Inorganic Chemistry, Vol.33, No.26, 6154-6162, 1994
Synthesis and Characterization of N,N-Diethyl, Pyrrolidyl, and Piperidyl Monothiocarbamate Derivatives of Dimethyltellurium(IV) - Crystal-Structures of Me(2)Te(Sconet(2))(2), Me(2)Tecl(Sconet(2)), Me(2)Tebr(Sconet(2)), and Me(2)Tei(Sconet(2))
The dimethylbis(monothiocarbamato)tellurium(IV) compounds Me(2)Te[SCONR(2)](2), where NR(2) = NEt(2), N(CH2)(3)-CH2, and N(CH2)(4)CH2, and the halodimethyl(N,N-diethyl and pyrrolidyl monothiocarbamato)tellurium(IV) compounds Me(2)TeX[SCONR(2)], where X = Cl, Br, and I and NR(2) = NEt(2) or N(CH2)(3)CH2, have been prepared, with yields of 80% or better, by the reaction of the sodium salts of the monothiocarbamic acids, in excess or in equimolar amounts, with dimethyltellurium dihalide. The compounds were characterized by elemental analysis and H-1, C-13, and Te-125 NMR, infrared, and Raman spectroscopy. The crystal structures of Me(2)Te[SCONEt(2)](2), Me(2)TeCl[SCONEt(2)], Me(2)TeBr[SCONEt(2)], and Me(2)TeI[SCONEt(2)] were determined. Me(2)Te[SCONEt(2)](2) (1), which crystallizes as monoclinic in space group P2(1)/n (No. 14), has the cell parameters a = 11.184(2) Angstrom, b = 10.036(2) Angstrom, c = 16.531(2) Angstrom, beta = 94.08(1)degrees, V = 2424(1) Angstrom(3), Z = 4, R = 0.0337, and RW(=) 0.0270. Me(2)TeCl[SCONEt(2)] (4), which crystallizes as monoclinic in space group P2(1)/c (No. 14), has the cell parameters a = 10.539(2) Angstrom, b = 10.864(2) Angstrom, c = 11.511(2) Angstrom, beta = 112.23(1)degrees, V = 1220.0(4) Angstrom(3), Z = 4, R = 0.0319, and R(W) = 0.0289. Me(2)TeBr[SCONEt(2)] (5), which also crystallizes as monoclinic in space group P2(1)/c (No. 14), has the cell parameters 10.533(4) Angstrom, b = 10.965(2) Angstrom, c = 11.814(4) Angstrom, beta = 113.11(2)degrees, V = 1254.9(7) Angstrom(3), Z = 4, R = 0.0528, and R(W) = 0.0462. Me(2)TeI[SCONEt(2)] (6), which also crystallizes as monoclinic in space group P2(1)/c (No. 14), has the cell parameters a = 10.702(2) Angstrom, b = 11.241(1) Angstrom, c = 12.280(3) Angstrom, beta = 114.51(2)degrees, V = 1344.2(5) Angstrom(3), Z = 4, R = 0.0430, and R(W) = 0.0343.