The reaction of CpRu(PPh3)2+ with organic thiols. Synthesis and characterization of [CpRu(PPh3)2(RSH)]BF4 (R=benzyl, phenethyl) and the molecular and crystal structure of [CpRu(PPh3)2(C6H5CH2CH2SH)]BF4·CH2Cl2

Park, Haengsoon; Minick, David; Draganjac, M.; Cordes, A. W.; Hallford, Randal; Eggleton, Gordon L.

doi:10.1016/s0020-1693(00)82925-4

Cited by 13 publications

(12 citation statements)

References 19 publications

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“…3; see also structural and NMR and discussions above and below, respectively), bridging hydrogen atoms were apparent between B(7) and B (8), and between B(8) and B (9). Overall, the NMR parameters measured for 3 are in clear parallel to the corresponding parameters reported for the closely related and previously characterised {Ru(C 6 Me 6 )} analogue, 8 11 B and 1 H NMR spectra consistent with the molecular plane of symmetry (Fig. 3).…”

Section: Nmr Spectroscopysupporting

confidence: 66%

“…For [5-(p-cym)-arachno-5,4,6-RuS 2 B 6 H 8 ] 3, as with compound 1 above, the mirror-plane symmetry is manifest in the relative intensity patterns for the cluster 11 B and 1 H resonances. The assignment of the bridging hydrogen resonances to their positions, as summarized in the experimental section, is noteworthy.…”

Section: Nmr Spectroscopymentioning

confidence: 82%

“…It is not possible to choose between these descriptions on the basis of the evidence from the solid state structure analysis or the NMR spectroscopic results, vide infra. Comparison of the Ru-S distances in 1, of 2.3978( 14) and 2.3941(15) A ˚, with Ru-S distances in coordination compounds such as the bidentate xanthate derivative [Ru(g 2 -S 2 CSPr n )(PPh 3 )(g 5 -Cp)] at 2.374(4) and 2.362(2) A ˚,14 or monodentate sulfur-ligand species such as [Ru(C 3 H 6 S)(PPh 3 ) 2 (g 5 -Cp)][CF 3 SO 3 ] at 2.3459(20) A ˚10 and [Ru(PhCH 2 CH 2 SH)(PPh 3 ) 2 (g 5 -Cp)][BF 4 ] at 2.369(2) A ˚}, 11 and in the arachno cluster [(g 6 -C 6 Me 6 )-arachno-5,4,6-RuS 2 B 6 H 8 ] 9 at 2.369(2) and 2.367(2) A ˚,8 shows the distances in 1 are somewhat longer. However, the distance in 1 is similar to that in [Ru(C 6 H 11 SH)(PPh 3 ) 2 (g 5 -Cp)][BF 4 ] at 2.389(2) A ˚12 and the compound [Ru(g 1 -1,2-S 2 B 6 H 9 )(PPh 3 ) 2 (g 5 -Cp)] 2 at 2.4021(9) A ˚.…”

Section: Crystal and Molecular Structuresmentioning

confidence: 99%

“…Salient points of comparison or of other interest are summarized in the following three paragraphs. For all compounds it may be noted that there was a general absence of [ 11 B- 11 B] correlations between pairs of boron atoms flanked by heteroatoms or by hydrogen bridges. This is a well-recognized phenomenon, and signifies a smaller coupling 1 J( 11 B-11 B) for such environments, and is consistent with the longer interboron distances often observed for these positions, and therefore weaker direct interboron bonding, and concurs with the structural discussion section above.…”

Section: Nmr Spectroscopymentioning

confidence: 99%

“…The phenomenon is categorised by Heřmáneks 'l-H Rule , 17 and is classically manifested in the ca. 30 ppm difference in 11 B shielding at the B(2) and B(4) positions when nido-B 10 H 14 and the [arachno-B 10 H 14 ] 2− anion are compared. In the more directly relevant ninevertex arachno system, the phenomenon is exhibited by the [arachno-B 9 H 14 ] − anion itself, which exhibits both types of site.…”

Section: Nmr Spectroscopymentioning

confidence: 99%

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Coordination and cluster compounds of ruthenium with the [hypho-1,2-S2B6H9]– ligand

Ferguson¹,

Gallagher

Kennedy

et al. 2005

Dalton Trans.

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The reaction between [tmndH][hypho-1,2-S(2)B6H9](tmnd =N,N,N',N'-tetramethylnaphthalene-1,8-diamine) and [RuCl(PPh3)2(eta5-Cp)] in CH2Cl2 at room temperature afforded two ruthenathiaboranes, [5-(eta(5)-Cp)-5-(PPh3)-5,4,6-RuS2B6H9], 1, and [Ru(eta(1)-1,2-S2B6H9)(PPh3)2(eta5-Cp)], 2, in 6 and 48% yields, respectively. The heating of a solution of [Ru(eta(1)-1,2-S2B6H9)(PPh3)2(eta5-Cp)] 2 in CH2Cl2 at reflux temperature afforded 1 in 59% yield. Compound 1 could be described as either a hypho nine-vertex {RuS2B6} cluster or a coordination compound of ruthenium which contains a bidentate eta2-dithiaborate cluster ligand; the latter description is preferred. Compound 2 contains an eight-atom hypho-type {1,2-S2B6} cage bonded to the ruthenium atom of the {Ru(PPh3)2(eta5-Cp)} unit by one sulfur atom and may be described as a compound of ruthenium coordinated eta(1)- to the dithiaborate cluster ligand. The reaction between [tmndH][hypho-1,2-S2B6H9] and [RuCl2(eta6-MeC6H4Pri)]2 in CH2Cl2 at room temperature afforded [5-(eta6-MeC6H4Pri)-arachno-5,4,6-RuS2B6H8], 3, in 94% yield. Further reaction of 3 and PMePh2 afforded another arachno{RhS2B6}cluster, [5-(eta6-MeC6H4Pri)-8-(PMePh2)-arachno-5,4,6-RuS2B6H6], 4, in 25% yield. Compounds 1, 2, and 4 were characterised with single crystal X-ray analyses.

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