Synthesis and reactivity of Ru-, Os-, Rh-, and Ir-halide-sulfoxide complexes.

The chemistry of binuclear palladium(II) and platinum(II) complexes

Two families of mixed-ligand osmium(II) complexes, namely trans,cis,cis-[OsIICl2(azole)2(dmso)2] [azole = indazole (1), pyrazole (2), benzimidazole (3) and imidazole (4)] and cis,fac-[OsIICl2(azole)(dmso)3] [azole = indazole (5), pyrazole (6), benzimidazole (7) and imidazole (8)] have been prepared by taking advantage of the destabilising trans effect of the S-bonded dmso ligands. These complexes have been characterised by microanalysis, IR, UV/Vis, 1H and 13C NMR spectroscopy, electrospray mass spectrometry, cyclic voltammetry and X-ray crystallography. They have been found to catalyse the hydration of trichloroacetonitrile to trichloroacetamide and dichloroacetonitrile to dichloroacetamide with high selectivity. The catalyst efficiency depends strongly on the nature of the complex and the azole ligand present. The highest turnover (TON of 412 for trichloroacetamide and 578 for dichloroacetamide) and product yield (82.7 % for trichloroacetamide and 75.3 % for dichloroacetamide) have been achieved with complex 7. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007)

The Complexes [OsCl2(azole)2(dmso)2] and [OsCl2(azole)(dmso)3]: Synthesis, Structure, Spectroscopic Properties and Catalytic Hydration of Chloronitriles

Publisher Summary This chapter discusses the aspects of the coordination chemistry of organoantimony ligands and antimony ligands free of substituents without the inclusion of the other pnicogens. The ligand systems discussed include tertiary stibines, R 3 Sb and R 2 Sb, RSb or Sb units in different environments and with various coordination patterns. The majority of the complexes involve coordination on transition metals but complexes with main group (including Sb) acceptors are also discussed. General features of organoantimony ligands compared with their lighter congeners are related to the low stability of Sb–C or Sb–Sb bonds, to the relative weak Lewis basicity and to a larger tendency for higher coordination. Several comparative studies reveal a higher reactivity and flexibility of antimony ligand systems compared to analogous P or As compounds. However, the differences between related antimony and bismuth ligands appear to be considerably larger. Many tertiary stibines have donor properties similar to phosphines or arsines and they are easily coordinated witha large variety of metal complex fragments, whereas bismuthines are often weak donors. X-ray diffractometry is a very useful tool for the study of antimony ligands, including labile systems which are protected from rapid decomposition only in the sphere of complex.

n Ligands Coordination Compounds with Organoantimony and Sbn Ligands

The kinetics and mechanism of the reaction between [PtI3(AsPh3)](-) and pyridine in acetonitrile solvent has been studied by use of stopped-flow spectrophotometry. Substitution of iodide trans to arsine is irreversible under the conditions used and takes place via parallel direct and solvolytic pathways. By comparing the rate constants of the direct pathway with literature values of the corresponding phosphine and stibine complexes the following trans effect series can be obtained: Ph3Sb > Ph3P > Ph3As. The crystal and molecular structures of reactant and product have been determined. Based on Pt-I distances for the investigated arsine complex and literature data for the corresponding phosphine and stibine complexes the following trans influence series was derived: Ph3P greater than or equal to Ph3As > Ph3Sb. To the best of our knowledge this is the first comparison of all the three heavier pnictogens as donor atoms using strictly analogous complexes with identical cis-ligands.

The trans effect and trans influence of triphenyl arsine in platinum(II) complexes. A comparative mechanistic and structural study

The reaction of [Ru(dmf)6][CF3SO3]3, LiX and Ph2SbCH2SbPh2 (dpsm) yielded trans-[RuX2(η1-dpsm)4] (X = Cl or Br) or [RuI2(η1-dpsm)2(η2-dpsm)]. The latter was shown by an X-ray study to contain two monodentate and one chelating dpsm ligands and is the first example with any metal of a distibinomethane acting as a chelate to be authenticated crystallographically. The chelate ring is highly strained as shown by the Sb–Ru–Sb angle (74.3°) and the longer Ru–Sb distances than in the η1-ligands. Corresponding reactions of trans-[OsX2(dmso)4] and dpsm produced trans-[OsCl2(η1-dpsm)4] and [OsBr2(η1-dpsm)2(η2-dpsm)] identified spectroscopically. The reactions of RhX3 (X = Cl, Br or I) with dpsm afford [RhX3(dpsm)2] which on the basis of NMR spectroscopic data contain one chelating and one monodentate dpsm ligand. Palladium(II) and platinum(II) halides form both 1∶1 and 1∶2 complexes with dpsm. The former are dimeric and crystal structures of [M2X4(dpsm)2] (M = Pt, X = Cl or Br; M = Pd, X = Br) revealed a distibine bridged structure with square-planar MX2Sb2 metal centres, one with a cis geometry, the other trans. The structures cis,trans-[X2M(μ-dpsm)2MX2] are the first examples of this geometry to be established crystallographically. In contrast [I2M(μ-dpsm)2MI2] are assigned as trans,trans isomers on the basis of spectroscopic data. Multinuclear NMR studies show that [PtX2(dpsm)2] (X = Cl or Br) contain η1-dpsm and are a mixture of cis and trans isomers in solution, but the [PtI2(dpsm)2] contains only a single form, probably the trans isomer. The [PdX2(dpsm)2] have also been characterised and for X = Cl shown to undergo facile fragmentation in solution to form trans,trans-[Pd2Cl2(σ-Ph)2(dpsm)2]. The complexes [M(L–L)2]Y (M = Cu, Ag or Au; Y = BF4 or PF6; L–L = dpsm or Me2SbCH2SbMe2) and [Rh2Cl2(CO)2(μ-L–L)2] have also been prepared. All complexes have been characterised by analysis, IR, UV-VIS, multinuclear NMR (1H, 13C-{1H}, 195Pt, 63Cu and 109Ag) spectroscopies as appropriate. Comparisons are drawn between the various co-ordination modes of the distibines and those of Ph2PCH2PPh2 and related ligands.

Synthesis, properties and structures of complexes of platinum metal halides and Group 11 metals with two distibinomethane ligands, R2SbCH2SbR2 (R = Me or Ph)

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Synthesis, properties and structures of complexes of platinum metal halides and Group 11 metals with two distibinomethane ligands, R2SbCH2SbR2 (R = Me or Ph)