Polarographie Behaviour of Transition Metal Nitrosyl Complexes in Nonaqueous Media. IV. Cyclopentadienylnitrosylnickel
نویسنده
چکیده
H 9 : Mg : Cl = 0,152 : 0,575 : 1,080, d.h. es lag ein Gemisch von 0,152 Mol ,HMgCl‘ mit 0,423 Mol MgCl2 (beide solvatisiert mit THF) vor. Bei der Bestimmung des aktiven Wasserstoffs wurde eine mit fl. N2 gekühlte, mit Kieselgel gefüllte Falle vorgeschaltet um eventuell bei der Hydrolyse freigesetztes Äthan (C2H5MgCl = HCl —> C2H6 + MgCl2) vom gebildeten Wasserstoff ab zutrennen. In keinem Versuch war jedoch Äthan an wesend, desgleichen auch Bor, falls in der Tabelle nicht anders vermerkt. Die Gegenwart von BH4 oder ande rem Alkylboranat läßt sich besonders empfindlich IRspektroskopisch nachweisen. Bei Versuchen, in denen 3 Mole RMgCl mit 2 Molen BH3 umgesetzt wurden, bestand der bei — 25° ausfallende Niederschlag aus MgCl(BH4) -2 THF im Gemisch mit MgCl2*nTHF. Aus ätherischen G r i g n a r d Lösungen ließen sich keine Festprodukte bei Umsetzungen mit Diboran bei — 25° isolieren.
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