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二甲基碲（IV）化合物的吡咯烷基和哌啶基二硫代甲酸酯衍生物的合成与光谱表征。Me(2)Te[S(2)CN(CH(2))(3)CH(2)](2)、Me(2)Te[S(2)CN(CH(2))(4)CH(2)](2)、Me(2)Te{[S(2)CN(CH(2))(3)CH(2)][S(2)CN(CH(2))(4)CH(2)]}、Me(2)TeCl[S(2)CN(CH(2))(3)CH(2)]、Me(2)TeBr[S(2)CN(CH(2))(3)CH(2)]、Me(2)TeI[S(2)CN(CH(2))(3)CH(2)]、Me(2)TeCl[S(2)CN(CH(2))(4)CH(2)]和Me(2)TeI[S(2)CN(CH(2))(4)CH(2)]的晶体结构

Synthesis and Spectroscopic Characterization of Pyrrolidyl and Piperidyl Dithioformate Derivatives of Dimethyltellurium(IV) Compounds. Crystal Structures of Me(2)Te[S(2)CN(CH(2))(3)CH(2)](2), Me(2)Te[S(2)CN(CH(2))(4)CH(2)](2), Me(2)Te{[S(2)CN(CH(2))(3)CH(2)][S(2)CN(CH(2))(4)CH(2)]}, Me(2)TeCl[S(2)CN(CH(2))(3)CH(2)], Me(2)TeBr[S(2)CN(CH(2))(3)CH(2)], Me(2)TeI[S(2)CN(CH(2))(3)CH(2)], Me(2)TeCl[S(2)CN(CH(2))(4)CH(2)], and Me(2)TeI[S(2)CN(CH(2))(4)CH(2)].

作者信息

Drake John E., Yang Jincai

机构信息

Department of Chemistry and Biochemistry, University of Windsor, Windsor, Ontario, Canada N9B 3P4.

出版信息

Inorg Chem. 1997 Apr 23;36(9):1890-1903. doi: 10.1021/ic9608455.

DOI:10.1021/ic9608455
PMID:11669795
Abstract

Dimethylbis(pyrrolidyl and piperidyl dithioformato)tellurium(IV) compounds and the corresponding halodimethyl compounds, Me(2)TeX[S(2)CN(CH(2))(n)()CH(2)], where n = 3, 4 and X = Cl, Br, and I, have been prepared. The compounds were characterized by elemental analysis and IR, Raman, and multinuclear NMR spectroscopies, including some variable temperature studies. The following crystallize as monoclinic in space group P2(1)/c (No. 14). Me(2)TeS(2)CN(CH(2))(3)CH(2) (1): a = 6.38(1) Å, b = 18.902(7) Å, c = 14.672(6) Å, beta = 97.73(6) degrees V = 1752(2) Å(3), Z = 4, R = 0.0636, R(w) = 0.0642. Me(2)Te{[S(2)CN(CH(2))(3)CH(2)][S(2)CN(CH(2))(4)(CH(2))]} (3): a = 6.55(1) Å, b = 19.716(6) Å, c = 14.900(9) Å, beta = 95.27(8) degrees, V = 1928(3) Å(3), Z = 4, R = 0.0618, R(w) = 0.0511. Me(2)TeCl[S(2)CN(CH(2))(3)CH(2)] (4): a = 9.952(3) Å, b = 6.386(3) Å, c = 18.834(3) Å, beta = 95.32(2) degrees, V = 1191.7(6) Å(3), Z = 4, R = 0.0358, R(w) = 0.0314. Me(2)TeBr[S(2)CN(CH(2))(3)CH(2)] (5): a = 10.085(4) Å, b = 6.446(4) Å, c = 19.020(5) Å, beta = 95.08(3) degrees, V = 1231.7(8) Å(3), Z = 4, R = 0.0559, R(w) = 0.0469. Me(2)TeCl[S(2)CN(CH(2))(4)CH(2)] (7) is P2(1)/a (No. 14) with a = 9.756(2) Å, b = 11.242(2) Å, c = 12.028(3) Å, beta = 92.26(3) degrees, V = 1318.2(7) Å(3), Z = 4, R = 0.0438, R(w) = 0.0442, and Me(2)TeI[S(2)CN(CH(2))(4)CH(2)] (9) is P2(1) (No. 4) with a = 6.019(3) Å, b = 8.986(4) Å, c = 13.012(2) Å, beta = 100.61(3) degrees, V = 691.7(6) Å(3), Z = 2, R = 0.0364, R(w) = 0.0305. Me(2)TeI[S(2)CN(CH(2))(3)CH(2)] (6) is orthorhombic in Pbca (No. 61) with a = 13.951(6) Å, b = 19.849(8) Å, c = 9.261(4) Å, V = 2564(1) Å(3), Z = 8, R = 0.0392, R(w) = 0.0326, and Me(2)TeS(2)CN(CH(2))(4)CH(2) (2) is triclinic in P&onemacr; (No. 2) with a = 9.624(2) Å, b = 12.904(3) Å, c = 9.008(2) Å, alpha = 98.29(2) degrees, beta = 111.19(2) degrees, gamma = 99.64(2) degrees, V = 1002.5(4) Å(3), Z = 2, R = 0.0504, R(w) = 0.0454. The immediate environment about Te is that of a sawhorse structure in which the lone pair is apparently stereochemically active and occupying an equatorial position in a distorted trigonal bipyramid. The second sulfur atom appears also to be in the coordination sphere resulting in the following distorted arrangements about Te: pseudo pentagonal bipyramidal in 1 and 3, octahedral in 2, and square pyramidal in 5, 6, 7, and 9.

摘要

已制备出二甲基双（吡咯烷基和哌啶基二硫代甲酸根）碲（IV）化合物以及相应的卤代二甲基化合物Me(2)TeX[S(2)CN(CH(2))(n)CH(2)]，其中n = 3、4且X = Cl、Br和I。通过元素分析以及红外光谱、拉曼光谱和多核核磁共振光谱对这些化合物进行了表征，包括一些变温研究。以下化合物结晶为单斜晶系，空间群为P2(1)/c（编号14）。Me(2)TeS(2)CN(CH(2))(3)CH(2)（1）：a = 6.38(1) Å，b = 18.902(7) Å，c = 14.672(6) Å，β = 97.73(6)°，V = 1752(2) Å(3)，Z = 4，R = 0.0636，R(w) = 0.0642。Me(2)Te{[S(2)CN(CH(2))(3)CH(2)][S(2)CN(CH(2))(4)CH(2)]}（3）：a = 6.55(1) Å，b = 19.716(6) Å，c = 14.900(9) Å，β = 95.27(8)°，V = 1928(3) Å(3)，Z = 4，R = 0.0618，R(w) = 0.0511。Me(2)TeCl[S(2)CN(CH(2))(3)CH(2)]（4）：a = 9.952(3) Å，b = 6.386(3) Å，c = 18.834(3) Å，β = 95.32(2)°，V = 1191.7(6) Å(3)，Z = 4，R = 0.0358，R(w) = 0.0314。Me(2)TeBr[S(2)CN(CH(2))(3)CH(2)]（5）：a = 10.085(4) Å，b = 6.446(4) Å，c = 19.020(5) Å，β = 95.08(3)°，V = 1231.7(8) Å(3)，Z = 4，R = 0.0559，R(w) = 0.0469。Me(2)TeCl[S(2)CN(CH(2))(4)CH(2)]（7）属于P2(1)/a（编号14），a = 9.756(2) Å，b = 11.242(2) Å，c = 12.028(3) Å，β = 92.26(3)°，V = 1318.2(7) Å(3)，Z = 4，R = 0.0438，R(w) = 0.0442，而Me(2)TeI[S(2)CN(CH(2))(4)CH(2)]（9）属于P2(1)（编号4），a = 6.019(3) Å，b = 8.986(4) Å，c = 13.012(2) Å

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