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.
引用
收藏
页码:593 / 598
页数:6
相关论文
共 35 条
[1]   PREPARATION AND CHARACTERIZATION OF DI-MU-SULFIDO BINUCLEAR COMPOUNDS OF W(IV) AND W(V) - UNAMBIGUOUS EXAMPLES OF FORMAL SINGLE AND DOUBLE-BONDS BETWEEN TUNGSTEN ATOMS [J].
BINO, A ;
COTTON, FA ;
DORI, Z ;
SEKUTOWSKI, JC .
INORGANIC CHEMISTRY, 1978, 17 (10) :2946-2950
[2]   RHENIUM COMPLEXES WITH DI-THIOLATE AND TRI-THIOLATE LIGANDS - THE SYNTHESIS AND X-RAY CRYSTAL-STRUCTURES OF SQUARE PYRAMIDAL [PPH4][REO(SCH2CH2S)2] AND [NME4][RES(SCH2CH2S)2] AND TRIGONAL PRISMATIC [PPH4][RE((SCH2)3CCH3)2] [J].
BLOWER, PJ ;
DILWORTH, JR ;
HUTCHINSON, JP ;
NICHOLSON, T ;
ZUBIETA, J .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1986, (07) :1339-1345
[3]   TUNGSTEN CARBONYL-COMPLEXES WITH DITHIOCARBAMATE LIGANDS [J].
BROOMHEAD, JA ;
YOUNG, CG .
AUSTRALIAN JOURNAL OF CHEMISTRY, 1982, 35 (02) :277-285
[4]   CONVERSION OF A DITHIOCARBAMATE LIGAND TO A THIOCARBOXAMIDO LIGAND TO FORM W(S)(PHC=CPH)(S2CNET2)(SCNET2) [J].
BROWER, DC ;
TONKER, TL ;
MORROW, JR ;
RIVERS, DS ;
TEMPLETON, JL .
ORGANOMETALLICS, 1986, 5 (06) :1093-1097
[5]  
CHEN GJJ, 1976, INORG CHIM ACTA, V17, pL67
[6]   UNIQUE REACTIVITY CHARACTERISTICS OF MO-COORDINATED S-2(2-) AND S-4(2-) LIGANDS [J].
COUCOUVANIS, D ;
HADJIKYRIACOU, A ;
DRAGANJAC, M ;
KANATZIDIS, MG ;
ILEPERUMA, O .
POLYHEDRON, 1986, 5 (1-2) :349-356
[8]  
Coucouvanis D., 1979, PROG INORG CHEM, V26, P301, DOI [10.1002/9780470166277.ch5, DOI 10.1002/9780470166277.CH5]
[9]  
Cromer D.T, 1974, INT TABLES XRAY CRYS, VIV
[10]   SYNTHESIS, INTERCONVERSIONS, AND STRUCTURAL CHARACTERIZATION OF THE [(S4)2MOO]2-, (MO2S10)2-, AND (MO2S12)2- ANIONS [J].
DRAGANJAC, M ;
SIMHON, E ;
CHAN, LT ;
KANATZIDIS, M ;
BAENZIGER, NC ;
COUCOUVANIS, D .
INORGANIC CHEMISTRY, 1982, 21 (09) :3321-3332