Synthesis, molecular structure, and nuclear magnetic resonance spectra of the anionic monocarbametallaborane [NEt4][(CO)3(PPh3)(OH)-closo-MoCB10H10]·CH2Cl2
Abstract
Reaction between arachno-[B10H14]2– and a mixture of [Mo(CO)3(MeCN)3] and PPh3 results in the formation of the twelve-vertex closo-carbamolybdaborane anion [1,1,1,1-(CO)3(PPh3)-2-(OH)-closo-1,2-MoCB10H10]–, isolated in 50% yield as its tetraethylammonium salt. Crystals of [NEt4][(CO)3(PPh3)MoC(OH)B10H10]·CH2Cl2 are triclinic, space group P(no. 2), with a= 962.0(3), b= 1 006.9(3), c= 2 156.3(3) pm, α= 95.10(3), β= 100.55(3), and γ= 101.63(2)°, and Z= 2. The structure was refined to R= 0.0505, R′= 0.0507 using 4 427 observed data [I > 2σ(I)]. Magnetic multiple-resonance spectroscopy was used for the tentative assignment of the 11B and 1H n.m.r. spectra.