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• W2080494827 abstract "The bis((dimethylphosphino)methyl)-substituted alcohol (Me2PCH2)2CHOH (1) was prepared from the respective bis(3,5-dimethylbenzyl)phosphonium dichloride by reductive elimination of mesitylene with lithium alanate in 56% yield. Deprotonation with n-butyllithium or elemental sodium gave the respective alkali metal alcoholates [(Me2PCH2)2CHOM]6 (M = Li (2), Na (3)). Both compounds have a core consisting of two stacked M3O3 hexagons held together by short M−O bonds. In 2, in addition to three oxygen atoms, each lithium atom is coordinated by one phosphino group of an adjacent ligand in a distorted tetrahedral geometry (Li−P = 2.60(1) Å). In 3 each sodium atom is coordinated by two phosphino groups from different ligands in addition to the oxygen atoms. The coordination geometry at the sodium atom is a distorted trigonal bipyramid (O3P2), the two phosphine donors being in axial and equatorial positions, respectively (Na−P = 3.083(2), 3.151(2) Å). The tris((dimethylphosphino)methyl)-substituted alcohol (Me2PCH2)3COH (4) was synthesized from 1-chloro-2,3-epoxy-2-(chloromethyl)propane by reaction with 3 equiv of LiPMe2 in 69% yield. Its crystal structure contains a O−H···P hydrogen bond (O···P = 3.460(1) Å). Reaction of 4 with excess n-butyllithium in the absence of solvent gave the dimeric polylithium mixed-anion aggregate [(Me2PCH2)3COLi·2Li-n-Bu]2 (5), the core of which consists of two stacked LiOLiCLiC hexagons. Each (Me2PCH2)3CO- anion is coordinated to three Li+ cations via O−Li and P−Li bonds. The same reaction in toluene led to further deprotonation of the methylene groups in 4, subsequent loss of Li2O, and formation of the symmetrically tris(phosphino)-substituted trimethylenemethane dianion. It crystallizes as the mixed-anion aggregate [(Me2PCH2)3CO-·3Li+·(Me2PCH)3C2-] (6), consisting of an almost equilateral triangle of lithium atoms sandwiched between the two anions. Each lithium atom has a severly distorted tetrahedral coordination geometry consisting of two phosphino donors, one oxygen atom, and one methylene group." @default.
• W2080494827 created "2016-06-24" @default.
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• W2080494827 date "2003-06-24" @default.
• W2080494827 modified "2023-10-17" @default.
• W2080494827 title "Multidentate Phosphinoalkoxides: Synthesis, Deprotonation, and Building Blocks in Polylithium Mixed-Anion Aggregates" @default.
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• W2080494827 doi "https://doi.org/10.1021/om030118z" @default.
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