PRODUCTS OF COMPLETE OXIDATIVE DECARBONYLATION OF TRICARBONYL(HYDROTRIS(3,5-DIMETHYL-1-PYRAZOLYL)BORATO)TUNGSTATE(O) BY TETRAALKYLTHIURAM DISULFIDES - (HB(ME2C3N2H)3)WS(S2CNET2), W2(MU-S)2(S2CNET2)4, AND [W(S2CNET2)4]+

被引:21
作者
YOUNG, CG
BRUCK, MA
ENEMARK, JH
机构
[1] LA TROBE UNIV,DEPT CHEM,BUNDOORA,VIC 3083,AUSTRALIA
[2] UNIV ARIZONA,DEPT CHEM,TUCSON,AZ 85721
关键词
D O I
10.1021/ic00030a013
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The final products of the reaction of NEt4[{HB(Me2pz)3}W(CO)3] and tetraethylthiuram disulfide in refluxing acetonitrile include the red, diamagnetic, air-stable thiotungsten(IV) complex {HB(Me2pz)3}WS(S2CNEt2) (1) and known W2(mu-S)2(S2CNEt2)4 (2) and [W(S2CNEt2)4]+ (isolated as chloride salt 3). The intermediate products of this reaction, {HB(Me2pz)3}W(CO)2(S2CNEt2) and {HB(Me2pz)3}W(CO)2(mu-S)W(S2CNEt2)2(SCNEt2), are described in the preceding paper in this issue. 1 (C20H32BN7S3W) crystallizes in triclinic space group P1BAR with a = 10.271 (2) angstrom, b = 10.467 (3) angstrom, c = 14.222 (4) angstrom, alpha = 96.53 (2)-degrees, beta = 91.03 (2)-degrees, gamma = 118.89 (2)-degrees, V = 1325.4 angstrom 3, and Z = 2. The structure was solved by Patterson and Fourier methods followed by least-squares refinement, using 3619 reflections, to a conventional R value of 0.045 (R(w) = 0.055). The monomeric complex exhibits a distorted octahedral fac-N3-fac-S3 coordination sphere composed of tridentate HB(Me2pz)3-, bidentate S2CNEt2- and terminal thio (W = S = 2.153 (2) angstrom) ligands. The spectroscopic (IR, electronic, H-1 NMR, ESR) properties of 1-3 are reported.
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页码:593 / 598
页数:6
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