109889-98-7Relevant academic research and scientific papers
Preparation and crystal structures of (1,1′-ruthenocenedithiolato-S,S′,Ru)(triphenylphosphine)-nickel(II) and (1,1′-metallocenedioxalato-O,O′,Fe-(or Ru))(triphenylphosphine)palladium(II): The metal (Fe or Ru)-metal (Pd or Ni) dative bond
Akabori, Sadatoshi,Kumagai, Takeshi,Shirahige, Toshio,Sato, Sadao,Kawazoe, Kayoko,Tamura, Chihiro,Sato, Masaru
, p. 2105 - 2109 (2008/10/08)
The reaction of 1,2,3-trithia[3](1,1′)ruthenocenophane with Ni(PPh3)4 in THF at room temperature gave [Ru(η5-C5H4S)2]NiPPh 3, although [Fe(η5-C5H4S)2]NiPPh3 could not be obtained in a similar reaction between Ni(PPh3)4 and 1,2,3-trithia[3](1,1′)ferrocenophane. [Fe(η5-C5H4O)2]PdPPh3 and [Ru(η5-C5H4O)2]PdPPh3 were obtained by the reaction of the disodium salt of the metallocenediols (M = Fe or Ru) with Pd(PPh3)2C12 in 28% yield. Palladium complexes could not be obtained via analogous methods. [Ru(η5-C5H4S)2]-NiPPh 3·1/2C6H5CH 3 crystallizes in the monoclinic space group C2/c with Z = 8 and unit cell parameters a = 39.036 (7) A?, b = 10.463 (2) A?, c = 13.793 (4) A?, and β = 102.03 (2)°. The structure was refined to give R = 3.7 % using 3840 independent reflections with Fo ≥ 2σ(Fo). [Ru(η5-C5H4O)2]PdPPh3 crystallizes in the monoclinic space group P21/n with Z = 4 and unit cell parameters a = 11.022 (6) A?, b = 14.872 (10) A?, c = 14.454 (5) A?, and β = 99.14 (3)°. The structure was refined to R = 3.9% using 3699 independent reflections with Fo ≥ 2σ(Fo). X-ray crystal data showed that [Ru(η5-C5H4O)2]PdPPh3 and [Fe(η5-C5H4O)2]PdPPh3 are isomorphous. The distances between the metal-metal and the large chemical shifts between the α- and β-ring protons in the 1H NMR spectra of their complexes provide for appreciable evidence of Ru-Pd (or Fe-Pd and Ru-Ni) dative bonding.
