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Alternative syntheses and X-ray diffraction analyses of the parent tricarbaborane compounds [nido-7,8,9-C(3)B(8)H(11)](-), [nido-7,8,10-C(3)B(8)H(11)](-) and [1-(eta(5)-C(5)H(5))-closo-1,2,4,10-FeC(3)B(8)H(11)]
Authors: Holub Josef | Růžička Aleš | Padělková Zdeňka | Štíbr Bohumil
Year: 2011
Type of publication: článek v odborném periodiku
Name of source: Journal of Organometallic Chemistry
Page from-to: 2742-2745
Titles:
Language Name Abstract Keywords
cze Alternativní syntéza a X-ray difrakční analýza trikarbaboránových sloučenin [nido-7,8,9-C(3)B(8)H(11)](-), [nido-7,8,10-C(3)B(8)H(11)](-) a [1-(eta(5)-C(5)H(5))-closo-1,2,4,10-FeC(3)B(8)H(11)] Reakce neutrálního trikarbaboranu nido-7,8,9-C(3)B(8)H(12) (1) s triethylaminz s CH(2)Cl(2) vede kvantitativně k deprotonaci a izolaci odpovídající soli Et(3)NH(+)[nido-7,8,9-C(3)B(8)H(11)](-) (2). Tato sůl byla modifikována PSH(+) a Me(4)N(+)cestou methatetické iontové výměny. Zahřátím Me(4)N(+)[7,8,9-C(3)B(8)H(11)](-) v minerálním oleji na 350 stupňů po 2 h byla získána isomerní sloučenina Me(4)N(+)[7,8,10-C(3)B(8)H(11)](-). Sloučenina 910 bzla komplexována reakcí s [CpFe(CO)(2)](2) (Cp = eta(5)-C(5)H(5)) za vzniku [1-Cp-closo-1,2,4, 10-FeC(3)B(8)H(11)] (4) v 60% výtěžku. Struktury připravených sloučenin 1 (PSH(+) sůl), 2 (MePPh(3)(+)sůl), a 4 byly determinovánz X-ray analýzou. X-ray difrakční analýza;trikarbaboránová sloučenina;krystalografie
eng Alternative syntheses and X-ray diffraction analyses of the parent tricarbaborane compounds [nido-7,8,9-C(3)B(8)H(11)](-), [nido-7,8,10-C(3)B(8)H(11)](-) and [1-(eta(5)-C(5)H(5))-closo-1,2,4,10-FeC(3)B(8)H(11)] Reaction of the neutral tricarbaborane nido-7,8,9-C(3)B(8)H(12) (1) with triethylamine in CH(2)Cl(2) led to quantitative deprotonation and isolation of the corresponding Et(3)NH(+) salt of the [nido-7,8,9-C(3)B(8)H(11)](-) anion (2). This was converted into PSH(+) and Me(4)N(+) salts via metathetic cation exchange. Heating of the solid Me(4)N(+)[7,8,9-C(3)B(8)H(11)](-) in mineral oil at 350 degrees C for 2 h resulted in thermal rearrangement and isolation of the cage isomeric compound Me(4)N(+)[7,8,10-C(3)B(8)H(11)](-). Finally, compound 1 was directly complexed via reaction with [CpFe(CO)(2)](2) (Cp = eta(5)-C(5)H(5)) to generate the ferratricarbollide sandwich [1-Cp-closo-1,2,4, 10-FeC(3)B(8)H(11)] (4) in 60% yield. The structures of all the generic compounds of tricarbollide chemistry, 1 (PSH(+) salt), 2 (MePPh(3)(+)salt), and 4, were established unambiguously by an X-ray diffraction analysis. Carboranes;Crystallography;Iron complexes;Metallacarboranes;Tricarbaboranes;Tricarbollides

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