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  • Rhenium complexes  (4)
  • Transition metals  (3)
  • 1
    Electronic Resource
    Electronic Resource
    Wasserlösliche Metallkomplexe und Katalysatoren, IV. 2,2′-Bipyridin-5-sulfonsäure: Synthese, Reinigung, Derivate und Metallkomplexe (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 1953-1961 
    Details
    ISSN: 0009-2940
    Keywords: Transition metals ; Water-soluble organometallic compounds ; Chelating sulfonated ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Water-Soluble Metal Complexes and Catalysts, IV.  -  2,2′-Bipyridine-5-sulfonic Acid Synthesis, Purification, Derivatives and Metal ComplexesThe synthesis of 2,2′-bipyridine-5-sulfonic acid (1a) is achieved by mercury(II)-catalyzed sulfonation of 2,2′-bipyridine in oleum (30% SO3) in 10-50-g amounts. The crude product is purified by extraction of 1a as tetra(n-butyl)ammonium salt into dichloromethane and re-extraction of the free acid with conc, hydrobromic acid. Melting of 1a together with potassium hydroxide gives 5-hydroxy-2,2′-bipyridine (2). The salts 1b-d (Na+, [N(n-C4H9)4]+, [P(C6H5)4]+) and sulfonamides 1f-h (tert-butyl, benzyl, 2-pyridylmethyl) of the acid 1a are ligands of different solubility. The coordination chemistry of these N,N-chelating ligands is studied. The compounds 4-14 of chromium, molybdenum, tungsten, manganese, rhenium, and osmium containing carbonyl or oxo ligands are prepared as examples of chelate complexes with metals in low and high oxidation states. The solubility of the complexes is mostly determined by the cations: sodium salts are usually soluble in water and/or in short-chained alcohols. Tetra-n-butylammonium and tetraphenylphosphonium salts and the sulfonamides are soluble in polar organic solvents. On the other hand, the distribution of charge has an influence on solubility. Increased polarity of the anion, caused by high oxidation states of the metals, decreases the solubility of the complex in organic solvents.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901231005
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  • 2
    Electronic Resource
    Electronic Resource
    Wasserlösliche Metallkomplexe und Katalysatoren, V. 2,2′-Bipyridin-5-sulfonsäure und metallorganische Komplexe: Spektroskopie und Strukturchemie (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 1963-1970 
    Details
    ISSN: 0009-2940
    Keywords: Transition metals ; Chelating sulfonated ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Water-Soluble Metal Complexes and Catalysts, V.  -  2,2′-Bipyridine-5-sulfonic Acid and Organometallic Complexes: Spectroscopy and StructuresCoplanar orientation of the pyridine rings in 2,2′-bipyridine-5-sulfonic acid (1a) and in metal complexes of this ligand is evident from NMR studies. While the free acid 1a exists as a planar zwitter-ion the rings of the salts 1b-d (Na+, [N(C4H9)4]+,[P(C6H5)4)]+) and sulfonamides 1f-h (tert-butyl, benzyl, 2-pyridylmethyl) are twisted. X-ray crystal structures determined for four complexes 4e, h, 1, and 10b of the sulfonic acid and sulfonamide derivatives of 2,2′-bipyridine show that there is no influence of the sulfonic acid and the sulfonamide groups (meta-position) on the complex chemistry of the chelate ligand. Variation of solubility should, therefore, occur without principal changes of reactivity.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901231006
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  • 3
    Electronic Resource
    Electronic Resource
    α-CH-Acidität von Allyliden-Komplexen: Rheniumorganische Derivate des 1,2,3-Butatriens durch Dehydrochlorierung von Rhena(V)-allylidenen. Synthese und Strukturchemie (1989)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 2035-2040 
    Details
    ISSN: 0009-2940
    Keywords: CH Acidity ; Rhenium complexes ; Allylidene ; Butatriene ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: α-CH Acidity of Allylidene Complexes: Organorhenium Derivatives of 1,2,3-Butatriene by Dehydrochlorination of Rhena(V) Allylidenes. Synthesis and StructureThe rhena(V) allylidene complex (η5-C5Me5)ReCl2 [η1:η3-(CH3)-CC(Cl)CH2] (2) is quantitatively converted into the novel organorhenium 1,2,3-butatriene derivative (η5-C5Me5)ReCl2[η3-H2CC(C5H5N)CCH2] (3) by lithium hydroxide in the presence of excess pyridine. This result shows so far not investigated CH acidity of methyl groups, that are substituting π-bonded allylidene frameworks at the α-position. According to an X-ray structure analysis, the coordination geometry of the 1,2,3-butatriene ligand is very similar to related allyl complexes of the (η5-C5Me5)ReCl2 fragment.
    Notes: Der Rhena(V)-allyliden-Komplex (η5-C5Me5)ReCl2 [η1:η3-(CH3)-CC(Cl)CH2] (2) wird durch Lithiumhydroxid in Gegenwart von überschüssigem Pyridin quantitativ zu dem neuartigen rhenium-organischen 1,2,3-Butatrien-Derivat (η5-C5Me5)ReCl2[η3-H2CC(C5H5N)CCH2] (3) dehydrohalogeniert. Dieses Ergebnis weist auf die bisher nicht beachtete CH-Acidität von Methylgruppen hin, die ein π-gebundenes Allyliden-Gerüst α-ständig substituieren. Einer Röntgenstrukturanalyse zufolge ist der von 1,2,3-Butatrien abgeleitete Ligand allylartig an das (η5-C5Me5)ReCl2-Fragment gebunden.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19891221102
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  • 4
    Electronic Resource
    Electronic Resource
    Metallcarbonyl-Synthesen, XXI. Einfache Synthese eines präparativ nützlichen Alkoxy(carbonyl)metallats (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 1795-1799 
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    ISSN: 0009-2940
    Keywords: Carbonyl complexes ; Rhenium complexes ; Alkoxy carbene, structure of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Carbonyl Syntheses, XXI. - Straightforward Synthesis of a Synthetically Useful Alkoxy(carbonyl)metallateAnionic methoxy complexes are formed upon carbonylation of ammonium perrhenate in methanol at 230-240°C. Thus, the dinuclear ionic complex [N(CH3)4][Re2(CO)6(μ-OCH3)3] (2) results in 80% yield at CO pressures of ca. 100 bar, while the trinuclear derivative [N(CH3)4][Re3(CO)9(μ3-OCH3)3(μ3-OCH3)] (3) is due to lower pressure conditions (ca. 50 bar); 2 yields the bis(carbene) complex 4 of formula fac-Re(CO)3L2I upon treatment with a bis(imidazolium) iodide, thus demonstrating that carbonylrhenium chemistry not necessarily depends on the availability of Re2(CO)10.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250803
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  • 5
    Electronic Resource
    Electronic Resource
    Mehrfachbindungen zwischen Hauptgruppenelementen und Übergangsmetallen, LXXXII. Zweikernige μ-Benzylidin-Komplexe mit Doppelbindung zwischen Rheniumatomen (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 1971-1974 
    Details
    ISSN: 0009-2940
    Keywords: Alkylidyne ligands ; Rhenium complexes ; Metal-metal multiple bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Multiple Bonds Between Main-Group Elements and Transition Metals, LXXXII.  -  Dinuclear p-Benzylidyne Complexes Having a Double Bond between Rhenium AtomsThe dialkylrhenium(V) complex (η5-C5Me5)Re(=O)(CH2Ph)2 (3) reacts with the organotitanium reagents (η5-C5H5)TiX3 (X = Cl, Br) to yield the dinuclear rhenium(IV) complexes (η5C5Me5)2 Re2X3(CC6H5) (4a, b). According to a single-crystal X-ray diffraction analysis, 4a′ (C5Me4Et in place of C5Me5) represents one of the few known examples of μ-alkylidyne complexes that have metal-to-metal multiple bonds. The molecule of C2 symmetry has a planar four-membered Re,Cl,Re′,C-ring geometry and two trans-oriented sets of ligands. Very small angles at the bridging chloro ligand and alkylidyne carbon atom result from the short metal-metal distance (double bond).
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901231007
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  • 6
    Electronic Resource
    Electronic Resource
    Metallcarbonyl-Synthesen. 2322. Mitteilung: Siehe Lit. [1]. Kristallstruktur und Reaktionsverhalten von Carbonylmetall-Komplexen des Heptamethylindens (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1229-1236 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium complexes ; carbonyl complexes ; nitrosyl complexes ; heptamethylindene ; crystal structures ; σ/η-bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses of Metal Carbonyls. 23. Crystal Structure and Reactivity of Heptamethylindenyl Carbonyl Metal ComplexesReaction of heptamethylindene (C9(CH3)7, 1) with Re2(CO)10 yields [η5-C9(CH3)7]Re(CO)3 (2), which reacts with NO+BF4- to form the cationic complex [{η5-C9(CH3)7}Re(CO)2NO]+BF4- (3). Irradiation of 2 with UV light in the presence of triethyl phosphite leads to formation of [η5-C9(CH3)7]Re(CO)2[P(OC2H5)3] (4). Alkylation of (CH3)3SnCl with Ind*Li gives [η1-C9(CH3)7]Sn(CH3)3 (5). All compounds were characterized by spectroscopic methods. The molecular structures of 3 and 5 were determined by single crystal X-ray diffraction (3: P21/n (14), a = 1497.7(4) pm, b = 879.0(2) pm, c = 1609.0(4) pm and β = 110.99(2)°, R1 = 0.038, wR2 = 0.080; 5: P21/n (14), a = 726.1(1) pm, b = 2930.7(3) pm, c = 930.0(1) pm and β = 112.834(5)°, R1 = 0.044, Rw = 0.048). Complexes 2-4 exhibit a piano stool configuration with a η5-coordinated permethylindenyl ligand (Ind*). Compound 5 displays a η1 -coordination of the Ind* ligand. Temperature enhancement causes a hapticity change, as observed by NMR spectroscopy.
    Notes: Heptamethylinden (C9(CH3)7H, 1) reagiert mit Re2(CO)10 zu [η5-C9(CH3)7]Re(CO)3 (2), das durch Umsetzung mit NO+BF4- die kationische Verbindung[{η5-C9(CH3)7}Re (CO)2NO]+BF4- (3) und unter Bestrahlung mit UV-Licht in Anwesenheit von Triethylphosphit [η5-C9(CH3)7]Re(CO)2[P(OC2H5)3] (4) ergibt. Durch Alkylierung von (CH3)3SnCl wird [η1-C9(CH3)7]Sn(CH3)3 (5) erhalten. Alle Verbindungen wurden mit spektroskopischen Methoden vollständig charakterisiert. Von 3 und 5 wurden die Kristallstrukturen röntgenstrukturanalytisch bestimmt (3: P21/n (14), a = 1497.7(4) pm, b = 879.0(2) pm, c = 1609.0(4) pm und β = 110.99(2)°, R1 = 0.038, wR2 = 0.080; 5: P21/n (14), a = 726.1(1) pm, b = 2930.7(3) pm, c = 930.0(1) pm und β = 112.834(5)°, R1 = 0.044, Rw = 0.048). Während bei den Komplexen 2-4 der Heptamethylindenligand (Ind*) einen Halbsandwich-Komplex bildet (η5-Bindung zum Metall), so liegt in Derivat 5 erwartungsgemäß eine σ-Bindung zwischen einem C-Atom des Ind*-Liganden und dem Metallzentrum vor. Bei Temperaturerhöhung tritt eine Änderung der Haptizitätsverhältnisse ein (NMR-Evidenz).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230808
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  • 7
    Electronic Resource
    Electronic Resource
    Multiple Bonds between Transition Metals and “Bare” Main Group Elements: Links between Inorganic Solid State Chemistry and Organometallic ChemistryIn memoriam Professor Wilhelm Klemm (1986)
    Weinheim : Wiley-Blackwell
    Angewandte Chemie International Edition in English 25 (1986), S. 56-76 
    Details
    ISSN: 0570-0833
    Keywords: Transition metals ; “Bare” main group elements ; Main group elements ; Solid-state reactions ; Organometallic compounds ; Cluster compounds ; Metal-metal interactions ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The last two decades have seen a dramatic development in the study of metal-metal multiple bonds, particular successes being recorded in the field of organometallic chemistry. Syntheses designed to produce novel transition metal complexes with single, double, triple and quadruple metal-metal bonds occupy a most important place in such research, as also do reactivity studies. A striving to establish general principles has provided much of the motivation for such work, but one less obvious goal - the commercial application of the catalytic properties of metal-metal multiple bonding systems, in the medium and long term - should not be overlooked. All aspects of the investigations of metal-metal multiple bonds also apply to a particular class of compound that has, however, enjoyed little lime-light and thus deserves the present review: complexes with multiple bonds between transition metals and substituent-free (“bare”) main group elements. Although based mostly on accidental discoveries, the few noteworthy examples are now beginning to unfold general concepts of synthesis that are capable of being extended and thus are deserving of exploitation in preparative chemistry. The availability of further structural patterns exhibiting multiple bonds between transition metals and ligand-free main group elements might enable preparative organometallic chemistry to expand in a completely new direction (for instance by the stabilizing or activation of small molecules at the metal complex). This essay discusses the chemistry of complexes of bare carbon, nitrogen, and oxygen ligands (carbido-, nitrido-, and oxo-complexes) and their relationships to higher homologues from both a synthetic and a structural point of view.
    Additional Material: 37 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/anie.198600561
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