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  • 1
    Electronic Resource
    Electronic Resource
    Diastereoselective Synthesis and Molecular Structure of a Bicyclic and a Cage Phosphane (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1547-1550 
    Details
    ISSN: 0009-2940
    Keywords: Phosphane ; 1,3α., 5,7β-Tetrakis(trifluoromethyl)-6,-9-dioxa-2-phosphabicyclo[3.3.1]nonane-3β, 7α-diol ; 1,7-Trifluoromethyl-3,5-methyl1-2,4.8-trioxa-6-phosphaadamantane ; Phosphorus heterocycles ; Ketones ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A two-step formal insertion of 1,1,1,5,5,5-hexafluoro- (2a) and 1,111-trifluoropentane-2,4-dione (2b) into the P-H bonds of phosphane gave the primary a-hydroxyphosphanes 3 and 4, precursors for the resulting secondary phosphanes, 6,9-dioxa-2-phosphabicyclo[3.3.l]nonane (6a) and 2,4,8-trioxa-6-phosphaadamantane (7), both formed diastereospecifically. The molecular structures of 6a and 7 were established by single-crystal X-ray structure analysis which revealed two independent molecules for 6a in the unit cell possessing a chair-boat conformation with a C-P-C angle of 95.4(2)°, and a characteristic heteroadamantane geometry for 7, with the corresponding angle being smaller by 4.9°.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301031
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  • 2
    Electronic Resource
    Electronic Resource
    Preparation of Methyl 2-[Bis(trimethylsiloxy)phosphoryl]-3,3,3-trifluoro-2- (trimethylsiloxy)propionate and Some Derivatives-Molecular Structure of Methyl 2-[Bis(trimethylsiloxy)phosphoryl]-3,3,3-trifluoro-2-hydroxypropionate (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 279-281 
    Details
    ISSN: 0009-2940
    Keywords: Methyl trifluoropyruvate ; Tris(trimethylsilyl) phosphite ; Methyl 2-[bis(trimethylsiloxy)phosphoryl]-3,3,3- trifluoro-2-(trimethylsiloxy)propionate ; Bis(trimethylsilyl) [(2,2-difluoro-l-trimethylsiloxy)ethenyl]- phosphonate ; Solid-state structures ; Fluorine ; Phosphorus ; Silicon ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methyl trifluoropyruvate (1) and tris(trimethylsilyl) phosphite (3) reacted to give methyl 2-[bis(trimethylsiloxy)phosphoryl]- 3,3,3-trifluoro-2-(trimethylsiloxy) propionate (4). Partial hydrolysis furnished propionate 6, the molecular structure of which was obtained in the solid state. Attempted trimethylsilylation of the methylcarboxylato group in 4 using iodotrimethylsilane caused the formation of bis(trimethylsily1) [(2,2- difluoro- 1 -trimethylsiloxy)ethenyl]phosphonate (8). For comparison, methyl pyruvate (2) and 3 gave methyl 2-[bis(trimethylsiloxy)phosphoryl]-2-(trimethylsiloxy)propionate (5).
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300222
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  • 3
    Electronic Resource
    Electronic Resource
    N-Alkylation of Ammine - Undecahydro-Closo-dodecaborate(1-)Dedicate to Prof. Dr. Walter Siebert on the occasion of hbis 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 795-799 
    Details
    ISSN: 0009-2940
    Keywords: Boron ; Alkylations ; N ligands ; Dodecaborate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of the ammine-undecahydro-closo-dodecaborate(1-) anion with alkyl halides have been studied in detail. The degree of alkylation of the nitrogen was found to be dependent upon the steric demands of the alkyl groups. The derivatives were characterized by NMR and infrared spectroscopy. Four compounds were crystallized for single crystal X-ray diffraction studies. The tetrahedral coordination of the nitrogen atom of the bis-alkylated derivatives was found to deviate towards planarity with increasing steric hindrance of the substitutents. - The syntheses, crystal structures, and spectral properties of four N-alkyl derivatives of [H3N—B12H11]-, ammine - undecahydro-closo-dodecaborate(1-) (3), are reported. Alkylation of 3 with ethyl iodide was achieved in dimethyl sulfoxide using potassium hydroxide as base. This led to orthorhombic crystals of [N(nC4H94][(CH3CH2)3N—B12H11] (4). The reaction of 3 with benzyl chloride resulted in the bisbenzylated product, isolated as triclinic crystals of [PPN][(C6H5CH2)2 NH—B12H11] (5). The alkylation of 3 with 2-bromopropane gave a mixture of the mono- and bisalkylated products. The monoalkylated derivative [PPN][(CH3)2CH)NH2-12H11] (6, crystallized in the triclinic space group p1) and the bisalkylated product [PPN]{[(CH3)2NH—B12H11) (7, monoclinic, P21./c) were separated on the basis of their different water solubilities. The solid-state structures of the compounds 4-7 revealed a slight distortion of the B12 icosahedron. The length of the B(1)-N(1) bond was found to be dependent on the steric requirements of the attached amine, e.g. primary amine 〈 secondary amine 〈 tertiary amine. This is demonstrated by the variation in the B—N bond length; from 157.8(2) pm for 6, 158.5(5) pjm for 5, 160.0(3) pm for 7, to 163.7(6) pm for 4.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300619
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  • 4
    Electronic Resource
    Electronic Resource
    Organoantimony Oxides: Preparation and Crystal Structures of [(2-PhOC6H4)O (C6H4)2Sb]2O2 and (o-Tol2Sb)4O6Dedicated to Prof. Dr. Gottfried Huttner on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 959-961 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Air oxidation of (Oxydi-2,1-phenylene)(2-phenoxyphenyl)stibane (1) gives the phenoxystibane oxide [(2-PhOC6H4)O(C6H4)2Sb]2O2 (2). Single crystals of (o-Tol2Sb)4- O4(O2)2 (3) were obtained by air oxidation of o-TolSb-(SiMe3)2. Crystal structures of 2 and 3 are reported.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300724
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  • 5
    Electronic Resource
    Electronic Resource
    Rheniumpentacarbonylthiazylhalogenid-Komplexe [Re(CO)5(NSX)]AsF6: Strukturen und BindungsverhältnisseProfessor Max Herberhold zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 444-448 
    Details
    ISSN: 0044-2313
    Keywords: Thiazylhalides ; Thiazyl Complexes ; Rheniumpentacarbonyl Complexes ; X-ray Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Rheniumpentacarbonylthiazylhalide Complexes [Re(CO)5(NSX)]AsF6: Structures and Bonding PropertiesThe structures of [Re(CO)5(NSX)]AsF6 (X = F (1),Cl (3 a), and Br (3 b)) were determined by X-ray crystallography. From the ReN and ReC bond distances π-acceptor properties for the thiazylhalide ligands are derived.
    Notes: Die Strukturen von [Re(CO)5(NSX)]AsF6 (X = F (1), Cl (3a) und Br (3b)) wurden durch Röntgenstrukturanalyse bestimmt. Aus den ermittelten ReN- bzw. ReC-Bindungslängen wird π-Akzeptor-Verhalten für die Thiazylhalogenidliganden abgeleitet.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230171
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  • 6
    Electronic Resource
    Electronic Resource
    NSF3 und NSF2NMe2 als Liganden in der metallorganischen ChemieProfessor Gottfried Huttner zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1518-1524 
    Details
    ISSN: 0044-2313
    Keywords: Thiazyltrifluoride ; Thiazyldifluoridedimethylamide ; metal complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thiazyltrifluoride NSF3 and Thiazyldifluoridedimethylamide NSF2NMe2: Ligands in Organometallic ChemistryFrom the reaction of [Re(CO)5SO2]+AsF6- (1) and [CpFe(CO)2SO2]+AsF6- (6) with NSF3 (2) and NSF2NMe2 (4) the complexes [Re(CO)5NSF3]+AsF6- (3), [Re(CO)5NSF2NMe2]+AsF6- (5), [CpFe(CO)2NSF3]+AsF6- (7), and [CpFe(CO)2NSF2NMe2]+AsF6- (8) were obtained. The compounds have been characterised by X-ray crystallography, the ligand properties of 2 and 4 are discussed.
    Notes: Durch Umsetzung von [Re(CO)5SO2]+AsF6- (1) und [CpFe(CO)2SO2]+AsF6- (6) mit NSF3 (2) und NSF2NMe2 (4), wurden die Komplexe [Re(CO)5NSF3]+AsF6- (3), [Re(CO)5NSF2NMe2]+AsF6- (5), [CpFe(CO)2NSF3]+AsF6- (7) und [CpFe(CO)2NSF2NMe2]+AsF6- (8) dargestellt und durch Kristallstrukturanalysen charakterisiert. Die Ligandeneigenschaften von 2 und 4 werden diskutiert.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976231008
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  • 7
    Electronic Resource
    Electronic Resource
    Pentafluorethylschwefeltrifluorid: Synthese und ReaktionenProfessor Anton Meller zum 65. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1892-1896 
    Details
    ISSN: 0044-2313
    Keywords: Fluorinations ; Perfluoroalkylsulfurfluorides ; Perfluoroalkylsulfonium Salts ; X-Ray Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Pentafluorethyl Sulfurtrifluoride: Synthesis and ReactionsBy oxidation of (C2F5S-)2 (1) with AgF2 at 0°C a mixture of C2F5SF3 (2) and C2F5SF5 (3) besides C2F5S(O)F (4) is formed. With elemental fluorine only 3 is isolated, an intermediate in this reaction is (C2F5SF4-)2 (5). At -40 to -30°C the mixture of 2, 3 and 4 was reacted with TASF and AsF5, to give TAS+ C2F5SF4- (6), TAS+ C2F5S(O)F2- (7) and C2F5SF2+AsF6- (8), respectively. While 6 and 7 decompose rapidly in solution even at low temperatures, of thermally stable 8 the solid state structure was determined by x-ray diffraction.
    Notes: Durch Oxidation von (C2F5S-)2 (1) mit AgF2 bei 0°C entsteht ein Gemisch aus C2F5SF3 (2) und C2F5SF5 (3) daneben bildet sich C2F5S(O)F (4); mit elementarem Fluor wird nur 3 isoliert, ein Zwischenprodukt bei dieser Reaktion ist (C2F5SF4-)2 (5). Das Gemisch aus 2, 3 und 4 wurde bei T=-40 bis -30°C mit TASF bzw. AsF5 umgesetzt, mit TASF reagieren 2 und 4, mit AsF5 bildet lediglich 2 ein isolierbares Salz. Während sich TAS+ C2F5SF4- (6) und TAS+ C2F5S(O)F2- (7) bei tiefen Temperaturen in Lösung rasch zersetzen, konnte von dem thermisch stabilen C2F5SF2+AsF6- (8) eine Röntgenstrukturanalyse angefertigt werden.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976231212
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