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  • Boron  (4)
  • Chromium complexes  (2)
  • Transition Metal Complexes  (2)
  • 1
    ISSN: 0009-2940
    Keywords: Boron ; Diazaboroles ; Carbenes ; Heterocycles ; Imidazoles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2-Bromo-2,3-dihydro-1H-1,3,2-diazaboroles (3a-c) were synthesized by cyclocondensation of dilithiated 1,4-diazabutadienes (5a-c) with boron tribromide in hexane. 3a was also obtained by sodium amalgam reduction was conducted in ether solvents, diboroxane (2) resulted as the main product. Compound 3a and 1,3-dialkyl-4,5-dimethylimidazol2-ylidenes (6a, b) underwent halide displacement to afford the borolylimidazolium salts 7a, b. Compounds 2, 3a-c, and 7a, b were characterized by elemental analyses and spectroscopic methods (1H, 11B, 13C NMR; Ir; MS). The molecular structures of 2 and 7a were established by single-crystal X-ray diffraction analyses.
    Additional Material: 2 Ill.
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  • 2
    ISSN: 0009-2940
    Keywords: Diphosphapropenes ; CH insertion ; Diphosphiranes ; Chromium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Rearrangements of the Metallodiphosphapropenes (η5-C5Me5)(CO)2FeP(SiMe3  -  P = C(R)(SiMe3) (R = SiMe3, Ph)Heating of a methylcyclohexane solution of (η5-C5Me5)-(CO)2FeP(SiMe3)  -  P = C(SiMe3)2 (1a) gives rise to the insertion of the P = C moiety into the CH bond of a ring methyl group with formation of the chelate complex η5-ηC5Me4CH2P-[CH(SiMe3)2]P(SiMe3)Fe(CO)2 (2) which is converted into the pentacarbonylchromium derivative [5-C5Me4CH2P[CH-(SiMe3)2]P(SiMe3)[Cr(CO)5]Fe(CO)2] (3). In contrast, a similar treatment of (5-C5Me5)(CO)2FeP(SiMe3)  -  P = C(Ph)(SiMe3) (1 b) furnishes the diphosphirane (5-C5Me5)(CO)2FeP  -  C(Ph)-SiMe3)  -  P (SiMe3) (5). By chromatography of its (CO)5Cr adduct 6, the P  -  Si bond is hydrolyzed to give the (diphosphirane)-chromium complex [(5-C5Me5)(CO)2FeP-C(Ph)(SiMe3)P(H)]-Cr(CO)5 (8). The molecular structures of 3 and 8 are determined by single-crystal X-ray analysis.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 1553-1557 
    ISSN: 0009-2940
    Keywords: Phosphido complexes ; Phosphaalkenes ; Diphosphiranes ; Chromium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition-Metal-Substituted Diphosphenes, XXVII[1]. - Synthesis and Structure of the Diphosphirane (η5-C5Me5)(CO)2Fe-PH[Cr(CO)5(η5-C5Me5)(CO)2FePH2 (5), prepared from (η5-C5Me5)(CO)2Fe-P(SiMe3)2 and ethanol, reacts with one equivalent of ClP = C(SiMe3)2 to give the diphosphirane (η5-C5Me5)(CO)2FePH (8). Compound 8 is converted into the iron chromium complex [(η5-C5Me5)(CO)2Fe-H]Cr(CO)5(9). In contrast, the reaction of 5 with two equivalents of ClP=C(SiMe3)2 results in the formation of the cyclotri-phosphane [(η5-C5Me5)(CO)2Fe-[CH(SiMe3)2] (12). The molecular structure of 9 is elucidated by single-crystal X-ray analysis.
    Additional Material: 2 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 1145-1152 
    ISSN: 1434-1948
    Keywords: Boron ; Diazaboroles ; Halogens ; Isocyanides ; Heterocycles ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of differently substituted 2-chloro-, 2-fluoro- and 2-iodo-2,3-dihydro-1H-1,3,2-diazaboroles have been prepared by various methods. 1,3-Di-tert-butyl-2-fluoro-2,3-dihydro-1H-1,3,2-diazaborole (3a), 1,3-di-tert-butyl-2-chloro-2,3-dihydro-1H-1,3,2-diazaborole (5a), 1,3-bis(2,6-dimethyl-phenyl)-2-chloro-2,3-dihydro-1H-1,3,2-diazaborole (5b), 2-chloro-4,5-dimethyl-1,3-dineopentyl-2,3-dihydro-1H-1,3,2-diazaborole (5c), and 1,3-di-tert-butyl-2-iodo-2,3-dihydro-1H-1,3,2-diazaborole (6a) were formed from the corresponding lithiated Z-1,2-diaminoethenes, by treatment with BF3·OEt2, BCl3, or BI3 in n-hexane. Compounds 3a, 5a, and 5b are also available by sodium amalgam reduction of the adduct (tBu)(BF3)N=CH-CH=N(BF3)(tBu) (2a), and the borolium salts [RNa=CH-CH=Nb(R)BCl2]X (Na-B) (4a: R = tBu, X = BCl4 and 4b: R = 2,6-Me2C6H2, X = Cl) respectively. The iodo derivative (2,6-Me2C6H2)-Na-CH=CH-Nb(2,6-Me2C6H2)BI (Na-B) (6b) was synthesized in a redox reaction between the 1,4-diazabutadiene 1b and BI3. The novel compounds were characterized by 1H-, 11B- and 13C-NMR spectroscopy, as well as by an X-ray structure analysis of 6b.Supporting information for this article is available on the WWW under http://www.wiley-vch.de/contents/jc_2005/1998/98047_s.pdf or from the author.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 491-497 
    ISSN: 1434-1948
    Keywords: Boron ; Diazaboroles ; Hydrides ; Tin ; Heterocycles ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,3-Di-tert-butyl-2,3-dihydro-1H-1,3,2-diazaborole (4a) and 1,3-bis(2,6-dimethylphenyl)-2,3-dihydro-1H-1,3,2-diazaborole (4b) were formed by the reaction of the corresponding 2-bromo or 2-iodo derivatives 1a and 2b with LiAlH4. Treatment of 1a with n-butyllithium afforded 2-n-butyl-1,3-di-tert-butyl-2,3-dihydro-1H-1,3,2-diazaborole (5a), whereas 1,3-di-tert-butyl-2-cyano-2,3-dihydro-1H-1,3,2-diazaborole (3a) was converted into the 2-tert-butyl derivative 6a or the 2-ethynyl-1,3,2-diazaborole 7a by means of tert-butyllithium or by the ethylenediamine adduct of lithium acetylide. Similarly, 1,3-di-tert-butyl-2-trimethylstannyl-2,3-dihydro-1H-1,3,2-diazaborole (8a) and 1,3-bis(2,6-dimethylphenyl)-2-trimethylstannyl-2,3-dihydro-1H-1,3,2-diazaborole (8b) were accessible from 1a or 2b and trimethylstannyllithium. In the complex 9a the compound 3a serves as an η1 ligand towards the [Cr(CO)5] unit via the cyano group. These novel compounds were characterized by 1H-, 11B-, 13C-, and 119Sn-NMR spectroscopy, as well as by X-ray structure analyses of 4b, 8a, and 9a.
    Additional Material: 3 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 1193-1198 
    ISSN: 1434-1948
    Keywords: Boron ; Triazaboroles ; Heterocycles ; Halogens ; Cyanides ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 3,4-Dihydro-2,4-diphenyl-2H-1,2,4,3-triazaboroles 3a, 3b, and 4 were synthesized by cyclocondensation of N1,N3-diphenylformamidrazone (1) with dibromophenylborane, dibromomethylborane, and boron trichloride. 3-Chloro-3,4-dihydro-2,4-diphenyl-2H-1,2,4,3-triazaborole (4) was converted into 3,4-dihydro-2,4-diphenyl-2H-1,2,4,3-triazaborole (5) by treatment with LiAlH4. The corresponding 3-cyanato and 3-cyano derivatives 6 and 7 resulted from the reaction of 4 with AgOCN and AgCN, respectively. Compound 7 was transformed into the bis(1,2,4,3-triazaborolyl)oxane 8 by silver oxide. Compounds 1-8 were characterized by elemental analyses and spectroscopic methods (1H, 11B, and 13C NMR; IR; MS). The molecular structure of 8 was established by single-crystal X-ray diffraction analysis.
    Additional Material: 2 Ill.
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  • 7
    ISSN: 0044-2313
    Keywords: Metallophosphaalkenes ; Transition Metal Complexes ; X-Ray Structure Analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition-Metal Substituted Phosphaalkenes and Acyl Phosphanes. 31 [1] Reactivity of (η5-C5Me5)(CO)2FeP = C(NMe2)2 towards Tin Dichloride. X-Ray Structure Analysis of {(η5-C5Me5)[η1-(Me2N)2C = P—P = C(NMe2)2](CO)2Fe}+{[Me2N)2C]2P}+(FeCl4)2-Reaction of metallophosphaalkene (η5-C5Me5)(CO)2 · FeP = C(NMe2)2 (1) with anhydrous tin dichloride affords the salt-like compound {(η5-C5Me5)[η1-(Me2N)2C = P—P = C(NMe2)2] · (CO)2Fe}+{[(Me2N)2C]2P}+(FeCl4)2- 5 which is characterized by single crystal X-ray analysis and spectra (IR, 1H, 31P-NMR).
    Notes: Die Reaktion des Metallophosphaalkens (η5-C5Me5(CO)2FeP = C(NMe2) 2 (1) mit wasserfreiem Zinndichlorid liefert die salzartige Verbindung {(η5-C5Me5)[η1-(Me2N)2 · C = P—P = C(NMe2)2](CO)2Fe}+{[(Me2N)2C]2P}+(FeCl4)2-5, die durch Einkristall-Röntgenstrukturanalyse und Spektren (IR, 1H, 31P-NMR) charakterisiert wird.
    Additional Material: 2 Ill.
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  • 8
    ISSN: 0044-2313
    Keywords: 1,2-Diphosphaferrocenes ; Transition Metal Complexes ; X-Ray Structure Analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,2-Diphosphaferrocenes as Ligands in Transition Metal Complexes. X-Ray Structure Analysis of [(η5-1,3-tBu2C5H3){η5-1,2-[Co2(CO)6]-3,4-(Me3SiO)2-5-(Me3Si)P2C3}]Reaction of metallo-1,2-diphosphapropene (η5-tBuC5H4)(CO)2Fe—P(SiMe3)—P=C(SiMe3)2 with (Z-cyclooctene)Cr(CO)5 afforded the pentacarbonylchromium adduct of a 1,2-diphosphaferrocene [(η5-tBuC5C5H4){η5-1-[Cr(CO)5]-3,4-(Me3SiO)2-5-(Me3Si)P2C3}Fe] (1 c). Diphosphaferrocene [(η5-tBuC5H4){η5-3,4-(Me3SiO)2-5-(Me3Si)P2C3}Fe] (2 c) was formed when (η5-tBuC5H4)(CO)2FeBr was treated with (Me3Si)2P—P=C(SiMe3)2 in toluene at 60°C. Photolysis of molybdenum- and tungsten hexacarbonyl in the presence of [(η5-1,3-tBu2C5H3){η5-3,4-(Me3SiO)2-5-(Me3Si)P2C3}Fe] (2 b) gave the pentacarbonylmetal adducts 8 (M = Mo) and 9 (M = W), respectively. A corresponding manganese derivative resulted from the photochemical reaction of 2 b and (MeC5H4)Mn(CO)3. Treatment of 2 b with Co2(CO)8 yielded trinuclear [(η5-1,3-tBu2C5H3){η5-1,2-[Co2(CO)6]-3,4-(Me3SiO)2-5-(Me3Si)P2C3}Fe] (11). Constitution and configuration of compounds 1 c, 2 c, 8 - 11 were determined by elemental analyses and spectra (IR, 1H-, 13C-, 31P-NMR, MS). In addition the molecular structure of 11 was established by single crystal X-ray analysis.
    Notes: Die Reaktion des Metallo-1,2-diphosphapropens (η5-tBuC5H4)(CO)2Fe—P(SiMe3)—P=C(SiMe3)2 mit (Cycloocten)Cr(CO)5 liefert das Pentacarbonylchrom-Addukt eines 1,2-Diphosphaferrocenes [(η5-tBuC5H4){η5-1-[Cr(CO)5]-3,4-(Me3SiO)2-5-(Me3Si)P2C3}Fe] (1c). Das Carbonyl-metall-freie 1,2-Diphosphaferrocen [(η5-tBuC5H4){η5-3,4-(Me3SiO)2-5-(Me3Si)P2C3}Fe] (2 c) entsteht bei der Umsetzung von (η5-tBuC5H4)(CO)2FeBr mit (Me3Si)2P—P = C(SiMe3)2 in Toluol bei 60°C. Das 1,2-Diphosphaferrocen [(η5-1,3-tBu2C5H3){η5-3,4-(Me3SiO)2-5-(Me3Si)P2C3}Fe] (2 b) reagiert mit den Hexacarbonylen von Molybdän und Wolfram bei Bestrahlung zu den Pentacarbonylmetall-Addukten 8 (M = Mo) und 9 (M = W). Ein entsprechender Mangankomplex 10 wird bei der photochemischen Reaktion von 2 b mit (MeC5H4)Mn(CO)3 gebildet. Im Gegensatz hierzu entsteht bei der Behandlung von 2 b mit Co2(CO)8 der dreikernige Komplex [(η5-1,3-tBu2C5H3){η5-1,2-[Co2(CO)6]-3,4-(Me3SiO)2-5-(Me3Si)P2C3} Fe] (11). Konstitution und Konfiguration der Verbindungen 1 c, 2 c, und 8 - 11 wurden durch Elementaranalysen und Spektren (IR, 1H-, 13C-, 31P-NMR, MS) ermittelt. Von 11 wurde zusätzlich eine Einkristall-Röntgenstrukturanalyse durchgeführt.
    Additional Material: 1 Ill.
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