J. Janik, C. Narula, E. G. Gulliver
Apr 6, 1988
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Influential Citations
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Inorganic Chemistry
Abstract
Reactions of tris(trimethylsilyl)amine, N(SiMe/sub 3/)/sub 3/, with several monochloroboranes, CH/sub 3/NCH/sub 2/CH/sub 2/N(CH/sub 3/)BCl, o-OC/sub 6/H/sub 4/OBCl, and SCH/sub 2/CH/sub 2/SBCl, have been examined, and the ((trimethylsilyl)amino)boranes o-OC/sub 6/H/sub 4/OBN(SiMe/sub 3/)/sub 2/, (o-OC/sub 6/H/sub 4/OB)/sub 2/NSiMe/sub 3/, SCH/sub 2/CH/sub 2/SBN(SiMe/sub 3/)/sub 2/, and (SCH/sub 2/CH/sub 2/SB)/sub 2/NSiMe/sub 3/ have been prepared and characterized by spectroscopic methods. The molecular structure of (o-OC/sub 6/H/sub 4/OB)/sub 2/NSiMe/sub 3/ has been determined by single-crystal X-ray diffraction analysis and found to crystallize in the orthorhombic space group P2/sub 1/2/sub 1/2/sub 1/ (No. 19) with a = 7.189 (1) /angstrom/, b = 19.387 (4) /angstrom/, c = 24.508 (4) /angstrom/ Z = 8, V = 3416 (1) /angstrom//sup 3/, and /rho//sub calcd/ = 1.26 g cm/sup /minus/3/. The structure was solved by direct methods, and blocked least-squares refinement converged with R/sub F/ = 10.1% and R/sub wF/ = 9.2% on 3012 unique data with F > 2/sigma/(F). The structure contains two independent molecules in the unit cell, and the central nitrogen atoms have a trigonal-planar geometry. Important bond distances include B-N/sub av/ = 1.421 (13) /angstrom/, Si-N/sub av/ = 1.783 (7) /angstrom/, and B-O/sub av/ = 1.390 (13) /angstrom/. Attempts to prepare the 1,3,2-diazaborolidine CH/sub 3/NCH/submore » 2/CH/sub 2/N(CH/sub 3/)BN(SiMe/sub 3/)/sub 2/ and triborylamine compounds by this synthetic method were unsuccessful. 35 refs., 4 tabs.« less