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Synthesis and structure of N,C-chelated organoantimony(V) and organobismuth(V) compounds

Autoři: Vránová Iva | Jambor Roman | Růžička Aleš | Jirásko Robert | Dostál Libor

Rok: 2014

Druh publikace: článek v odborném periodiku

Název zdroje: Dalton Transactions

Název nakladatele: Royal Society of Chemistry

Místo vydání: Cambridge

Strana od-do: 505-512

Tituly:

Jazyk	Název	Abstrakt	Klíčová slova
cze	Syntéza a struktura N,C-chelatovaných organoantimoničných a organobismutičných sloučenin	Reakce N,C-chelatovaných Sb(III) a Bi(III) sloučenin LMCl2 (M = Sb (1), Bi (2), L = [o-(CH=N-2,6-iPr(2)C(6)H(3))C6H4]) s PhLi v poměru 1 : 1 a 1 : 2 vedlo k syntéze sloučenin LM(Ph)Cl (M = Sb (3) , Bi (4)) a LMPh2 (M = Sb (5), Bi (6)). Oxidace těchto sloučenin s SO2Cl2 vedlo k syntéze N,C-chelatovaných organoantimoničných a organobismutičných sloučenin LSbCl4 (7), LSb(Ph)Cl-3 (8) a LSbPh2Cl2 (9).	Syntéza; struktura; N,C-chelatované sloučeniny; organoantimoničné a organobismutičné sloučeniny
eng	Synthesis and structure of N,C-chelated organoantimony(V) and organobismuth(V) compounds	The reaction of N,C-intramolecularly coordinated organoantimony(III) and organobismuth(III) compounds LMCl2 (M = Sb (1) or Bi (2) and L = [o-(CH=N-2,6-iPr(2)C(6)H(3))C6H4]) with phenyllithium in a 1 : 1 or 1 : 2 molar ratio gave compounds LM(Ph)Cl (M = Sb (3) or Bi (4)) and LMPh2 (M = Sb (5) or Bi (6)) in moderate to good yields. Compound 3 could also be prepared by the treatment of the lithium compound LLi with in situ prepared PhSbCl2. Oxidation of the antimony(III) compounds 1, 3 and 5 with one equivalent of SO2Cl2 proceeded smoothly with formation of organoantimony(V) compounds LSbCl4 (7), LSb(Ph)Cl-3 (8) and LSbPh2Cl2 (9) in nearly quantitative yields. Compounds 7-9 are yellowish solids that are stable for a long time even in the presence of air. In contrast, only organobismuth(III) compounds 4 and 6 could be successfully oxidized using SO2Cl2 to give compounds LBi(Ph)Cl-3 (10) and LBiPh2Cl2 (11). Compound 11 is stable, but compound 10 readily decomposed in solution and could not be isolated and stored for a longer period. All attempts to prepare compound LBiCl4 by the oxidation of 2 with SO2Cl2 failed and resulted only in a mixture of products. All studied compounds were characterized by electrospray ionization (ESI) mass spectrometry, and H-1 and C-13 NMR spectroscopy. The molecular structures of 3-7, 9 and 11 were unambiguously established using single-crystal X-ray diffraction analysis.	bond covalent radii; chelated organoantimony(iii); dynamic-behavior; carbon-dioxide; ligands; coordination; complexes; r=2-(me2nch2)c6h4; derivatives; efficient

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