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  • 1
    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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  • 2
    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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  • 3
    ISSN: 0044-2313
    Keywords: Magnesium Compounds ; Phosphoraneiminato Complexes ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphaneimine and Phosphoraneiminato Complexes of Magnesium. The Crystal Structures of [MgBr1,25I0,75(Me3SiNPMe3)(OEt2)], [MgI2(Me3SiNPMe3)2], [Mg2I2(Me3SiNPMe2CH2)(Me3SiNPMe2CH2CH(Me)O)(OEt2)], and [MgBr(NPMe3)]4 · C7H8By reactions of the silylated phosphaneimine Me3SiNPMe3 with the Grignard reagents EtMgBr and MeMgI, respectively, the carbanionic phosphoraneiminato derivatives [XMg(CH2PMe2NSiMe3)]n (X = Br, I) can be isolated as main products. The by-products of these reactions, [MgBr1.25I0.75(Me3SiNPMe3)(OEt2)], [MgI2(Me3SiNPMe3)2] and [Mg2I2(CH2PMe2NSiMe3)(O(Me)CHCH2PMe2NSiMe3)(OEt2)] were identified by crystal structure determinations. The phosphoraneiminato complex [MgBr(NPMe3)]4 · C7H8 with hetero cubane structure is formed by a metathesis reaction of [ZnBr(NPMe3)]4 with RMgBr (R = Ph. Mes).
    Notes: Als Hauptprodukte der Umsetzungen des silylierten Phosphanimins Me3SiNPMe3 mit den Grignard-Reagentien EtMgBr und MeMgl wurden die carbanionischen Phosphaniminato-Derivate [XMg(CH2Pme2NSiMe3)]n (X = Br, I) isoliert. Als Nebenprodukte wurden [MgBr1,25I0,75(Me3SiNPMe3)(OEt2)], [Mgl2(Me3SiNPMe3)2] und [Mg2I2(CH2PMe2NSiMe3)(O(Me)CHCH2PMe2NSiMe3(OEt2)] durch röntgenographische Strukturanalysen identifiziert. Den Phosphaniminato-Komplex [MgBr(NPMe3)]4 · C7H8 mit Heterocuban-Struktur erhielten wir durch Metathese-Reaktion aus [ZnBr(NPMe3)]4 und RMgBr (R = Ph, Mes).
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  • 4
    ISSN: 0044-2313
    Keywords: Silylated λ5-Phosphazenes ; Synthesis ; NMR spectra ; 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 Silylated λ5-Phosphazenes R—C(CH2PPh2NSiMe3)3 with R = H and CH3The title compounds are obtained by Staudinger reaction from the corresponding tripodal phosphanes R—C(CH2PPh2)3 and trimethylsilylazide. Both complexes are characterized by their IR and NMR spectra and by crystal structure analyses.H—C(CH2PPh2NSiMe3)3 (1): Space group P21/c, Z = 4, structure determination with 7833 independent reflections, R = 0.055. Lattice dimensions at -50°C: a = 1399.5, b = 2311.4, c = 1678.9 pm, β = 112.92°.CH3—C(CH2PPh2NSiMe3)3 (2): Space group P1, Z = 2, structure determination with 9251 independent reflections, R = 0.057. Lattice dimensions at -50°C: a = 1276.5, b = 1386.9, c = 1790.2 pm; α = 85.55°, β = 69.39°, γ = 62.99°.1 and 2 form monomeric molecules which are distinguished by their conformation.
    Notes: Die Titelverbindungen werden durch Staudinger-Reaktion aus den entsprechenden tripodalen Phosphanen R—C(CH2PPh2)3 und Trimethylsilylazid hergestellt und durch ihre IR- und NMR-Spektren sowie durch Kristallstrukturanalysen charakterisiert.H—C(CH2PPh2NSiMe3)3 (1): Raumgruppe P21/c, Z = 4, Strukturbestimmung mit 7833 unabhängigen Reflexen, R = 0,055. Gitterkonstanten bei -50°C: a = 1399,5; b = 2311,4; c = 1678,9 pm; β = 112,92°.CH3—C(CH2PPh2NSiMe3)3 (2): Raumgruppe P1, Z = 2, Strukturbestimmung mit 9251 unabhängigen Reflexen, R = 0,057. Gitterkonstanten bei -50°C: a = 1276,5; b = 1386,9; c = 1790,2 pm; α = 85,55°; β = 69,39°; γ = 62,99°.1 und 2 bilden monomere Moleküle, die sich durch ihre Konformation unterscheiden.
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  • 5
    ISSN: 0044-2313
    Keywords: Polytellurides ; Syntheses ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of the Polytellurides [Ca(DMF)6]Te4, [Sr(15-Crown-5)2]Te4 · H2O, {[BaCl(18-Crown-6)(DMF)2]2[BaCl(18-Crown-6)(DMF) (H2O)]2(Te4)2}, and [Ph3PNPPh3]2Te5 · 2 DMFThe title compounds were formed by alkalimetal polytelluride solutions in dimethylformamide (DMF) in the presence of the corresponding counter ions as well as in the presence of 15-crown-5 or 18-crown-6. Single crystals were obtained upon using additional diethylether.[Ca(DMF)6]Te4: Space group C2/c, Z = 4, 1024 observed unique reflections, R = 0.055. Lattice dimensions at -70°C: a = 1776.1; b = 813.0 c = 2545.9pm; β = 102.90°. The compound consists of centrosymmetric [Ca(DMF)6]2+ ions, in which the calcium ions are octahedrally coordinated by the six oxygen atoms of the DMF molecules, and chain-like Te42-[Sr)15-crown-5)2]Te4 · H2O: Space group C2/c, Z = 4, 3322 observed unique reflections, R = 0.058. Lattice dimensions at -70°C: a = 1450.5; b = 1407.3; c = 1660.9 pm; β = 110.22°. The compounds forms centrosymmetric cations [Sr(15-crown-5) 2]2+, in which the Sr2+ ion is sandwich-like surrounded by the ten oxygen atoms of the crown ether molecules, and chain-like Te42- ions, which are associated in the lattice forming polymeric chains.{[BaCl(18-crown-6)(DMF) 2]2[BaCl(18-crown-6)(DMF)· (H2O)] 2(Te4)2}: Space group P1, Z = 1, 3189 observed unique reflections, R = 0.054. Lattice dimensions at 19°C: a = 986.1; b = 1052.8; c = 2696.4 pm; α = 89.34°; β = 88.68°; γ = 89.56°. The compound consists of chain-like Te42- ions without symmetry and of the two somewhat different cations [BaCl(18-crown-6)(DMF) 2]22+, in which the Ba2+ ions dimerize via centroysmmetric rings. Along with the six oxygen atoms of the crown ether molecules and the oxygen atoms of the DMF molecules, the oxygen atoms of the DMF and water molecule, respectively, the Ba+ ions achieve coordination number ten.[Ph3PNPPh3]2Te5 · 2DMF: Space group Pc, Z = 2, 5971 observed unique reflections, R = 0.058. Lattice dimensions at 20°C: a = 20°C: a = 1085.2; b = 1287.0; c = 2715.9 pm; β = 90.19°. The compounds consists of [Ph3PNPPh3]+ ions, chain-like Te52- ions, and incorporate DME molecules without bonding interaction. The 52- ions are associate via polymeric chains in which left- and right handed individuals are alternating.
    Notes: Die Titelverbindungen entstehen aus Alkalipolytelluridlösungen in Dimethylformamid (DMF) in Gegenwart der entsprechenden Gegenionen und der Kronenether 15-Krone-5 bzw. 18-Krone-6. Einkristalle werden durch Zusatz von Diethylether gebildet.[Ca(DMF)6]Te4: Raumgruppe C2/c, Z = 4, 1024 beobachtete unabhängige Reflexe, R = 0,055. Gitterabmessungen bei -70°C: a =1 776,1; b =813,0; c = 2 545,9 pm; β = 102,90°. Die Verbindung besteht aus zentrosymmetrischen Kationen [Ca(DMF)6]2+, in denen die Calciumionen oktaedrisch von den sechs O-Atomen der DMF-Moleküle umgeben sind, und Te42--Ionen mit Kettenstruktur.[Sr(15-Krone-5)2]Te4 · H2O: Raumgruppe C2/c, Z = 4, 3322 beobachtete unabhängige Reflexe, R = 0,058. Gitterabmessungen bei -70°C: a = 1 450,5; b = 1 407,3; c = 1 660,9 pm; β = 110,22°. Die Verbindung bildet Kationen [Sr(15-Krone-5)2]2+, in denen das Strontiumion zentrosymmetrisch und sandwichartig von den zehn O-Atomen der beiden Kronenethermoleküle umgeben ist, sowie kettenförmigen Te42--Ionen, die im Gitter zu polymeren Tellursträngen assoziiert sind.{[BaCl(18-Krone-6)(DMF)2]2[BaCl(18-Krone-6)(DMF)· (H2O)]2(Te4)2}: Raumgruppe P1, Z = 1, 3189 beobachtete unabhängige Reflexe, R = 0,054. Gitterabmessungen bei 19°C: a = 986,1; b = 1 052,8; c = 2 696,4 pm; α = 89,34°; β = 88,68°; γ= 89,56°. Die Verbindung besteht aus kettenförmigen Tetratelluridionen ohne Symmetrie und den beiden etwas verschiedenen Kationen [BaCl(18-Krone-6)(DMF)2]22+ und [BaCl(18-Krone-6)(DMF)(H2O)]22+. In diesen sind die Bariumionen zentrosymmetrisch über BaCl2Ba-Brücken dimerisiert, wodurch die Ba2+-Ionen mit den sechs O-Atomen des Kronenethers und den O-Atomen der DMF-Moleküle bzw. denen des DMF- und des H2O-Moleküls die Koordinationszahl zehn erreichen.[Ph3PNPPh3]2Te5 · 2 DMF: Raumgruppe Pc, Z = 2, 5971 beobachtete unabhängige Reflexe, R = 0,058. Gitterabmessungen bei 20°C: a = 1 085,2; b = 1 287,0; c = 2 715,9 pm; β = 90,19°. Die Verbindung besteht aus [Ph3PNPPh3]+-Ionen, kettenförmigen Pentatelluridionen und eingelagerten DMF-Molekülen ohne bindende Wechselwirkung. Die Te52--Ionen sind zu unendlichen Ketten assoziiert, wobei links- und rechtsdrehende Individuen einander abwechseln.
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  • 6
    ISSN: 0044-2313
    Keywords: Phosphaneimine Complexes of Zinc and Cobalt ; Synthesis ; IR spectra ; 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 Phosphaneimine Complexes MCl2(Me3SiNPMe3)2 with M = Zn and Co, and CoCl2(HNPMe3)2The molecular complexes MCl2(Me3SiNPMe3)2 (M = Zn, Co) have been prepared by the reaction of the dichlorides of zinc and cobalt with Me3SiNPMe3 in CH3CN and CH2Cl2, respectively, whereas the complex CoCl2(HNPMe3)2 has been prepared by the reaction of CoCl2 with NaF in boiling acetonitrile in the presence of Me3SiNPMe3. All complexes were characterized by IR spectroscopy and by crystal structure determinations. The complexes MCl2(Me3SiNPMe3)2 crystallize isotypically.ZnCl2(Me3SiNPMe3)2: Space group P212121, Z = 4, 2677 observed unique reflections, R = 0.024. Lattice dimensions at -70°C: a = 1243.6; b = 1319.0; c = 1464.7 pm.CoCl2(Me3SiNPMe3)2: Space group P212121, Z = 4, 3963 observed unique reflections, R = 0,071. Lattice dimensions at -80°C: a = 1236.3; b = 1317.4; c = 1457.6 pm.CoCl2(HNPMe3)2 · CH2Cl2: Space group Pbca, Z = 8, 1354 observed unique reflections, R = 0.055. Lattice dimensions at -80°C: a = 1247.3; b = 998.4; c = 2882.4 pm.All complexes have monomeric molecular structures, in which the metal atoms are coordinated in a distorted tetrahedral fashion by the two chlorine atoms and by the nitrogen atoms of the phosphaneimine molecules.
    Notes: Die Molekülkomplexe MCl2(Me3SiNPMe3)2 (M = Zn, Co) entstehen aus den wasserfreien Dichloriden von Zink und Cobalt mit Trimethylsilyl-trimethylphosphanimin in Dichlormethan bzw. Acetonitril, während der Trimethylphosphanimin-Komplex CoCl2(HNPMe3)2 aus CoCl2 mit Natriumfluorid in Gegenwart von Me3SiNPMe3 in siedendem Acetonitril gebildet wird. Die Verbindungen werden durch ihre IR-Spektren und durch Kristallstrukturanalysen charakterisiert. Die Komplexe MCl2(Me3SiNPMe3)2 (M = Zn, Co) sind miteinander isotyp.ZnCl2(Me3SiNPMe3)2: Raumgruppe P212121, Z = 4, Strukturlösung mit 2677 beobachteten unabhängigen Reflexen, R = 0,024. Gitterkonstanten bei -70°C: a = 1243,6; b = 1319,0; c = 1464,7 pm.CoCl2(Me3SiNPMe3)2: Raumgruppe P212121, Z = 4, Strukturlösung mit 3963 beobachteten unabhängigen Reflexen, R = 0,071. Gitterkonstanten bei -80°C: a = 1236,3; b = 1317,4; c = 1457,6 pm.CoCl2(HNPMe3)2 · CH2Cl2: Raumgruppe Pbca, Z = 8, Strukturlösung mit 1354 beobachteten unabhängigen Reflexen, R = 0,055. Gitterkonstanten bei -80°C: a = 1247,3; b = 998,4; c = 2882,4 pm.Alle Komplexe haben monomere Molekülstrukturen, in denen die Metallatome verzerrt tetraedrisch von den beiden Chloratomen und den N-Atomen der beiden Phosphaniminmoleküle koordiniert sind.
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  • 7
    ISSN: 0044-2313
    Keywords: Triphenylarsin-p-toluene sulfonylimine ; Zirconium tetrachloride complex ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of Triphenylarsin-p-toluene Sulfonylimine and of its Donor-Acceptor Complex [ZrCl4(Ph3AsNSO2Tol)]2The molecular structures of the title compounds are reported. In the donor-acceptor complex [ZrCl4(Ph3AsNSO2Tol)]2 the zirconium atoms are bridged by the oxygen atoms of the triphenylarsin-p-toluene sulfonylimine molecules, forming a centrosymmetric dimer with a puckered Zr2O4S2 eight-membered ring in the chair conformation.Ph3AsNSO2Tol: Space group P1, Z = 2, structure determination with 4 010 observed unique reflections, R = 0.036. Lattice dimensions at 19°C: a = 897.52(4), b = 1 071.82(6), c = 1 337,49(5) pm, α = 110.280(4)°, β = 98.814(4)°, γ = 109.872(4)°.[ZrCl4(Ph3AsNSO2Tol)]2: Space group P21/n, Z = 4, structure determination with 3 762 observed unique reflections, R = 0.078. Lattice dimensions at -60°C: a = 1 387.3(4), b = 1 434.9(2), c = 1 404.7(4) pm, β = 92.71(1)°.
    Notes: Es wird über die Molekülstrukturen der beiden Titelverbindungen berichtet. In dem Donor-Akzeptorkomplex [ZrCl4(Ph3AsNSO2Tol)]2 sind die Zirkoniumatome über die O-Atome der Triphenylarsin-p-toluolsulfonylimin-Moleküle zu einem zentrosymmetrischen Dimer mit einem Zr2O4S2-Achtring in der Sesselkonformation verknüpft.Ph3AsNSO2Tol: Raumgruppe P1, Z = 2, Strukturlösung mit 4 010 unabhängigen beobachteten Reflexen, R = 0,036. Gitterkonstanten bei 19°C: a = 897,52(4), b = 1 071,82(6), c = 1 337,49(5) pm, α = 110,280(4)°, β = 98,814(4)°, γ = 109,872(4)°.[ZrCl4(Ph3AsNSO2Tol)]2: Raumgruppe P21/n, Z = 4, Strukturlösung mit 3 762 unabhängigen beobachteten Reflexen, R = 0,078. Gitterkonstanten bei -60°C: a = 1 387,3(4), b = 1 434,9(2), c = 1 404,7(4) pm, β = 92,71(1)°.
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  • 8
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes of Antimony ; 121Sb Mössbauer Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorane Iminato Complexes of Antimony. The Crystal Structures of [Sb2Cl5(NPMe3)2][SbCl6] · CH3CN and [SbCl(NPPh3)]2[SbCl6]2 · 6 CH3CNThe title compounds are formed by reaction of antimony pentachloride in acetonitrile solution with the phosphorane iminato complexes SbCl2(NPMe3) and SbCl2(NPPh3), respectively, which themselves are synthesized by reaction of antimony trichloride with Me3SiNPR3 (R = Me, Ph). The complexionic compounds are characterized by 121Sb Mössbauer spectroscopy and by crystal structure determinations.[Sb2Cl5(NPMe3)2][SbCl6] · CH3CN: Space group P41, Z = 4, 3 698 observed unique reflections, R = 0.022. Lattice dimensions at -60°C: a = b = 1 056.0(1), c = 2 709.6(2) pm. The structure consists of SbCl6- ions and cations [Sb2Cl5(NPMe3)2(CH3CN)]+, in which one SbIII atom and one SbV atom are bridged by the N atoms of the phosphorane iminato ligands.[SbCl(NPPh3)]2[SbCl6]2 · 6 CH3CN: Space group P1, Z = 2, 5 958 observed unique reflections, R = 0.033. Lattice dimensions at -60°C: a = 989.4(11), b = 1 273(1), c = 1 396(1) pm, α = 78.33(7), β = 77.27(8)°, γ = 86.62(8)°. The structure consists of SbCl6- ions and centrosymmetric cations [SbCl(NPPh3)(CH3CN)2]22+, in which the antimony atoms are bridged by the N atoms of the phosphorane iminato ligands.
    Notes: Die Titelverbindungen entstehen durch Reaktion von Antimonpentachlorid in Acetonitrillösungen mit den Phosphaniminatokomplexen SbCl2(NPMe3) bzw. SbCl2(NPPh3), die ihrerseits aus Antimontrichlorid und Me3SiNPR3 (R = Me, Ph) hergestellt werden. Die ionisch aufgebauten Komplexe werden durch ihre 121Sb-Mößbauer-Spektren und durch Kristallstrukturanalysen charakterisiert.[Sb2Cl5(NPMe3)2][SbCl6] · CH3CN: Raumgruppe P41, Z = 4, 3 698 beobachtete unabhängige Reflexe, R = 0,022. Gitterabmessungen bei -60°C: a = b = 1 056,0(1); c = 2 709,6(2) pm. Die Struktur wird aus SbCl6--Ionen und Kationen [Sb2Cl5(NPMe3)2(CH3CN)]+ gebildet, in denen ein SbIII- und ein SbV-Atom über die N-Atome der Phosphaniminatoliganden verknüpft sind.[SbCl(NPPh3)]2[SbCl6]2 · 6 CH3CN: Raumgruppe P1, Z = 2, 5 958 beobachtete unabhängige Reflexe, R = 0,033. Gitterkonstanten bei -60°C: a = 989,4(11); b = 1 273(1); c = 1 396(1) pm; α = 78,33(7)°; β = 77,27(8)°; γ = 86,62(8)°. Die Verbindung besteht aus SbCl6--Ionen und zentrosymmetrischen Kationen [SbCl(NPPh3)(CH3CN)2]22+, in denen die beiden Antimonatome über die N-Atome der Phosphaniminatoliganden verknüpft sind.
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  • 9
    ISSN: 0044-2313
    Keywords: Alkoxy-Alkyne Complexes of Tungsten ; Synthesis ; 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 Tungsten(VI)-alkyne Complexes [W2(O)(OMe)6(Et—Se—C≡C—Se—Et)2] and Li[W(OMe)5(Et—Te—C≡C—Te—Et)]The title compounds have been prepared by reactions of lithium methanolate with [WCl4(Et—Se—C≡C—Se—Et)(THF)] and [WCl4(Et—Te—C≡C—Te—Et)(THF)], respectively, in diethylether suspensions. Both complexes were characterized by crystal structure determinations.[W2(O)(OMe)6(Et—Se—C≡C—Se—Et)2]: Space group P1, Z = 2, structure determination with 4 320 observed unique reflections, R = 0.041. Lattice dimensions at -70°C: a = 949.3, b = 1 225.3, c = 1 285.0 pm, α = 82.48°; γ = 82.44°; β = 81.44°. The tungsten atoms are bridged by three μ2-O-atoms of the OMe groups; the alkyne ligands are coordinated side-on in a metallacyclopropene-like fashion.Li[W(OMe)5(Et—Te—C≡C—Te—Et)]: Space group P1, Z = 2, structure determination with 9 381 observed unique reflections, R = 0.038. Lattice dimensions at -70°C: a = 983.4, b = 1606.9, c = 1971.5 pm, α = 66.09°, β = 84.29°, γ = 79.83°. The lithium ions link the [W(OMe)5(Et—Te—C≡C—Te—Et)]- anions to a trimeric ion ensemble via the O atoms of three OMe groups of each anion.
    Notes: Die Titelverbindungen werden durch Reaktion von Lithiummethanolat mit [WCl4(Et—Se—C≡C—Se—Et)(THF)] bzw. mit [WCl4(Et—Te—C≡C—Te—Et)(THF)] in Diethylether hergestellt und durch Kristallstrukturanalysen charakterisiert.[W2(O)(OMe)6(Et—Se—C≡C—Se—Et)2]: Raumgruppe P1, Z = 2, Strukturlösung mit 4 320 beobachteten unabhängigen Reflexen, R = 0,041. Gitterabmessungen bei -70°C: a = 949,3; b = 1225,3; c = 1285,0 pm, α = 82,48°; β = 82,44°; γ = 81,44°. Die beiden Wolframatome sind über drei μ2-OMe-Brücken verknüpft; die Alkinliganden sind seitlich entsprechend von Metallacyclopropengruppen koordiniert.Li[W(OMe)5(Et—Te—C≡C—Te—Et)]: Raumgruppe P1, Z = 2, Strukturlösung mit 9 381 beobachteten unabhängigen Reflexen, R = 0,038. Gitterabmessungen bei -70°C: a = 983,4; b = 1606,9; c = 1971,5 pm, α = 66,09°; β = 84,29°; β = 79,83°. Die Lithiumionen verknüpfen die [W(OMe)5(Et—Te—C≡C—Te—Et)]--Anionen über die O-Atome dreier OMe-Gruppen zu einem trimeren Ionenensemble.
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  • 10
    ISSN: 0044-2313
    Keywords: Functionalized Alkyne Complexes of Tungsten ; Synthesis ; IR spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Functionalized Alkyne Complexes of Tungsten(VI). Syntheses and Crystal Structures of [WCl4(Et—Se—C≡C—Se—Et)(THF)] and [WCl4(Et—Te—C≡C—Te—Et)(THF)]The title compounds have been prepared by reactions of [WCl4(SEt2)2] with the alkynes Et—X—C≡C—X—Et (X = Se, Te) in CCl4 solution and subsequent addition of tetrahydrofurane. Both complexes were characterized by crystal structure determinations.[WCl4(Et—Se—C≡C—Se—Et)(THF)]: Space group P21/n, Z = 4, structure determination with 2942 unique reflections, R = 0.038. Lattice dimensions at 20°C: a = 934.2, b = 1639.5, c = 1189.5 pm, β = 96.497°.[WCl4(Et—Te—C≡C—Te—Et)(THF)]: Space group P21/n, Z = 4, structure determination with 4097 unique reflections, R = 0.067, Lattice dimensions at -70°C: a = 899.2, b = 1691.9, c = 1213.3 pm, β = 96.82°.The complexes have monomeric molecular structures with the oxygen atom of the THF molecules in trans-position to the side-on bound alkyne ligands.
    Notes: Die Titelverbindungen werden aus [WCl4(SEt2)2] und den Alkinen Et—X—C≡C—X—Et (X = Se, Te) in CCl4-Lösung nach Zusatz von Tetrahydrofuran erhalten und durch Kristallstrukturanalysen charakterisiert.[WCl4(Et—Se—C≡C—Se—Et)(THF)]: Raumgruppe P21/n, Z = 4, Strukturverfeinerung mit 2942 unabhängigen Reflexen, R = 0,038. Gitterabmessungen bei 20°C: a = 934,2; b = 1639,5; c = 1189,5 pm, β = 96,497°.[WCl4(Et—Te—C≡C—Te—Et)(THF)]: Raumgruppe P21/n, Z = 4, Strukturverfeinerung mit 4097 unabhängigen Reflexen, R = 0,067. Gitterabmessungen bei -70°C: a = 899,2; b = 1691,9; c = 1213,3 pm, β = 96,82°.Beide Verbindungen haben monomere Molekülstrukturen, in denen sich das O-Atom des THF-Moleküls in trans-Position zum seitlich gebundenen Alkinliganden befindet.
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