SYNTHESIS AND CHARACTERIZATION OF THE MONOMERIC 3-COORDINATE INDIUM THIOLATE AND SELENOLATE COMPLEXES IN[E(2,4,6-T-BU3C6H2)]3 (E = S, SE)

The synthesis and characterization of the monomeric neutral three-coordinated indium thiolate and selenolate derivatives In[S(2,4,6-t-Bu3C6H2)]3 (1) and In[Se(2,4,6-t-Bu3C6H2)]3.2PhMe (2) are described. Compound 1 was synthesized by the reaction of In[N(SiMe3)2]3 with 3 equiv of HS(2,4,6-t-Bu3C6H2) in toluene whereas 2 was obtained by the reaction of InEt3 with 3 equiv of HSe(2,4,6-t-Bu3C6H2) in the same solvent. The compounds display an essentially planar trigonal coordination at the indium atom with an average In-S bond length of 2.398(6) angstrom and an average In-Se distance of 2.505(3) angstrom. The compounds were characterized by IR and H-1 NMR (Se-77 NMR in the case of 2) spectroscopy and by X-ray crystallography. Crystal data with Mo Kalpha (lambda = 0.710 69 angstrom) at 130 K: 1, a = 10.244(3) angstrom, b = 26.31(2) angstrom, c = 20.070(10) angstrom, beta = 90.74-degrees, V = 5409(5) angstrom3, Z = 4, space group P2(1)/n, 4834 (I > 2.5sigma(I)) data, R = 0.061; 2, a = 14.538(4) angstrom, b = 14.796(3) angstrom, c = 16.701(5) angstrom, alpha = 85.65(2)degrees, beta = 83.60(2)degrees, gamma = 61.64(2)degrees, V = 3140.4(13) angstrom3, Z = 2, space group P1BAR, 8415 (I > 3sigma(I)) data, R = 0.049.