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  • 1
    Electronic Resource
    Electronic Resource
    Synthesis and Characterization of cis- and trans-Tetrachlorobis(pyridine)platinum(IV)Dedicated to Professor Siegfried Engels on the Occasion of his 65th Birthday (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 603-607 
    Details
    ISSN: 0044-2313
    Keywords: Platinum complex ; crown ether ; Raman and IR data ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Charakterisierung von cis- und trans-Tetrachlorobis(pyridin)platin(IV)[Na(15-cr-5)]2[PtCl6] · 2 H2O reagiert mit Pyridin in Wasser als Lösungsmittel zu cis-[PtCl4(py)2] (1) und in MeCN, DMF sowie in CH2Cl2 zu trans-[PtCl4(py)2] (2). Die Substitutionsreaktion wird durch Bestrahlung mit sichtbarem Licht beschleunigt. Sowohl gelöst in DMSO, DMF und MeCN als auch bei 503 K im festen Zustand isomerisiert 1 zu 2.1 und 2 sind umfassend IR- und ramanspektroskopisch charakterisiert worden. Die Molekülstruktur des trans-Isomeren 2 wurde auch durch Röntgeneinkristallstrukturunterschung ermittelt (monoklin, C2/m, a = 14.143(5), b = 7.171(3), c = 7.199(3) Å, β = 116.42(4)°, Z = 2, R1 = 0.0331, wR2 = 0.0727). 2 weist angenähert D2h Symmetrie auf, wobei die beiden trans-ständigen Pyridinliganden in einer Ebene liegen. Nach quantenchemischen Berechnungen ist 2 (D2h-Symmetrie) um 48.28 kJ/mol stabiler als 1 (C2v-Symmetrie).
    Notes: [Na(15-cr-5)]2[PtCl6] · 2 H2O reacts with pyridine in water as solvent to give cis-[PtCl4(py)2] (1) and in MeCN, DMF or in CH2Cl2 to give trans-[PtCl4(py)2] (2). The substitution reaction can be accelerated by irradiation with visible light. 1 isomerizes to give 2 in DMSO, DMF and MeCN as well as in solid state at 503 K.1 and 2 were thoroughly characterized IR and Raman spectroscopically. The molecular structure of the trans isomer 2 was also established by X-ray structure analysis (monoclinic, C2/m, a = 14.143(5), b = 7.171(3), c = 7.199(3) Å, β = 116.42(4)°, Z = 2, R1 = 0.0331, wR2 = 0.0727). 2 has nearly D2h symmetry with two trans standing pyridine ligands lying in a plane. According to quantum chemical calculations, 2 (D2h symmetry) is more stable (48.28 kJ/mol) than 1 (C2v symmetry).
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230194
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  • 2
    Electronic Resource
    Electronic Resource
    Transition Metal Complexes with Sulfur Ligands, 123[Part 122: D. Sellmann, S. Emig, F. Heinemann, F. Knoch, Angew. Chem. submitted.[ Synthesis and Reactivity of New Complexes Containing the [Ru(“S4”)] Fragment [S42- = 1,2-Bis(2-mercaptophenylthio)ethane(2-)] (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 571-579 
    Details
    ISSN: 0009-2940
    Keywords: Labile ruthenium-sulfur complexes ; S2 Complexes ; Substitution reactions ; Ligand effects ; Structure-activity relationships ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to synthesize labile and well-soluble [Ru(L)(L')(“S4”)] complexes, [Ru(CI)2(DMSO)4] was treated With “S4”-Na2 (S42- = 1,2-bis(2-mercaptophenylthio)-ethane(2-1)] yielding [Ru(DMSO)2(“S4”)] (1 which contains two labile DMSO ligands. An X-ray structural analysis of 1, verifies that both DMSO ligands are coordinated via their S atoms. The reaction of 1 with small ligands such as PR3 (R = Et, nPr, nBu) or tetrahydrothiophene (THT) leads to substitution of both DMSO ligands yielding [Ru(PR3)2(“S4”)] (R = Et 3a, nPr 3b, nBu 3c) and [Ru(THT)2(“S4”] 2, respectively, while bulky phosphane ligands such as PCy3 and PiPr3 substitute one DMSO ligand to yield [Ru(DMSO)(PR3])(“S4”] (R = iPr 4a, Cy 4b). X-ray structural analyses of [Ru(PnPr3)2(“S4”)] · 0.5 MeOH (3b · 0.5 MeOH), [Ru(PnBu3)2(S4)} (3c), and [Ru(Pme3)2(“S4”)] (3d) confirm the pseudo-octahedral coordination of the Ru centers by four Sdonors and two cis P-donors and reveal close similarities bet ween the three complexes. Comparision of the structural parameters of 3b · 0.5 MeOH, 3c and 3d with those of [Ru(PPh3)2(“MeS, 4”)] [MeS4“2” = 1,2-bis(2-mercaptophenylthio)propane(2-1)] indicates that the inertness towards substitution of 3b · 0.5 MeOH, 3c and 3d as opposed to the substitution lability of [Ru(PPh3)2(,MeS4“)] is caused by the small cone angles of the alkyl phosphanes. In the DMSO/PCy3 complex 4b both coligands are labile, and which one is substituted depends on the size of the entering ligand. The reactions of 4b with PnR3 yield [Ru(DMSO)(PR3)('S4”)] (R = nPr 4c, nBu 4d) in contrast to the reaction with CO. PMe3, and SMe2 which give [Ru(CO)(Pcy3)(“S4”)] (5b), [Ru(P-Me3)(PCy3)(“S4”)] (6, and [Ru(SMe2)(PCy3)(“S4”)] (7, respectively. In an analogous manner, the CO complexes [Ru(CO(PR3)(“S4”)] (R = iPr 5a, nBu 5c) have been obtained by treatement of 4a and 4d with CO. The reactions of 4a and 4b with S8 yielded the readily soluble μ-S2 complexes [μ-S2[Ru(PR3)(“S4”)]2] (R - iPr 8a, Cy 8b). The spectroscopi9c data of complex 8b and its cyclic voltammogram, which exhibits four quasi-reversible redox waves, indicate a strong electronic coupling of the two [Ru(PCy3)(“S4”)] fragments via the μ-S2 bridge.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300507
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  • 3
    Electronic Resource
    Electronic Resource
    Chemie polyfunktioneller Moleküle, 125Part 124: Ref. Synthese und Kristallstruktur von N,N,N′,N“,N-Pentamethyl-diethylentriamin-cokoordiniertem Kalium-bis(diphenylphosphanyl)amidHerrn Prof. Dr. Gerhard Herberich zum 60. Geburtstage gewidmet. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 141-144 
    Details
    ISSN: 0009-2940
    Keywords: Alkali metal organophosphanylamide ; Carbon-potassium bonding ; Phosphazane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metalation of bis(diphenylphosphanyl)amine [HN-(PPh2)2,1 with KOtBu at 95°C in toluene affords a pale yellow precipitate of potassium bis(diphenylphosphanyl)amide (3a). On addition of liquid N,N,N′,N“,N“-pentamethyldiethylenetriamine (PMDTA, 4) the precipitate dissolves in toluene at 115°C to give a yellow solution, from which yellow-green blocks of [(Ph2P)2NK·PMDTA] (3b) are obtained. X-ray analysis reveals that the coordination sphere of potassium consists of the chelating triamine ligand and [N(PPh2)2]- as N-donor as well as η1 and η2 C-donor with two phenyl fragments. No phosphorus coordination of [N(PPh2)2]- is observed.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300124
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  • 4
    Electronic Resource
    Electronic Resource
    Untersuchungen zum elektronischen Einfluß von Organoliganden. XIII. Synthese und Charakterisierung von 2-funktionalisierten Vinylrhodoximen (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1946-1952 
    Details
    ISSN: 0044-2313
    Keywords: Vinyl rhodoximes, Organorhodoximes ; trans influence ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on the Electronic Influence of Organoligands. XIII. Synthesis and Characterization of 2-Functionalized Vinyl Rhodoximes2-Functionalized vinyl rhodoximes [Rh(dmgH)2 (PPh3)cis/trans-CH = CHZ] ([Rh]—CH = CHZ)) (1) can be prepared with a wide variation of the substituent Z (cis: OEt (1 a), OPh (1 b), Cl (1 c), Me (1 j), Ph (1 k), SMe (1 l), SPh (1 m); trans: SPh (1 d), Me (1 e), Ph (1 f), CMe3 (1 g), SiMe3 (1 h)) by oxidative addition of XCH = CHZ and/or by nucleophilic addition of HC≡CZ and Me3SiC≡CZ, respectively, to [Rh]-. 1 a is converted to [Rh]—CH2CHO (2) already in a weakly acid medium. 1 l is isomerized to trans-[Rh]—CH = CHSMe (1 n) in the presence of acids.The complexes 1 are characterized by microanalysis and by 1H, 13C and 31P NMR spectroscopy. The magnitude of the coupling constants 1J(103Rh, 31P) reveals only a small effect of Z on the (NMR) trans influence of the vinyl ligands CH = CHZ.The molecular structures of cis-[Rh]—CH = CHSPh (1 m) and trans-[Rh]—CH = CHSPh (1 d) show a distorted octahedral coordination of Rh with a mutual trans position of triphenyl-phosphine and the 2-phenylmercaptovinyl ligands. Van der Waals interactions exist between the sulfur and the equatorial dimethylglyoximato ligands in the cis complex 1 m.
    Notes: 2-Funktionalisierte Vinylrhodoxime [Rh(dmgH)2(PPh3)cis/trans-CH = CHZ] ([Rh]—CH = CHZ) Abkürzungen: [Rh] = [Rh(dmgH)2(PPh3)]; dmgH2 = Dimethylglyoxim; X = Cl, Br; Z = Substituent (Alkyl, Aryl, heteroatomfunktionalisierte Gruppe wie OR, SR, …)(1) sind bei breiter Variation des Substituenten Z (cis; OEt (1 a), OPh (1 b), Cl (1 c), Me (1 j), Ph (1 k), SMe (1 l), SPh (1 m); trans: SPh (1 d), Me (1 e), Ph (1 f), CMe3 (1 g), SiMe3 (1 h)) durch oxidative Addition von XCH = CHZ und/oder durch nucleophile Addition von HC≡CZ bzw. Me3SiC—CZ an [Rh]- zugänglich. 1 a unterliegt bereits im schwach sauren Medium einer Umwandlung zu [Rh]—CH2CHO (2). 1 l wird sauer katalysiert zu trans-[Rh]—CH = CHSMe (1 n) isomerisiert.Die Komplexe 1 sind durch Elementaranalyse sowie 1H-, 13C- und 31P-NMR-spektroskopisch charakterisiert. Die Größe der Kopplungskonstanten 1J(103Rh, 31P) läßt nur einen geringen Einfluß von Z auf den (NMR) trans-Einfluß des Vinylliganden CH = CHZ erkennen.Die Molekülstrukturen von cis-[Rh]—CH = CHSPh (1 m) und trans-[Rh]—CH = CHSPh (1 d) zeigen eine verzerrt oktaedrische Koordination von Rh mit einer gegenseitigen trans-Stellung von Triphenylphosphin und dem 2-Phenylmercaptovinyl-liganden. In der cis-Verbindung 1 m bestehen van der Waals Kontakte zwischen dem Schwefel und den äquatorialen Dimethylglyoximatoliganden.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966221122
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  • 5
    Electronic Resource
    Electronic Resource
    Synthese und Struktur der Kronenetherkomplexe von Kaliumhexachlorodipalladat(II) und -diplatinat(II) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1651-1656 
    Details
    ISSN: 0044-2313
    Keywords: Palladium Complexes ; Platinum Complexes ; Crown Ether Complexes ; Hexachlorodipalladate(II) ; Hexachlorodiplatinate(II) ; X-ray Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Crown Ether Complexes of Potassium Hexachlorodipalladate(II) and -diplatinate(II)K2[MCl4] (M = Pd, Pt) reacts with an excess of crown ether 18-crown-6 in water to give the crown ether complexes of potassium hexachlorodipalladate(II) and -diplatinate(II) [K(18-cr-6)]2[M2Cl6] (M = Pd, 1; M = Pt, 3), respectively, and in methylene chloride to give those of potassium tetrachloropalladate(II) and -platinate(II) [K(18-cr-6)]2[MCl4] (1) (M = Pd, 2; M = Pt, 4), respectively. 1-4 are characterized by microanalysis, NMR (1H, 13C), and vibrational spectroscopy. The X-ray structure analyses of the isotypic complexes 1 (P21/c; a = 10,9678(8), b = 8,2991(7), c = 22,469(2) Å, β = 98,523(5)°; Z = 2) and 3 (P21/c; a = 10,934(3), b = 8.376(3), c = 22,410(5) Å, β = 98,77(3)°; Z = 2) reveal [M2Cl6]2- anions of nearly D2h symmetry and [K(18-cr-6)]+ cations, in which the distance of K+ to the mean plane of the crown ether defined by its six oxygen atoms amounts to 0,830(4) Å in 1 and 0,821(2) Å in 3, respectively. There are tight contacts between cations and anions (d(K-Cl): 3,341(2)/3,260(2) Å (1); 3,348(4)/3,259(4) Å (3)).
    Notes: K2[MCl4] (M = Pd, Pt) reagiert mit überschüssigem Kronenether 18-Krone-6 in Wasser zu den Kronenetherkomplexen von Kaliumhexachlorodipalladat(II) bzw. -diplatinat(II) [K(18-cr-6)]2[M2Cl6] (M = Pd, 1; M = Pt, 3) und in Methylenchlorid zu denen von Kaliumtetrachloropalladat(II) bzw. -platinat(II) [K(18-cr-6)]2[MCl4] (M = Pd, 2; M = Pt, 4). 1-4 sind durch Elementaranalyse sowie NMR-(1H, 13C) und schwingungsspektroskopisch charakterisiert. Die Röntgeneinkristallstrukturanalysen der beiden isotypen Komplexe 1 (P21/c; a = 10,9678(8), b = 8,2991(7), c = 22,469(2) Å, β = 98,523(5)°; Z = 2) und 3 (P21/c; a = 10,934(3), b = 8,376(3), c = 22,410(5) Å, β = 98,77(3)°; Z = 2) zeigen [M2Cl6]2--Anionen von nahezu D2h-Symmetrie und [K(18-cr-6)]+-Kationen, in denen K+ in 1 um 0,830(1) Å bzw. in 3 um 0,821(2) Å aus der durch die sechs Sauerstoffatome des Kronenethers definierten Ebene ausgelenkt ist. Zwischen Kationen und Anionen bestehen enge Kontakte (d(K—Cl): 3,341(2)/3,260(2) Å (1); 3,348(4)/3,259(4) Å (3)).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976231028
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