MIXED ALKOXIDE-ANILIDE D3-D3 DIMERS OF MOLYBDENUM AND TUNGSTEN - THE X-RAY CRYSTAL-STRUCTURES OF M2(OBU-TERT)4(HNPH)2(H2NPH)2 (M = MO, W)

被引:8
作者
CHISHOLM, MH [1 ]
PARKIN, IP [1 ]
STREIB, WE [1 ]
FOLTING, KS [1 ]
机构
[1] INDIANA UNIV,CTR MOLEC STRUCT,BLOOMINGTON,IN 47405
关键词
D O I
10.1016/S0277-5387(00)86155-0
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The reactions in diethyl-ether/hexane solutions between aniline and M2(OBut)6 (M = Mo, W) produce M2(OBut)4(HNPh)2(H2NPh)2 in high yield (79-85%) as red-black crystals. The compounds are air-sensitive, soluble in aromatic hydrocarbon solvents, and exhibit dynamic NMR behaviour. The IR spectra show nu(N-H) at 3320 and 3100 cm-1, corresponding to aniline and anilide N-H stretches, respectively. The X-ray crystal structures of M2(OBut)4(HNPh)2(H2NPh)2 are isomorphous for molybdenum and tungsten and reveal eclipsed four-coordinate, essentially planar ends supporting a metal-metal triple bond. Some important bond lengths and angles for W2(OBut)4(HNPh)2(H2NPh)2 (Mo2(OBut)4(NHPh)2(NH2Ph)2 in parentheses) are as follows (at - 169-degrees-C and - 168-degrees-C): M-M 2.3225(8) [2.2538(7)], M-O = 1.93 (1.94) (ave), 1.98 (1.96) (ave), M-N (amide) 1.97 (ave) [1.99 (ave)], M-N (amine) 2.37 angstrom (ave) [2.36 angstrom (ave)].
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页码:2309 / 2316
页数:8
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