Organoimido complexes of tungsten and rhenium: Oxo-imido and bis-imido complexes of tungsten(VI), and phenylimido complexes of rhenium(VI) and (V). The X-ray crystal structures of [W(NCMe3)(NPh)Cl2(bipy)] and [Re(NPh)Cl3(NH2CMe3)2]
作者:George R. Clark、Alastair J. Nielson、Clifton E.F. Rickard
DOI:10.1016/s0277-5387(00)80456-8
日期:——
2′-bipyridyl (bipy) gives [W(NCMe3)2Cl2(bipy)] and insoluble oxo complexes. Reaction of WOCl4 with p-MeC6H4N(SiMe3)2 and then bipy gives [W(NC6H4Me-p)2Cl2(bipy)] and [W(O)(NC6H4Me-p)Cl2(bipy)]; [W(NPh)Cl4]2 reacts with p-MeC6H4N(SiMe3)2 and then bipy to give [W(NPh)(NC6H4Me-p)Cl2(bipy)]. [W(NCMe3)(μ-NPh)Cl2(NH2CMe3)]2 and bipy give [W(NCMe3)(NPh)Cl2(bipy)] (6). ReOCl4 reacts with PhNCO to give [Re(NPh)Cl4]x
MnO3Cl is prepared from KMnO4 und ClSO3H. The thermally very unstable compound is identified by its Raman spectrum and a single crystalstructure determination: a = 715.4(5), b = 1008.3(7), c = 500.9(4) pm, space group Cmc21. Solid MnO3Cl consists of molecules with only weak intermolecular interactions. The M–Cl bond length is 209.9(4) pm. The crystalstructure is compared to those of MnO3F, CrO2Cl2
Improved syntheses of tetrachloro-oxorhenium(<scp>VI</scp>) and chlorotrioxo-rhenium(<scp>VII</scp>). Synthesis of alkoxo- and dialkylamido-rhenium com-pounds. The crystal and molecular structures of di-µ-methoxo-tetramethoxo-µ-oxo-dioxodirhenium(<scp>VI</scp>)(Re–Re), bis[lithium pentaiso-propoxo-oxorhenate(<scp>VI</scp>)–lithiumchloride–tetrahydrofuran(1/1/2)], and trans-tetraphenoxobis(trimethylphosphine)rhenium(<scp>IV</scp>)
作者:Peter G. Edwards、Geoffrey Wilkinson、Michael B. Hursthouse、K. M. Abdul Malik
DOI:10.1039/dt9800002467
日期:——
interaction with phenol in the presence of trimethylphosphine leads to the compound trans-Re(OPh))4(PMe3)2, (C), while with lithium bis (trimethylsilyl)-amide a unique four-co-ordinate rhenium(V) compound, ReON(SiMe3)2}3, is obtained. The crystal and molecularstructures of (A)–(C) have been determined by X-ray crystallography. Compound (A) is monoclinic, space group P21/n, a= 12.142(1), b= 15.369(1)