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1995 (1)
1987 (1)
1Author    Dieter Sellmann, Gerhard BinkerRequires cookie*
 Title    Übergangsmetall-Komplexe mit Schwefelliganden, XXVII* Synthese und Reaktivität der Nitrosyl-und Nitrido-Ruthenium-Komplexe mit 1,2-Benzoldithiolat-Liganden [Ru(NO)(S 2 C 6 H 4 ) 2 r bzw. [Ru(N)(S 2 C 6 H 4 ) 2 r Transition Metal Complexes with Sulfur Ligands, XXVII* Synthesis and Reactivity of the Nitrosyl-and Nitrido-Ruthenium Complexes with 1,2-Benzenedithiolate Ligands [Ru(NO)(S 2 C 6 H 4 ) 2 ]~ and [Ru(N)(S 2 C 6 H 4 ) 2 ]~, Respectively  
 Abstract    The reaction of [Ru(NO) 2 (PPh 3) 2 ], [RuCl(NO) 2 (PPh 3) 2 ]PF 6 or [RuCl 3 (NO)(PPh 3) 2 ] with 1,2-benzenedithiolate(—2), C 6 H 4 S 2 : ~, leads to the 16e"-complex [Ru(NO)(S 2 C 6 H 4) 2 ]~, which was isolated as the NBu 4 + salt (1). The square pyramidal anion in [NBu 4 ][Ru(NO)(S 2 C 6 H 4) 2 ] coordi-nates PMe 3 with rearrangement of the sulfur ligands to give the six-coordinate cis-[NBu 4 ][Ru(NO)(PMe 3)(S 2 C 6 H 4) 2 ] (3); the rearrangement of the C 6 H 4 S 2 2 "-ligands from trans to eis coordination is proved by 13 C NMR spectroscopy. [Ru(NO)(S 2 C 6 H 4) 2 ]~ is rapidly reduced even under mild conditions. Reaction of 1 with NaBH 4 in MeOH leads to the reduction of NO to a nitrido ligand and the concomitant oxidation of (formal) Ru(III) to Ru(VI) yielding [NBu 4 ][Ru(N)(S^C 6 H 4)->] (2). This compound is also formed when the nitrosyl complex is reacted with SiMe 3 N 3 . [Ru(NO) 2 (PPh 3) 2 ] and [RuCl(NO) 2 (PPh 3) 2 ]PF 6 are denitrosylatedby dttd 2 ~ (dttd 2 " = 2,3,8,9-dibenzo-l,4,7,lÖ-tetrathiadecane(—2)) to give [Ru(dttd)(PPh 3) 2 ], 
  Reference    Z. Naturforsch. 42b, 341—347 (1987); eingegangen am 10. November 1986 
  Published    1987 
  Keywords    Ruthenium Sulfur Complexes, Synthesis, Reactions 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0341.pdf 
 Identifier    ZNB-1987-42b-0341 
 Volume    42 
2Author    Dieter Sellmann, Christine Rohm, Matthias Moll, Herrn Professor, H. P. FritzRequires cookie*
 Title    Protonierung und Alkylierung der  
 Abstract    Thiolatdonoren von Ru(II)-Komplexen mit [Ru(,buS5')]-Fragmenten ('buS5,-H 2 = 2,2'-Bis(2-mercapto-3,5-di-/-butylphenylthio)diethylsulfid) Transition Metal Complexes with Sulfur Ligands, CXV+. Protonation and Alkylation of Thiolate Donors in Ru(II) Complexes with [Ru('buS5')] Fragments ('buS5'-H 2 = 2,2'-Bis(2-mercapto-3,5-di-t-butylphenylthio)diethylsulfide) Reaction of meso-[Ru(L)(,buS5')] complexes (L = CO (1), PPh3, PCy3) with one equivalent of oxonium salts R3OBF4 (R = CH3, C2H5) yields the C, symmetrical monoalkyl derivatives [Ru(L)('buS5'-R)]BF4 (L = CO, R = CH3 (2), C2H5 (3); L = PPh3, R = CH3 (5); L = PCy3, R = CH3 (6)), in which one of the thiolate donors of the starting complexes is alkylated diastereospecifi-cally. Monoalkylation of the binuclear complex [Ru('buS5')]2 leads to Q symmetrical [Ru('buS5'-CH3)]2(BF4)2 (7) which gives the hydrazine complex [/i-N2H4{Ru('buS5'-CH3)}2](BF4)2-N2H4 (9) upon reaction with N2H4. Reaction of 1 with 1.5 equivalents of CF3S 03H yields the isolable thiol complex [Ru(CO)('buS5'-H)]CF3SOy0.5 CF3S03H (4). The 'H-NMR spectra are temperature-depen­ dent and indicate exchange of the thiol proton between the thiolate donors of the ,bus 5'2-ligand. Twofold protonation of 1 could only be proved IR-spectroscopically, dialkylation of 1, however, yields isolable [Ru(CO)('buS5'-(CH3)2)](BF4)2 (8) as a mixture of diastereomers. The IR stretching frequencies i/(CO) of the CO complexes indicate that the electron densities at the ruthenium centers are decreased and the Ru-L bonds are weakened. However, the ligands L in the [Ru(L)('buS5'-R)]BF4 complexes do not exchange more readily than in the parent complexes. Ubergangsmetallkomplexe mit Schwefelliganden, CXV+. 
  Reference    Z. Naturforsch. 50b, 1729—1738 (1995); eingegangen am 2. Mai 1995 
  Published    1995 
  Keywords    Ruthenium Sulfur Complexes, Alkylation, Protonation 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1729.pdf 
 Identifier    ZNB-1995-50b-1729 
 Volume    50