Polynuclear nitrosyl carbonyl ReI complexes with thiolate and sulfide bridges |
| |
| Authors: | S E Nefedov A A Sidorov H Berke I L Eremenko |
| |
| Institution: | (1) N. S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, 31 Leninsky prosp., 117907 Moscow, Russian Federation;(2) Institute of Inorganic Chemistry, Zurich University, 190 Winterthurer Strasse, CH-8057, Zurich, Switzerland |
| |
| Abstract: | The reaction of the complex Re2(CO)4(NO)2Cl4 (1) with NaSCMe3 (2) (in THF or MeCN, 65–80°C, 24 h) was studied at different ratios of the reagents (from 1∶2 to 1∶6). At the reagent ratio
of 1∶2, the binuclear complex Re2(CO)4(NO)2Cl2(μ-SCMe3)2 (3) was obtained as a mixture ofsyn andanti isomers (3a and3b, respectively) containing Re2S2 fragments with different structures (the butterfly-like structure in3a and the planar fragment in3b). When the initials were taken in ratios from 1∶4 to 1∶6, two compounds were isolated: the binuclear complex Re2(CO)4(NO)2(μ-SCMe3)2(μ-S)4 (cocrystallized as a mixture ofsyn andanti isomers,4a and4b, respectively) and the triangular cluster Re3(CO)3(NO)3(μ-SCMe3((μ3-S)(μ3-Cl) (5). Apparently, complex4 is formed in the course of isolation as a result of elimination of SR2 from the unstable tetrathiolate dimer Re2(CO)4(NO)2(SCMe3)2(μ-SCMe3)2 (6). Cluster5 is the product of the reaction between compounds3 and4. Products of interaction of compound6 with silica gel upon column chromatography of the reaction mixture were studied. Four complexes containing hydroxy and oxo
bridging groups, (CO)2(NO)Re(μ-SCMe3)2(μ-OH)Re(SCMe3)(CO)(NO) (7), (CO)3(NO)3RE3(μ-SCMe3)3(μ3-SCME3)(μ3-O) (8), (CO)2(NO)2Re2(SCMe3)2(μ-SCMe3)2(μ-OH)]Na(THF)(Et2O)] (9), and (CO)2(NO)2Re2(SCMe3)2(μ-SCMe3)2(μ-OH)]2−Na(H2O)6]H5O2] (10), were isolated. The structures of complexes3, 4, 5, 7, 8, 9, and10 were established by X-ray diffraction study.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 1030–1044, May, 1998. |
| |
| Keywords: | rhenium complexes rhenium clusters nitrosyl ligands thiolate and sulfide bridges X-ray analysis |
| 本文献已被 SpringerLink 等数据库收录！ |
|
