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  • 1
    ISSN: 0570-0833
    Keywords: ab initio calculations ; imines ; phosphorus compounds ; sulfur compounds ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 2
    ISSN: 0947-6539
    Keywords: ab initio calculations ; crystal structure ; halogen compounds ; nitrides ; selenium compounds ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Se2NBr3, a planar molecule shaped liked dividers, was formed by the reaction of SeBr4 with N(SiMe3)3, which reduced the selenium to the trivalent state. Under the same conditions, Se2NCl5 was obtained by the reaction of SeCl4 with N(SiMe3)3, retaining the tetravalent state of selenium. The molecule is formed by two edge-sharing pseudotrigonal bipyramids with selenium as their central atoms. Se2NCl5 reacts with PPh4Cl to form the Se2NCl-6 ion by the addition of a Cl- ion to only one of the two selenium atoms, resulting in pseudooctahedral coordination of this atom. Ab initio calculations for all the compounds reported confirm the experimentally determined structures.
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  • 3
    ISSN: 0570-0833
    Keywords: cobalt compounds ; heterocubanes ; manganese compounds ; phosphorane iminato complexes ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 4
    ISSN: 0570-0833
    Keywords: arene complexes ; bridging ligands ; platinum silver ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 5
    ISSN: 0044-8249
    Keywords: Ab-initio-Rechnungen ; Imine ; Phosphorverbindungen ; Schwefelverbindungen ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 6
    ISSN: 0044-8249
    Keywords: Carbanionen ; Kupfer ; Phosphazene ; Zink ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 7
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes of Aluminium, Gallium and Antimony, Syntheses, Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Phosphorane Iminato Complexes [MCl2(NPPh3)]2 with M = Al and Ga, [SbCl2(NPMe3)(DMF)]2, and of the Phosphorane Imine Complex [Ph3PNH · BF3] · THFThe phosphorane iminato complexes [MCl2(NPPh3)]2 with M = Al and Ga and [SbCl2(NPMe3)(DMF)]2 are formed as colourless crystals by reactions of the anhydrous trichlorides MCl3 (M = Al, Ga, Sb) with the corresponding silylated phosphorane imines Me3SiNPR3 in acetonitrile and in dimethyl formamide, respectively. The phosphorane imine derivative [Ph3PNH · BF3] · THF is formed from Me3SiNPPh3 and boron trifluoride etherate in boiling tetrahydrofuran. The compounds are characterized by their i. r. spectra and by crystal structure analyses.[AlCl2(NPPh3)]2: Space group P1, Z = 1, structure solution with 1 585 observed unique reflections, R = 0.061. Lattice dimensions at -70°C: a = 917.6, b = 1 053.5, c = 1 145.2 pm, α = 111.72°, β = 100.80°, γ = 109.95°.[GaCl2(NPPh3)]2: Space group P1, Z = 1, structure solution with 2 586 observed unique reflections, R = 0.066. Lattice dimensions at -70°C: a = 917.5, b = 1 058.3, c = 1 153.7 pm, α = 105.52°, β = 107.75°, γ = 109.88°.In both compounds the metal atoms are linked to planar M2N2 four-membered rings via the N-atoms of the phosphorane iminato groups.[SbCl2(NPMe3)(DMF)]2: Space group P21/n, Z = 4, structure solution with 3 805 observed unique reflections, R = 0.038. Lattice dimensions at -70°C: a = 1 913.0, b = 726.8, c = 2 040.7 pm, β = 113.62°. The unit cell contains two symmetry independent dimeric molecules, in which the antimony atoms are centrosymmetricly μ2 linked via the N-atoms of the phosphorane iminato groups. Along with the oxygen atom of the dimethyl formamide molecule the Sb atoms achieve a ψ-octahedral environment.[Ph3PNH · BF3] · THF: Space group C2/c, Z = 8, structure solution with 2 048 observed unique reflections, R = 0.058. Lattice dimensions at -70°C: a = 2 460.4, b = 869.2, c = 1 978.0 pm, β = 116.35°.
    Notes: Die Phosphaniminatokomplexe [MCl2(NPPh3)]2 mit M = Al und Ga und [SbCl2(NPMe3)(DMF)]2 entstehen bei Reaktionen der wasserfreien Trichloride MCl3 (M = Al, Ga, Sb) mit den entsprechenden silylierten Phosphaniminen Me3SiNPR3 in Acetonitril bzw. in Dimethylformamid als farblose Einkristalle. Das Phosphanimin-Derivat [Ph3PNH · BF3] entsteht aus Me3SiNPPh3 und Bortrifluorid-Etherat in siedendem Tetrahydrofuran. Die Verbindungen werden durch ihre IR-Spektren und durch Kristallstrukturanalysen charakterisiert.[AlCl2(NPPh3)]2: Raumgruppe P1, Z = 1, Strukturlösung mit 1 585 beobachteten unabhängigen Reflexen, R = 0,061. Gitterkonstanten bei -70°C: a = 917,6; b = 1 053,5; c = 1 145,2 pm; α = 111,72°; β = 100,80° γ = 109,95°.[GaCl2(NPPh3)]2: Raumgruppe P1, Z = 1, Strukturlösung mit 2 586 beobachteten unabhängigen Reflexen, R = 0,066. Gitterkonstanten bei -70°C: a = 917,5; b = 1 058,3; c = 1 153,7 pm; α = 105,52°; β = 107,75°; γ = 109,88°. In beiden Verbindungen sind die Metallatome über die N-Atome der Phosphaniminatogruppen zu planaren M2N2-Vierringen verknüpft.[SbCl2(NPMe3)(DMF)]2: Raumgruppe P21/n, Z = 4, Strukturlösung mit 3 805 beobachteten unabhängigen Reflexen, R = 0,038. Gitterkonstanten bei -70°C: a = 1 913,0; b = 726,8; c = 2 040,7 pm; β = 113,62°. Die Elementarzelle enthält zwei symmetrieunabhängige dimere Moleküle, in denen die Antimonatome zentrosymmetrisch ψ2 über die N-Atome der Phosphaniminatogruppen verknüpft sind. Zusammen mit dem O-Atom des Dimethylformamid-Moleküls erreichen die Sb-Atome ψ-oktaedrische Umgebung.[Ph3PNH · BF3] · THF: Raumgruppe C2/c, Z = 8, Strukturlösung mit 2 048 beobachteten unabhängigen Reflexen, R = 0,058. Gitterkonstanten bei -70°C: a = 2 460,4; b = 869,2; c = 1 978,0 pm; β = 116,35°.
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  • 8
    ISSN: 0044-2313
    Keywords: Selenium ; Phosphorane Iminato Complex of Selenium ; Synthesis ; IR Spectrum ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of the Selenyl-Phosphoraneiminato Complex SeO(NPPh3)2SeO(NPPh3)2 has been prepared from SeO2 and Me3SiNPPh3 in a SeO2 suspension in acetonitrile, forming colourless crystals. The compound is characterized by IR spectroscopy and by a crystal structure determination. Space group P1, Z = 2, structure solution with 5 344 observed unique reflections, R = 0.064. Lattice dimensions at -40°C: a = 931.6, b = 947.6, c = 1 762 pm, α = 77.50°, β = 81.78°, γ = 79.23°. The compound forms monomeric molecules in which the selenium atom is ϕ-tetrahedrally surrounded with bond lengths SeO = 161.7 pm and SeN = 179.9 and 181.6 pm.
    Notes: SeO(NPPh3)2 entsteht in Form farbloser Kristalle bei der Reaktion einer Suspension von SeO2 mit Me3SiNPPh3 in Acetonitril. Die Verbindung wird durch das IR-Spektrum und durch eine Kristallstrukturanalyse charakterisiert. Raumgruppe P1, Z = 2, Strukturlösung mit 5 344 beobachteten unabhängigen Reflexen, R = 0,064. Gitterkonstanten bei -40°C: a = 931,6; b = 947,6; c = 1 762 pm, α = 77,50°, β = 81,78°, γ = 79,23°. Die Verbindung bildet monomere Moleküle, in denen das Selenatom verzerrt ϕ-tetraedrisch umgeben ist mit Abständen SeO = 161,7 pm und SeN = 179,9 und 181,6 pm.
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  • 9
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes of Titanium ; Syntheses ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorane Iminato Complexes of Titanium(IV) and Titanium(III). The Crystal Structures of [TiCl2(OMe)(NPPh3)]2, [TiBr2(NPPh3)]2 · 3C7H8, and [Ph3PNH2]Br · CH2Cl2TiCl3(NPPh3) reacts with a solution of methyllithium in diethyl ether in the presence of lithiummethylate forming yellow [TiCl2(OMe)(NPPh3)]2. On reaction with benzyl magnesium bromide TiCl3(NPPh3) in diethyl ether is converted into green [TiBr2(NPPh3)]2 under reduction and ligand exchange. [TiBr2(NPPh3)]2 crystallizes from toluene with three molecules C7H8. [Ph3PNH2]Br · CH2Cl2 originates as a side product of this reaction. The products are characterized by their i.r. spectra and by crystal structure analyses.[TiCl2(OMe)(NPPh3)]2. Space group P1, Z = 2, structure solution with 2909 independent reflections, R = 0.063. Lattice dimensions at 20°C: a = 1005.1, b = 1044.5, c = 1068.6 pm, α = 66.98°, β = 89.35°, γ = 80.24°. The compound forms centrosymmetric dimeric molecules with μ2-OMe bridges and five-fold coordinated titanium atoms. The (NPPh3-) ligand is terminally connected with a Ti = N distance of 174.8 pm and with a TiNP bond angle of 165.3°.[TiBr2(NPPh3)]2 · 3 C7H8. Space group P1, Z = 2, structure solution with 5548 independent reflections, R = 0.053. Lattice dimensions at -70°C: a = 983.3, b = 1162.7, c = 1376.5 pm, α = 100.53°, β = 110.30°, γ = 105.24°. The compound forms centrosymmetric dimeric molecules with μ2-NPPh3 bridges and tetrahedral coordination at the titanium atoms. With 195.9 pm the Ti-N bonds correspond with single bonds. The Ti … Ti distance of 260.0 pm is exceptionally short.[Ph3PNH2]Br · CH2Cl2. Space group P1, Z = 1, structure solution with 3091 independent reflections, R = 0.049. Lattice dimensions at 20°C: a = 909.4, b = 1004.4, c = 1158.5 pm, α = 108.09°, β = 94.67°, γ = 91.92°. The bromide ions are bonded to a one-dimensional infinite network via hydrogen bridge bonds of the cation and of the dichloromethane.
    Notes: TiCl3(NPPh3) reagiert mit einer Lösung von Methyllithium in Diethylether in Gegenwart von Lithiummethylat unter Bildung von gelbem [TiCl2(OMe)(NPPh3)]2. Bei der Umsetzung mit Benzylmagnesiumbromid wird TiCl3(NPPh3) in Diethylether unter Reduktion und Ligandenaustausch in grünes [TiBr2(NPPh3)]2 umgewandelt, das aus Toluol mit drei Molekülen C7H8 kristallisiert. Als Nebenprodukt dieser Reaktion entsteht [Ph3PNH2]Br · CH2Cl2. Die Produkte werden durch die IR-Spektren und durch Kristallstrukturanalysen charakterisiert.[TiCl2(OMe)(NPPh3)]2. Raumgruppe P1 Z = 2, Strukturlösung mit 2 909 unabhängigen Reflexen, R = 0,063. Gitterkonstanten bei 20°C: a = 1005,1; b = 1044,5; c = 1068,6 pm; α = 66,98°; β = 89,35°; γ = 80,24°. Die Verbindung bildet zentrosymmetrische dimere Moleküle mit μ2-OMe-Brücken und fünffach koordinierten Titanatomen. Der (NPPh3-)-Ligand ist terminal gebunden mit einem Ti=N-Abstand von 174,8 pm und einem TiNP-Bindungswinkel von 165,3°.[TiBr2(NPPh3)]2 · 3 C7H8. Raumgruppe P1, Z = 2, Strukturlösung mit 5548 unabhängigen Reflexen, R = 0,053. Gitterkonstanten bei -70°C: a = 983,3; b = 1162,7; c = 1376,5 pm; α = 100,53°; β = 110,30°; γ = 105,24°. Die Verbindung bildet zentrosymmetrische dimere Moleküle mit μ2-NPPh3-Brücken und tetraedrischer Koordination an den Titanatomen. Die Ti-N-Bindungen entsprechen mit 195,9 pm Einfachbindungen. Der Ti … Ti-Abstand ist mit 260,0 pm ungewöhnlich kurz.[Ph3PNH2]Br · CH2Cl2. Raumgruppe P1, Z = 1, Strukturlösung mit 3091 unabhängigen Reflexen, R = 0,049. Gitterkonstanten bei 20°C: a = 909,4; b = 1004,4; c = 1158,5 pm, α = 108,09°; β = 94,67d; γ = 91,92°. Die Bromidionen sind über Wasserstoffbrückenbindungen des Kations und des Dichlormethans zu einem eindimensional unendlichen Netzwerk verknüpft.
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  • 10
    ISSN: 0044-2313
    Keywords: Phosphoraneiminato Complexes of Antimony(III) ; Fluoro Complexes ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of the Phosphoraneiminato Complexes [SbF2(NPEt3)]2 and [SbF(NPEt3)2]2 as well as of NMe4+SbF4-The title compounds have been prepared from antimony trifluoride with the silylated phosphaneimine Me3SiNPEt3 and [NMe4]F, respectively. They were characterized by IR spectroscopy and by crystal structure determinations.[SbF2(NPEt3)]2: Space group Pbca, Z = 8, structure determination with 1264 unique reflections, R1 = 0.028 for reflections with I 〉 2σ(I). Lattice dimensions at -80°C: a = 1284.8, b = 1162.4, c = 1380.4 pm. The compound forms centrosymmetric dimeric molecules, in which the Ψ-trigonal-bipyramidal coordinated antimony atoms are linked via μ2-N bridges of the NPEt3- ligands.[SbF(NPEt3)2]2: Space group P21/c, Z = 4, structure determination with 2270 unique reflections, R1 = 0.029 for reflections with I 〉 2μ(I). Lattice dimensions at -75°C: a = 815.8, b = 1121.2, c = 2068.5 pm, β = 101.09°. The compound forms centrosymmetric dimeric molecules, in which the Ψ-trigonal-bipyramidal coordinated antimony atoms are linked via μ2-N bridges of one of the two NPEt3- ligands. The other NPEt3- group is terminally connected.NMe4+SbF4-: Space group P21/c, Z = 4, structure determination with 1503 unique reflections, R1 = 0.069 for reflections with I 〉 2μ(I). Lattice dimensions at -50°C: a = 539.80, b = 896.10, c = 1760.3 pm, β = 90.338°. The compound includes monomeric SbF4- ions with distorted Ψ-trigonal-bipyramidal environment of the antimony atoms.
    Notes: Die Titelverbindungen entstehen durch Reaktion von Antimontrifluorid mit dem silylierten Phosphanimin Me3SiNPEt3 bzw. mit Tetramethylammonium-Fluorid. Sie werden IR-spektroskopisch und durch Kristallstrukturanalysen charakterisiert.[SbF2(NPEt3)]2: Raumgruppe Pbca, Z = 8, Strukturlösung mit 1264 unabhängigen Reflexen, R1 = 0,028 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -80°C: a = 1284,8; b = 1162,4; c = 1380,4 pm. Die Verbindung bildet zentrosymmetrische dimere Moleküle, in denen die Ψ-trigonal-bipyramidal koordinierten Antimonatome über μ2-N-Brücken der NPEt3--Liganden verknüpft sind.[SbF(NPEt3)2]2: Raumgruppe P21/c, Z = 4, Strukturlösung mit 2270 unabhängigen Reflexen, R1 = 0,029 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -75°C: a = 815,8; b = 1121,2; c = 2068,5 pm; β = 101,09°. Die Verbindung bildet zentrosymmetrische dimere Moleküle, in denen die Ψ-trigonal-bipyramidal koordinierten Antimonatome über μ2-N-Brücken eines der beiden NPEt3--Liganden verknüpft sind. Die zweite NPEt3--Gruppe ist terminal gebunden.NMe4+SbF4-: Raumgruppe P21/c, Z = 4, Strukturlösung mit 1503 unabhängigen Reflexen, R1 = 0,069 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -50°C: a = 539,80; b = 896,10; c = 1760,3 pm; β = 90,338°. Die Verbindung enthält monomere SbF4--Ionen mit verzerrt Ψ-trigonal-bipyramidaler Umgebung der Antimonatome.
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