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In order to study the properties of sulfur coordinated metal centres, the chromium and tungsten complexes [Cr(NO)(µ-′S 4 ′)] 2  (4), (NR 4 ) 2 [W(NO) 2 (′S 2 ′) 2 ] (1) (R = Me (la), n-Bu (lb)), [W(NO) 2 (′S 4 ′)] (2), [µ-O{W(NO)(′S 4 ′)} 2 ] (3) and [W(NPR 3 )(NO)(′S 4 ′)] (5) (R = Me (5a), Et (5 b)) were synthesized (′S 2  ′2-  = 1.2-benzenedithiolate(2-); ′S 4  ′2-  = 1.2-bis(2-mercaptophenylthio)ethane(2-)). la and lb result from the reductive nitrosylation of Li 2 [W(′S 2 ′) 3 ] which was prepared by reduction of [W(′S 2 ′) 3 ] with n-BuLi. la was also obtained from [W(NO) 2 (Cl) 2 ] n , ′S 2  ′2-  and NMe 4  + . Alkylation of la or lb by 1.2-dibromoethane yields 2, whose X-ray structure analysis shows that W is pseudooctahedrally coordinated by two trans thiolato S, two cis thioether S and two cis N atoms of linear W-NO groups. 2 was also obtained from [W(NO) 2 (CH 3 CN) 4 ](BF 4 ) 2  or [W(NO) 2 (Cl) 2 ] n  and ′S 4  ′2- -. The reaction of [W(NO) 2 (Cl) 2 ] n  yielded the dinuclear oxo-bridged complex 3 as a by-product in small amounts. In preparative amounts, 3 was synthesized by hydrolysis of [W(Cl)(NO)(′S 4 ′)]. In contrast to the analogous Mo complex, 2 does not react with N 2 H 4 ; with the ligands PMe 3  and PEt 3 , it gives the corresponding phosphiniminato complexes 5 and free phosphineoxides OPR 3 . In order to compare the [M(NO) 2 (′S 4 ′)] complexes (M = Cr, Mo, W), the structure of [Cr(NO) 2 (′S 4 ′)] was determined by X-ray structure analysis. The Cr complex exhibits the same molecular coordination geometry as 2. While growing crystals of [Cr(NO) 2 (′S 4 ′)], the dinuclear Cr complex 4 was also formed. Its X-ray structure analysis shows each of the Cr centres to be coordinated pseudooctahedrally by five sulfur donors and one nitrosyl N donor. 4 was also obtained by the reaction of [Cr(CO) 4 (nor)] with ′S 4  ′2-  and NOBF 4 .

zeitschrift für naturforschung b

Übergangsmetallkomplexe mit Schwefelliganden, LXI / Transition Metal Complexes with Sulfur Ligands, LXI: Chrom- und Wolfram-Nitrosyl-Komplexe mit schwefeldominierten Koordinationssphären: [Cr(ΝO) x (′S 4 ′)] y , (x = 1, y = 2; x = 2, y = 1), (NR 4 ) 2 [W(NO) 2 (′S 2 ′) 2 ] (R = Me, n-Bu), [W(L)(ΝO)(′S 4 ′)](L = NO, NPMe 3 , NPEt 3 ) und [µ-O{W(NO)(′S 4 ′)} 2 ](′S 2  ′2-  = 1,2-Benzoldithiolat(2–); ′S 4  ′2  = 1,2-Bis(2-mercaptophenylthio)ethan(2–)); Synthesen, Eigenschaften und Röntgenstrukturanalysen / Chromium and Tungsten Nitrosyl Complexes with Sulfur Dominated Coordination Spheres: [Cr(NO)x(′S 4 ′)] y  (x = 1,y = 2; x = 2,y = 1), (NR 4 ) 2 [W(NO) 2 (′S 2 ′) 2 ] (R = Me, n-Bu), [W(L)(NO)(′S 4 ′)] (L = NO, NPMe 3 , NPEt 3 ) and [µ-O{W(NO)(′S 4 ′)} 2 ] (′S 2  ′2  = 1.2-Benzenedithiolate(2–); ′S 4  ′2  = 1.2-Bis(2-mercaptophenylthio)ethane(2–)); Syntheses, Properties and X-Ray Structure Analyses