Ruthenium compounds analysis

When carried out in refluxing xylene, the above reaction also produces (C8H8)Ru2(CO)a (55) for which the spectral data suggest (55, 141) a structure in solution identical to that of the iron analog (126). The ruthenium compound does not appear to undergo the isomerization in solution demonstrated by the iron compound (332). A preliminary X-ray analysis (141, footnote 1 la) establishes, however, that in the solid state the complex does not have the structure (126) in that there is no symmetry plane and the Ru-Ru bond is nearly perpendicular to the direction of that suggested for the Fe-Fe bond. 

The chemical structure of the polymers was confirmed by NMR and elemental analysis, and spectroscopically characterized in comparison with monodisperse low molecular weight model compounds. Scheme 5 outlines the approach to the model compounds. Model compounds 31-34 were synthesized by complexation of the ruthenium-free model ligands 29/30 with 3/4. The model ligands were synthesized in toluene/diisopropylamine, in a similar fashion as the polycondensation using Pd(PPh3)4 and Cul as catalyst (Sonogashira reaction) [34,47-49]. 

Ruthenium and its compounds are analyzed by flame AA method using nitrous oxide-acetylene flame. ICP-AES, ICP/MS, and neutron activation analysis are also applicable. The metal or its insoluble compounds may be solubilized by fusion with alkah and leached with water. 

The metallacyclopentanes 55d and 55e were characterised by elemental analysis, mass spectrometry, IR, H and 13C NMR.55 57 In general, the osmium compounds were found to be much more stable than their ruthenium analogues,60 both decompose on heating to give cis- and trans-2-butenes, and in the presence of CO... 

This type of receptor is represented by compounds 16a,b bearing ruthenium ) bipyridine moieties. Both calixarenes [18] exhibit 1 1 binding of chloride and bromide anions (DMSO-d6), and they are especially suitable for the complexation of H2POj (X16a=2.8-104 M-1 K16b=5.2 103 M"1). On the other hand, if we compare these results with those for similar non-calixarene receptors, where the bipyridine unit is substituted by alkyl, aryl or ethylene glycol substituents, the introduction of calixarene does not bring any substantially new features into the complexation abilities of these derivatives. As shown by X-ray analysis, the anion is encapsulated within the cavity formed by amidic functions with the contributions of CH...anion interactions from the bipyridine unit. 

Although the third structure type was established for ruthenium pentafluoride (88), the results were based on restricted single-crystal data, giving less accurate molecular dimensions. Full data were used for the structure analysis of the osmium compound (89 ) but the results were still unsatisfactory, because of the predominant scattering by the... 

Winter and co-workers used the proton NMR spectra of niobium(v) complexes with 5-phenyltetrazolate ligand recorded at temperatures between —80 and +40°C in toluene-structural analysis <2001IC6451>. One- and two-dimensional 111 NMR methods in solution and solid state were used for analyzing the structure of irbesartan 83 <1998J(P2)475> as well as for the analysis of the structure of coordination compounds of ruthenium(n) and iron(n) with 5-aryltetrazolates <2002OM3774, 2003JOM(669)135, 2006IC695>. 

Complex 125 in which one phenyl group of BPh4 is it bonded to ruthenium, has been synthesized in low yield (20%) by reaction of compound 129 with sodium tetraphenylborate in boiling methanol (80,81) [Eq. (12)]. The zwitterionic structure has been confirmed by X-ray structural analysis (82). 

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