RHENIUM COMPLEX OF A TRIPLY DEPROTONATED CHELATED THIOSEMICARBAZIDE AND ITS CONVERSION TO A NITRIDE COMPLEX VIA A HYDRAZIDE INTERMEDIATE - CRYSTAL-STRUCTURE OF [RECL2(NH)(NHNH2)(PPH(3))(2)]

被引：16
作者：
DILWORTH, JR
LEWIS, JS
MILLER, JR
ZHENG, YF
机构：
来源：
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS | 1995年 / 08期
关键词：
D O I：
10.1039/dt9950001357
中图分类号：
O61 [无机化学];
学科分类号：
070301 ; 081704 ;
摘要：
Reaction of [Re(O)X(3)(PPh(3))(2)] (X = Cl or Br) with thiosemicarbazides RNHCSNHNH(2) (R = Me or Ph) in ethanol under reflux in the presence of aqueous HX and PPh(3) gave the rhenium(V) S,N-chelated thiosemicarbazide(3-) complexes [ReX(2)(NNCSNHR)(PPh(3))(2)]. On extended reflux for X = Cl the purple imide-hydrazide [ReCl2(NH)(NHNH2)(PPh(3))(2)] was formed, and a crystal structure determination showed a pseudo-octahedral geometry with trans PPh(3) and nitrogen ligands and a significantly bent M-N-N system (145.5 degrees). Further reflux gave the known nitride complex [Re(N)Cl-2(PPh(3))(2)] in good yield.
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页码：1357 / 1361
页数：5
相关论文
共 20 条
[1]  
CAI S, 1991, INORG CHEM, V30, P4107
[2]  
CAMBELL MJM, 1975, COORDIN CHEM REV, V15, P279
[3]   SOME BENZOYLAZO-COMPLEXES OF RHENIUM HALIDES WITH TERTIARY PHOSPHINES, AND RELATED COMPOUNDS [J].
CHATT, J ;
DILWORTH, JR ;
LEIGH, GJ ;
GUPTA, VD .
JOURNAL OF THE CHEMICAL SOCIETY A -INORGANIC PHYSICAL THEORETICAL, 1971, (16) :2631-&
[4]   NITRIDO-COMPLEXES OF RHENIUM WHICH CONTAIN TERTIARY PHOSPHINES, AND ATTEMPTS TO PREPARE THEIR OSMIUM ANALOGUES [J].
CHATT, J ;
FALK, CD ;
LEIGH, GJ ;
PASKE, RJ .
JOURNAL OF THE CHEMICAL SOCIETY A -INORGANIC PHYSICAL THEORETICAL, 1969, (15) :2288-&
[5]   COMPLEX COMPOUNDS OF TERTIARY PHOSPHINES AND A TERTIARY ARSINE WITH RHENIUM(V), RHENIUM(III), AND RHENIUM(II) [J].
CHATT, J ;
ROWE, GA .
JOURNAL OF THE CHEMICAL SOCIETY, 1962, (10) :4019-&
[6]   PREPARATION, CRYSTAL AND MOLECULAR-STRUCTURE OF [MOCL2(NH)O(ETPH2PO)2] - EXAMPLE OF TERMINAL, NON-LINEAR IMIDO-COORDINATION [J].
CHATT, J ;
CHOUKROUN, R ;
DILWORTH, JR ;
HYDE, J ;
VELLA, P ;
ZUBIETA, J .
TRANSITION METAL CHEMISTRY, 1979, 4 (01) :59-63
[7]   PREPARATION AND PROTONATION OF [REBR(N2PH)2(PPH3)2]. STRUCTURE OF [REBR2(NNPH)(NNHPH)(PPH3)2], A COMPLEX WITH A HYDRAZIDO(2-) LIGAND WITH A LARGE ANGULAR DISTORTION [J].
DILWORTH, JR ;
HARRISON, SA ;
WALTON, DRM ;
SCHWEDA, E .
INORGANIC CHEMISTRY, 1985, 24 (17) :2594-2595
[8]   PREPARATION AND CRYSTAL AND MOLECULAR-STRUCTURE OF A TRIS(THIOBENZOYLDIAZENE)MOLYBDENUM COMPLEX - EXAMPLE OF DISTORTED TRIGONAL-PRISMATIC COORDINATION [J].
DILWORTH, JR ;
HYDE, J ;
LYFORD, P ;
VELLA, P ;
VENKATASUBRAMAMAN, K ;
ZUBIETA, JA .
INORGANIC CHEMISTRY, 1979, 18 (02) :268-274
[9]   THE CLEAVAGE OF THE N-N BOND OF N,N-DISUBSTITUTED HYDRAZINES ON RHENIUM - THE PREPARATION, REACTIONS AND X-RAY CRYSTAL-STRUCTURES OF [RECL2(NH3)(NNCOC6H4-4-R)(PPH3)2] (R = H, -OME, -NO2), [RECL3(NNPH2)(PPH3)2], [RECL2(N)(NNPH2)(PPH3)] AND [RECL(N)(ME2CNNCOPH)(PPH3)2] [J].
DILWORTH, JR ;
JOBANPUTRA, P ;
MILLER, JR ;
PARROTT, SJ ;
CHEN, Q ;
ZUBIETA, J .
POLYHEDRON, 1993, 12 (05) :513-522
[10]  
DILWORTH JR, 1982, CRYST STRUCT COMMUN, V11, P1135
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