CHEMISTRY OF ORGANOINDIUM HYDRIDES - SYNTHESIS, CHARACTERIZATION, AND CRYSTAL-STRUCTURE OF K(H[IN(CH2CME3)3]2)

Two new organoindium hydrides K{H[In(CH2CMe3)3]2} and K[HIn(CH2CMe3)3] have been prepared and fully characterized according to their physical properties, partial elemental analyses, molecular weight studies, and IR and H-1 and C-13 NMR spectral studies. The unique hydrogen atoms bonded to indium in the two compounds provide characteristic infrared bands and H-1 NMR resonances, which have been identified by comparative studies with the corresponding deuterium derivatives. The indium hydride K{H[In(CH2CMe3)3]2} crystallizes in the monoclinic space group C2/c (No. 15) with cell parameters of a = 22.243 (5) angstrom, b = 17.021 (3) angstrom, c = 21.290 (3) angstrom, beta = 110.350 (10)-degrees, V = 7557 (2) angstrom 3, and Z = 8. Final discrepancy indicies were R = 6.32% and R(w) = 4.97% for all 4947 independent data and R = 2.96% and R(w) = 3.67% for those 2924 reflections with \F(o)\ > 6-sigma(F(o)). The crystal is composed of K+ cations and (Me3CCH2)3In-H-In(CH2CMe3)3- anions, each of which lie on 2-fold axes. In-C(neopentyl) distances range from 2.199 (6) to 2.231 (6) angstrom (averaging 2.213 angstrom), while In-(mu-H) distances are 1.933 (15) and 1.950 (23) angstrom. In-H-In angles are 151 (5) and 161 (5)-degrees.