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  • 1
    Digitale Medien
    Digitale Medien
    The Catalytic Ring-opening Cyclooligomerization (ROC) of Thietane by the Complexes M(CO)5L (M = Cr and W; L = CO, thietane and 1,5,9-Trithiacyclododecane) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 313-318 
    Details
    ISSN: 0009-2940
    Schlagwort(e): Thietane ; Catalysis ; Tungsten ; Macrocycle ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The following four compounds have been synthesized: M(CO)5L (3 and 4, where M = Cr and W, and L = H2), W(CO)5(12S3) (5, where 12S3 = 1,5,9-trithia-cyclododecane), and [W(CO)5]2(12S3) (6). The molecular structures of 4 and 5 were established by single-crystal X-ray diffraction analyses. Both compounds contain a W(CO)5 group coordinated to one of the sulfur atoms of the hetero-cycle. The ability of the compounds M(CO)6, 1 and 2 (M = Cr and W), and 3 - 5 to catalytically produce ring opening cyclooligomerization (ROC) of thietane into 12S3 and 24S6, (24S6 = 1,5,9,13,17,21-hexathiacyclotetracosane) has been investigated. Compounds 1 - 3 have relatively low activity. Compounds 4 and 5 have the highest activity and selectivity for 12S3 formation. Crystal Data for 4: space group = P212121, a = 12.906(2) Å, b = 13.730(4) Å, c = 6.427(1) Å, Z = 4, 1306 reflections, R = 0.033; for 5: space group = P1¯, a = 12.703(1) Å, b = 13.510(2) Å, c = 5.833(1) Å, α = 101.75(1)°, β = 97.54(1)°, γ = 101.70(1)°, Z = 2, 2225 reflections, R = 0.023.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/cber.19961290311
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  • 2
    Digitale Medien
    Digitale Medien
    Synthese und Struktur der Phosphor-verbrückten Übergangsmetallkomplexe [Fe2(CO)6(PR)6] (R = tBu, iPr), [Fe2(CO)4(PiPr)6], [Fe2(CO)3Cl2(PtBu)5], [Co4(CO)10(PiPr)3], [Ni5(CO)10(PiPr)6] und [Ir4(C8H12)4Cl2(PPh)4] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1821-1831 
    Details
    ISSN: 0044-2313
    Schlagwort(e): Cyclotriphosphanes ; transition metal carbonyl complexes of Fe, Co, Ir, and Ni ; phosphorus-bridged ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: Synthesis and Structure of the Phosphorus-bridged Transition Metal Complexes [Fe2(CO)6(PR)6] (R = tBu, iPr), [Fe2(CO)4(PiPr)6], [Fe2(CO)3Cl2(PtBu)5], [Co4(CO)10(PiPr)3], [Ni5(CO)10(PiPr)6], and [Ir4(C8H12)4Cl2(PPh)4](PtBu)3 and (PiPr)3 react with [Fe2(CO)9] to form the dinuclear complexes [Fe2(CO)6(PR)6] (R = tBu: 1; iPr: 2). 2 is also formed besides [Fe2(CO)4(PiPr)6] (3) in the reaction of [Fe(CO)5] with (PiPr)3. When PiPr(PtBu)2 and PiPrCl2 are allowed to react with [Fe2(CO)9] it is possible to isolate [Fe2(CO)3Cl2(PtBu)5] (4). The reactions of (PiPr)3 with [Co2(CO)8] and [Ni(CO)4] lead to the tetra- and pentanuclear clusters [Co4(CO)10(PiPr)3] (5), [Ni4(CO)10(PiPr)6] [2] and [Ni5(CO)10(PiPr)6] (6). Finally the reaction of [Ir(C8H12)Cl]2 with K2(PPh)4 leads to the complex [Ir4(C8H12)4Cl2(PPh)4] (7). The structures of 1-7 were obtained by X-ray single crystal structure analysis (1: space group P21/c (Nr. 14), Z = 8, a = 1 758.8(16) pm, b = 3 625.6(18) pm, c = 1 202.7(7) pm, β = 90.07(3)°; 2: space group P1 (Nr. 2), Z = 1, a = 880.0(2) pm, b = 932.3(3) pm, c = 1 073.7(2) pm, α = 79.07(2)°, β = 86.93(2)°, γ = 72.23(2)°; 3: space group Pbca (Nr. 61), Z = 8, a = 952.6(8) pm, b = 1 787.6(12) pm, c = 3 697.2(30) pm; 4: space group P21/n (Nr. 14), Z = 4, a = 968.0(4) pm, b = 3 362.5(15) pm, c = 1 051.6(3) pm, β = 109.71(2)°; 5: space group P21/n (Nr. 14), Z = 4, a = 1 040.7(5) pm, b = 1 686.0(5) pm, c = 1 567.7(9) pm, β = 93.88(4)°; 6: space group Pbca (Nr. 61), Z = 8, a = 1 904.1(8) pm, b = 1 959.9(8) pm, c = 2 309.7(9) pm. 7: space group P1 (Nr. 2), Z = 2, a = 1 374.4(7) pm, b = 1 476.0(8) pm, c = 1 653.2(9) pm, α = 83.87(4)°, β = 88.76(4)°, γ = 88.28(4)°).
    Notizen: Die Cyclotriphosphane (PtBu)3 und (PiPr)3 reagieren mit [Fe2(CO)9] unter Bildung der Zweikernkomplexe [Fe2(CO)6(PR)6] (R = tBu: 1; iPr: 2). 2 entsteht auch bei der Reaktion von [Fe(CO)5] mit (PiPr)3 neben dem Komplex [Fe2(CO)4(PiPr)6] (3). Aus der Reaktion von PiPr(PtBu)2 und PiPrCl2 mit [Fe2(CO)9] kann weiterhin [Fe2(CO)3Cl2(PtBu)5] (4) isoliert werden. Die Umsetzungen von (PiPr)3 mit [Co2(CO)8] und [Ni(CO)4] führen zu den vier- und fünfkernigen Clustern [Co4(CO)10(PiPr)3] (5), [Ni4(CO)10(PiPr)6] [2] und [Ni5(CO)10(PiPr)6] (6). Weiterhin kann aus der Reaktion von [Ir(C8H12)Cl]2 mit K2(PPh)4 der Komplex [Ir4(C8H12)4Cl2(PPh)4] (7) erhalten werden. Die Strukturen von 1-7 konnten durch Einkristall-Röntgenstrukturanalyse aufgeklärt werden (1: Raumgruppe P21/c (Nr. 14), Z = 8, a = 1 758,8(16) pm, b = 3 625,6(18) pm, c = 1 202,7(7) pm, β = 90,07(3)°; 2: Raumgruppe P1 (Nr. 2), Z = 1, a = 880,0(2) pm, b = 932,3(3) pm, c = 1 073,7(2) pm, α = 79,07(2)°, β = 86,93(2)°, γ = 72,23(2)°; 3: Raumgruppe Pbca (Nr. 61), Z = 8, a = 952,6(8) pm, b = 1 787,6(12) pm, c = 3 697,2(30) pm; 4: Raumgruppe P21/n (Nr. 14), Z = 4, a = 968,0(4) pm, b = 3 362,5(15) pm, c = 1 051,6(3) pm, β = 109,71(2)°; 5: Raumgruppe P21/n (Nr. 14), Z = 4, a = 1 040,7(5) pm, b = 1 686,0(5) pm, c = 1 567,7(9) pm, β = 93,88(4)°; 6: Raumgruppe Pbca (Nr. 61), Z = 8, a = 1 904,1(8) pm, b = 1 959,9(8) pm, c = 2 309,7(9) pm. 7: Raumgruppe P1 (Nr. 2), Z = 2, a = 1 374,4(7) pm, b = 1 476,0(8) pm, c = 1 653,2(9) pm, α = 83,87(4)°, β = 88,76(4)°, γ = 88,28(4)°).
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/zaac.19946201027
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  • 3
    Digitale Medien
    Digitale Medien
    Neue Phosphor-verbrückte Übergangsmetallcarbonyl-Komplexe Die Kristallstrukturen von [Re2(CO)7(PtBu)3], [Co4(CO)10(PtBu)2], [Ir4(CO)6(PtBu)6] und [Ni4(CO)10(PiPr)6] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 58-66 
    Details
    ISSN: 0044-2313
    Schlagwort(e): Cyclotriphosphanes ; multinuclear phosphorus-bridged complexes of Re, Mn, Co, Ir and Ni ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: New Phosphorus-bridged Transition Metal Carbonyl Complexes. The Crystal Structures of [Re2(CO)7(PtBu)3], [Co4(CO)10(PtBu)2], [Ir4(CO)6(PtBu)6], and [Ni4(CO)10(PiPr)6],(PtBu)3 reacts with [Mn2(CO)10], [Re2(CO)10], [Co2(CO)8] and [Ir4(CO)12] to form the multinuclear complexes [M2(CO)7(PtBu)3] (M = Re (1), Mn (5)), [Co4(CO)10(PtBu)2] (2) and [Ir4(CO)6(PtBu)6] (3). The reaction of (PiPr)3 with [Ni(CO)4] leads to the tetranuclear cluster [Ni4(CO)10(PiPr)6] (4). The complex structures were obtained by X-ray single crystal structure analysis: (1: space group P1 (Nr. 2), Z = 2, a = 917.8(3) pm, b = 926.4(3) pm, c = 1 705.6(7) pm, α = 79.75(3)°, β = 85.21(3)°, γ = 66.33(2)°; 2: space group C2/c (Nr. 15), Z = 4, a = 1 347.7(6) pm, b = 1 032.0(3) pm, c = 1 935.6(8) pm, β = 105.67(2)°; 3: space group P1 (Nr. 2), Z = 4, a = 1 096.7(4)pm, b = 1 889.8(10)pm, c = 2 485.1(12) pm, α = 75.79(3)°, β = 84.29(3)°, γ = 74.96(3)°; 4: space group P21/c (Nr. 14), Z = 4, a = 2 002.8(5) pm, b = 1 137.2(8) pm, c = 1 872.5(5) pm, β = 95.52(2)°).
    Notizen: Das Cyclotriphosphan (PtBu)3 reagiert mit [Mn2(CO)10], [Re2(CO)10], [Co2(CO)8] und [Ir4(CO)12] unter Bildung der Mehrkernkomplexe [M2(CO)7(PtBu)3] (M = Re (1), Mn (5)), [Co4(CO)10(PtBu)2] (2) und [Ir4(CO)6(PtBu)6] (3). Die Umsetzung von (PiPr)3 mit [Ni(CO)4] führt zu dem vierkernigen Cluster [Ni4(CO)10(PiPr)6] (4). Die Strukturen der Komplexe konnten durch Einkristall-Röntgenstrukturanalyse aufgeklärt werden (1: Raumgruppe P1 (Nr.2), Z = 2, a = 917,8(3)pm, b = 926,4(3)pm, c = 1 705,6(7)pm, α = 79,75(3)°, β = 85,21(3)°, γ = 66,33(2)°; 2: Raumgruppe C2/c (Nr. 15), Z = 4, a = 1 347,7(6) pm, b = 1 032,0(3) pm, c = 1 935,6(8) pm, β = 105,67(2)°; 3: Raumgruppe P1 (Nr. 2), Z = 4, a = 1 096,7(4) pm, b = 1 889,8(10) pm, c = 2 485,1(12) pm, α = 75,79(3)°, β = 84,29(3)°, γ = 74,96(3)°; 4: Raumgruppe P21/c (Nr. 14), Z = 4, a = 2 002,8(5) pm, b = 1 137,2(8) pm, c = 1 872,5(5) pm, β = 95,52(2)°).
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/zaac.19946200110
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  • 4
    Digitale Medien
    Digitale Medien
    Neue Phosphor-verbrückte Übergangsmetall-Komplexe Die Kristallstrukturen von [Co4(CO)10(PiPr)2], [Fe3(CO)9(PtBu)(PPh)], [Cp3Fe3(CO)2(PPtBu)(PtBu)], [(NiPPh3)2(PiPr)6], [(NiPPh3)Ni{(PtBu)3}2] und [Ni8(PtBu)6(PPh3)2] (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1731-1739 
    Details
    ISSN: 0044-2313
    Schlagwort(e): transition metal carbonyl complexes of Fe, Co, Ni, with cyclotriphosphanes, cyclotetraphosphanes ; structure ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: New Phosphorus-bridged Transition Metal Complexes The Crystal Structures of [Co4(CO)10(PiPr)2], [Fe3(CO)9(PtBu)(PPh)], [Cp3Fe3(CO)2(PPtBu)· (PtBu)], [(NiPPh3)2(PiPr)6], [(NiPPh3)Ni{(PtBu)3}2], and [Ni8(PtBu)6(PPh3)2]By the reaction of cyclophosphines with transition metal carbonyl-derivatives polynuclear complexes are built, in which the PR-ligands (R = organic group) are bonded in different ways to the metal. Depending on the reaction conditions the following compounds can be characterized: [Co4(CO)10 · (PiPr)2] (2), [Fe3(CO)9(PtBu)(PPh)] (3), [Cp3Fe3(CO)2(PPtBu) · (PtBu)] (4), [(NiPPh3)2(PiPr)6] (5), [(NiPPh3)Ni{(PtBu)3}2] (6) and [Ni8(PtBu)6(PPh3)2] (7). The structures of 2-7 were obtained by X-ray single crystal structure analysis (2: space group Pccn (No. 56), Z = 4, a = 1001,4(2) pm, b = 1375,1(3) pm, c = 1675,5(3) pm; 3: space group P21 (No. 4), Z = 2, a = 914,3(4) pm, b = 1268,7(4) pm, c = 1028,2(5) pm, β = 101,73(2)°; 4: space group P1 (No. 2), Z = 2, a = 946,0(5) pm, b = 1074,4(8) pm, c = 1477,7(1,0) pm, α = 107,63(5)°, β = 94,66(5)°, γ = 111,04(5)°; 5: space group P1 (No. 2), Z = 2, a = 1213,6(2) pm, b = 1275,0(2) pm, c = 2038,8(4) pm, α = 92,810(10)°, β = 102,75(2)°, γ = 93,380(10)°; 6: space group P1 (No. 2), Z = 2, a = 1157,5(5) pm, b = 1371,9(6) pm, c = 1827,6(10) pm; α = 69,68(3)°, β = 80,79(3)°, γ = 69,36(3)°; 7: space group P3 (No. 147), Z = 1, a = 1114,1(2) pm, b = 1114,1(2) pm, c = 1709,4(3) pm).
    Notizen: Bei der Umsetzung von Cyclophosphanen mit Übergangsmetallcarbonylderivaten entstehen mehrkernige Komplexe, in denen die PR-Liganden (R = organische Gruppe) in unterschiedlicher Form an das Metall gebunden sind. Abhängig von den Reaktionsbedingungen konnten folgende Verbindungen charakterisiert werden: [Co4(CO)10(PiPr)2] (2), [Fe3(CO)9 · (PtBu)(PPh)] (3), [Cp3Fe3(CO)2(PPtBu)(PtBu)] (4), [(NiPPh3)2 · (PiPr)6] (5), [(NiPPh3)Ni{(PtBu)3}2] (6) und [Ni8(PtBu)6(PPh3)2] (7). Die Strukturen von 2 - 7 konnten durch Einkristall-Röntgenstrukturanalyse aufgeklärt werden (2: Raumgruppe Pccn (Nr. 56), Z = 4, a = 1001,4(2) pm, b = 1375,1(3) pm, c = 1675,5(3) pm; 3: Raumgruppe P21 (Nr. 4), Z = 2, a = 914,3(4) pm, b = 1268,7(4) pm, c = 1028,2(5) pm, β = 101,73(2)°; 4: Raumgruppe P1 (Nr. 2), Z = 2, a = 946,0(5) pm, b = 1074,4(8) pm, c = 1477,7(1,0) pm, α = 107,63(5)°, β = 94,66(5)° γ = 111,04(5)°; 5: Raumgruppe P1 (Nr. 2), Z = 2, a = 1213,6(2) pm, b = 1275,0(2) pm, c = 2038,8(4) pm, α = 92,810(10)°, β = 102,75(2)°, γ = 93,380(10)°; 6: Raumgruppe P1 (Nr. 2), Z = 2, a = 1157,5(5) pm, b = 1371,9(6) pm, c = 1827,6(10) pm; α = 69,68(3)°, β = 80,79(3)°, γ = 69,36(3)°; 7: Raumgruppe P3 (Nr. 147), Z = 1, a = 1114,1(2) pm, b = 1114,1(2) pm, c = 1709,4(3) pm).
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/zaac.19966221018
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