Atome sind ein Amin-N, drei Benzimidazol-N und ein SCN--N-Atom. Auffällig hier ist der 2.539(6)Å große Zn—Namin-Bindungsabstand. Das Koordinationspolyeder des Eisenkomplexes ist weniger stark verzerrt als das in 1 und wird von einem Amin- und drei Benzimidazol-Stickstoffatomen des Liganden sowie zwei Sauerstoffatomen des Acetylacetonats gebildet. Die Fe—O-Bindungslängen zeigen eine Differenz von ca. 0.1 Å, die wie die ungewöhnlich lange Zn—N-Bindung durch einen Trans-Effekt verursacht wird. 1 kristallisiert triklin in der Raumgruppe P1 mit: a = 9.530(1), b = 13.402(1), c = 13.578(2)Å, α = 98.83(1), β = 95.19(1), γ = 101.21(1)°, Z = 2; 2 ist ebenfalls triklin, P1, mit: a = 9.875(6), b = 12.929(10), c = 18.635(15)Å, α = 94.95(8), β = 101.01(6), γ = 111.09(4)°, Z = 2.
    Notes: The tripodal ligand N-tris(2-benzimidazolylmethyl)-amine (ntb) was used for the preparation of zinc(II) and iron(III) complexes, [Zn(SCN)(ntb)](SCN) · iPrpOH (1) and [Fe(acac)(ntb)](ClO4)2 · 2CH2Cl2 · iPrpOH (2). 1 has a highly distorted trigonal-bipyramidal ZnN5 coordination geometry. The donor atoms are nitrogens of one amine, three benzimidazoles and one SCN-. A striking feature of the complex is the length of the Zn—Namine bond of 2.539(6)Å. The octahedral N4O2 coordination sphere of the iron in 2 is less distorted than that of the zinc in 1. The metal is surrounded by an amine and three benzimidazole nitrogens of the ligand and two oxygens of the bidentate acetylacetonate co-ligand. The Fe—O bond lengths differ by about 0.1 Å. As for the unusual long Zn—N bond in 1 this is a result of a trans effect. 1 crystallizes in the space group P1 with: a = 9.530(1)Å, b = 13.402(1)Å, c = 13.578(2)Å, α = 98.83(1), β = 95.19(1), γ = 101.21(1)°, Z = 2; 2 is also triclinic, space group P1, with: a = 9.875(6)Å, b = 12.929(10)Å, c = 18.635(15)Å, α = 94.95(8)°, β = 101.01(6)°, γ = 111.09(4)°, Z = 2.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220221
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