184477-87-0Relevant articles and documents
Methylene-bridged group 13-15 compounds, R2MCH2PPh2 (R = CH2CMe3, CH2SiMe3; M = Ga, In). Crystal structure of [(Me3CCH2)2InCH2PPh 2]2·C6D6, a molecule containing an In-C-P-In-C-P ring in a chair conformation
Beachley Jr.,Banks, Michael A.,Churchill, Melvyn Rowen,Feighery, William G.,Fettinger, James C.
, p. 3036 - 3040 (2008/10/08)
A series of compounds of the type R2MCH2PPh2 (R = CH2CMe3, CH2SiMe3; M = Ga, In) has been prepared by metathetical reactions between the appropriate diorganometal halide and LiCH2PPh2 in pentane or Et2O at -78°C. All compounds were characterized by physical properties, partial elemental analyses (C, H), and cryoscopic molecular weight measurements in benzene solution as well as IR, 1H NMR, and 31P NMR spectroscopic data. All appropriate data support the existence of dimeric molecules. The monomeric species dimerize by apparent Lewis acid-base interactions. These interactions are sufficiently strong that the compounds do not form stable adducts with oxygen- or nitrogen-containing Lewis bases. [(Me3CCH2)2InCH2PPh 2]2·C6D6 crystallizes in the centrosymmetric triclinic space group P1 (No. 2) with a = 13.142 (3) A?, b = 15.109 (3) A?, c = 15.746 (4) A?, α = 85.27 (2)°, β = 67.99 (2)°, γ = 66.00 (1)°, V = 2639 (1) A?3, and Z = 2. Diffraction data (Mo Kα, 20 = 4.5-45.0°) were collected on a Syntex P21 diffractometer; the structure was solved and refined to RF = 6.0% and RwF = 6.4% for all 6932 independent reflections (RF = 4.5% and RwF = 6.2% for those 5495 data with |Fo| > 6σ(|Fo|)). The crystal is composed of two crystallographically independent [(Me3CCH2)InCH2PPh2]2 molecules (each having precise Ci symmetry) and a C6D6 molecule of solvation. The two independent [(Me3CCH2)InCH2PPh2]2 molecules have similar configurations. Each is based upon a six-membered In-CH2-P-In-CH2-P ring with a chair conformation. Bond lengths of interest include In-P = 2.694 (2)-2.703 (2) A?, In-CH2 = 2.255 (7)-2.261 (8) A?, and In-neopentyl = 2.216 (7)-2.234 (7) A?.
