PHOSPHORUS-SUBSTITUTED N,N'-DIMETHYLTHIOUREA COMPOUNDS .3. ASYMMETRICALLY BISPHOSPHORYLATED DERIVATIVES

被引:5
作者
GRUBER, M [1 ]
SCHMUTZLER, R [1 ]
SCHOMBURG, D [1 ]
机构
[1] GESELL BIOTECHNOL FORSCH MBH, MASCHERODER WEG 1, W-3300 BRAUNSCHWEIG, GERMANY
关键词
N; N'-DIMETHYLTHIOUREA; INTRAMOLECULAR P-P INTERACTION; FLUORIDE-ABSTRACTION; X-RAY;
D O I
10.1080/10426509308036894
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The unsymmetrically bisphosphorylated N,N'-dimethyl thiourea derivatives, 2, 3 and 5 were synthesized and investigated by H-1, C-13, F-19, and P-31 n.m.r. spectroscopy. It is concluded from the n.m.r. investigation that there is a phosphorus-phosphorus through-space interaction in these compounds. A single-crystal X-ray diffraction study conducted on N-(dimethylphosphino)-N'-(diphenylphosphino)-N,N'-dimethyl thiourea, 3 revealed a short non-bonding PP distance of 300 pm. Abstraction of a fluoride ion from Ph2P-N(Me)-C(:S)-N(Me)PF2, 2 with phosphorus pentafluoride has generated an unusual PP-bonded heterocyclic cation as a hexafluorophosphate salt, [Ph2P-N(Me)-C(:S)-N(Me)PF]+ PF6-, 8.
引用
收藏
页码:205 / 217
页数:13
相关论文
共 36 条
[1]   IMPROVED SYNTHESIS OF HALO-PHOSPHORUS(III) FLUORIDES [J].
ALBERS, W ;
KRUGER, W ;
STORZER, W ;
SCHMUTZLER, R .
SYNTHESIS AND REACTIVITY IN INORGANIC AND METAL-ORGANIC CHEMISTRY, 1985, 15 (02) :187-195
[2]   EXCHANGE-REACTIONS OF TETRAKIS(TRIFLUOROMETHYL)DIPHOSPHINE WITH PNICOGEN-PNICOGEN, PHOSPHORUS-HYDROGEN, AND PHOSPHORUS-CHLORINE BONDS [J].
AVENS, LR ;
CRIBBS, LV ;
MILLS, JL .
INORGANIC CHEMISTRY, 1989, 28 (02) :211-214
[3]   A NEW MODE OF FORMATION OF THE PHOSPHORUS PHOSPHORUS BOND - SYNTHESIS AND CRYSTAL-STRUCTURE DETERMINATION OF 1,5-DICHLORO-2,4-DIMETHYL-2,4-DIAZA-1,5-DIPHOSPHA-1,5-DIPHENYLPENTAN-3-ONE AND OF 1,4-DIMETHYL-2,3-DIPHENYL-1,4,3,2-DIAZADIPHOSPHOLIDIN-5-ONE-2-OXIDE AND ITS OXIDATION WITH TETRACHLOROORTHOBENZOQUINONED [J].
BETTERMANN, G ;
SCHMUTZLER, R ;
POHL, S ;
THEWALT, U .
POLYHEDRON, 1987, 6 (10) :1823-1831
[4]   VAN DER WAALS VOLUMES + RADII [J].
BONDI, A .
JOURNAL OF PHYSICAL CHEMISTRY, 1964, 68 (03) :441-+
[5]  
BREKER J, 1988, THESIS TU BRAUNSCHWE
[6]   DIFLUORODIMETHYLPHOSPHORUS(V) CATION [ME2PF2]+ [J].
BROWNSTEIN, M ;
SCHMUTZLER, R .
JOURNAL OF THE CHEMICAL SOCIETY-CHEMICAL COMMUNICATIONS, 1975, (08) :278-278
[7]   THE PREPARATION, STRUCTURES, AND REACTIONS OF 2-COORDINATE PHOSPHORUS CATIONS [J].
COWLEY, AH ;
CUSHNER, MC ;
LATTMAN, M ;
MCKEE, ML ;
SZOBOTA, JS ;
WILBURN, JC .
PURE AND APPLIED CHEMISTRY, 1980, 52 (04) :789-797
[8]   DERIVATIVES OF ACETAMIDE CONTAINING DIFLUOROPHOSPHINO-GROUPS [J].
EBSWORTH, EAV ;
RANKIN, DWH ;
STEGER, W ;
WRIGHT, JG .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1980, (09) :1768-1770
[9]   SOME DIPHOSPHINES AND TRIPHOSPHINES CONTAINING PF2-GROUPS [J].
EBSWORTH, EAV ;
HUTCHISON, DJ ;
MACDONALD, EK ;
RANKIN, DWH .
INORGANIC & NUCLEAR CHEMISTRY LETTERS, 1981, 17 (1-2) :19-21
[10]  
FERGUSSON JE, 1974, STEREOCHEMISTRY BOND, P176