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Synthesis and X‐ray Structures of the Polycyclic Dimers {[PhB(μ‐N t Bu) 2 AsN( t Bu)H]LiI} 2 and [PhB(μ‐N t Bu) 2 AsN( t Bu)Li] 2
Author(s) -
Konu Jari,
Chivers Tristram
Publication year - 2008
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.200700543
Subject(s) - adduct , dimer , diethyl ether , chemistry , lithium (medication) , monomer , iodide , solvent , nuclear magnetic resonance spectroscopy , medicinal chemistry , ether , yield (engineering) , crystallography , stereochemistry , derivative (finance) , inorganic chemistry , organic chemistry , materials science , medicine , economics , financial economics , metallurgy , endocrinology , polymer
The metathesis of [PhB( μ ‐N t Bu) 2 ]AsCl and t BuN(H)Li in 1:1 molar ratio in diethyl ether produced the amido derivative [PhB(μ‐N t Bu) 2 AsN( t Bu)H] ( 1 ) in good yield. The lithiation of 1 with one equivalent of n BuLi afforded the lithium salt [PhB(μ‐N t Bu) 2 AsN( t Bu)Li] ( 2a ). Both 1 and 2a were characterized by multinuclear NMR spectroscopy. The crystal structure of 2a is comprised of a U‐shaped, centrosymmetric dimer in which the monomeric [PhB(μ‐N t Bu) 2 AsN( t Bu)] − Li + units are linked by Li‐N interactions to give a six‐rung ladder. Oxidation of 2a with one‐half equivalent of I 2 in diethyl ether resulted in hydrogen abstraction from the solvent to give the dimeric lithium iodide adduct {[PhB(μ‐N t Bu) 2 AsN( t Bu)H]LiI} 2 ( 1 ·LiI) with a central Li 2 I 2 ring.