Cyclic S---N compounds and phosphorus reagents—XV [1]. Synthesis, spectral and X-ray structural characterization of (Ph)(DCA)(R)P=N---S3N3 [R=(C2H5)2N—; (n-C4H9)
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- 作者：Gopalakrishnan ; Janarthanan ; Sudheendra Rao ; M. N. ; Srinivas ; Janaswamy ; Srinivasamurthy ; G.
- 关键词：asymmetric phosphines ; phosphiniminocyclotrithiazenes ; synthesis ; spectra ; X-ray structure
- 刊名：Polyhedron
- 出版年：1997
- 出版时间：January 23, 1997
- 年：1997
- 卷：16
- 期：7
- 页码：1089-1094
- 全文大小：358 K
文摘
Room-temperature reactions of asymmetric phosphines, (Ph)(DCA)(R)P (R = Et2N--, Bun2N--) with S4N4 in acetonitrile afforded phosphiniminocyclotrithiazenes, (Ph)(DCA)(R)P
N--S3N3 (R = Et2N--,I ; Bun2N--, II) in modest yields (ca 50 % ). The heterocycles have been characterized by spectroscopic [IR, UV- vis, NMR (1H and 31P) and mass] and single crystal X-ray diffraction methods. Strikingly, the angle at P--N(4)--S(1) is 135° in I, the largest observed so far and is 119.3° in II. This is also accompanied by the shortest exocyclic S(1)--N(4) bond length of 1.537 Å observed in the case of I. In the unit cell of II, two types of molecules with slightly differing degree of deviation of the tricoordinate sulfur (0.664 and 0.673 Å from the mean plane [N(1)--S(2)--N(2)--S(3)--N(3)] are observed.
N--S3N3 (R = Et2N--,I ; Bun2N--, II) in modest yields (ca 50 % ). The heterocycles have been characterized by spectroscopic [IR, UV- vis, NMR (1H and 31P) and mass] and single crystal X-ray diffraction methods. Strikingly, the angle at P--N(4)--S(1) is 135° in I, the largest observed so far and is 119.3° in II. This is also accompanied by the shortest exocyclic S(1)--N(4) bond length of 1.537 Å observed in the case of I. In the unit cell of II, two types of molecules with slightly differing degree of deviation of the tricoordinate sulfur (0.664 and 0.673 Å from the mean plane [N(1)--S(2)--N(2)--S(3)--N(3)] are observed.