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

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

Electrospray mass spectrometry: a tool for elemental speciation

Rhodium is used for a number of large processes that rely on homogeneous rhodium-catalyzed reactions, for instance rhodium-catalyzed hydroformylation of alkenes, carbonylation of methanol to acetic acid and hydrodesulfurization of thiophene derivatives (in crude oil) Many laboratory applications in organometallic chemistry and catalysis involve organorhodium chemistry and a wealth of rhodium coordination compounds is known For these and other areas, 103Rh NMR spectroscopy appears to be a very useful analytical tool In this review, most of the literature concerning 103Rh NMR spectroscopy published from 1989 up to and including 2003 has been covered After an introduction to several experimental methods for the detection of the insensitive 103Rh nucleus, a discussion of factors affecting the transition metal chemical shift is given Computational aspects and calculations of chemical shifts are also briefly addressed Next, the application of 103Rh NMR in coordination and organometallic chemistry is elaborated in more detail by highlighting recent developments in measurement and interpretation of 103Rh NMR data, in relation to rhodium-assisted reactions and homogeneous catalysis The dependence of the 103Rh chemical shift on the ligands at rhodium in the first coordination sphere, on the complex geometry, oxidation state, temperature, solvent and concentration is treated Several classes of compounds and special cases such as chiral rhodium compounds are reviewed Finally, a section on scalar coupling to rhodium is provided Copyright © 2004 John Wiley & Sons, Ltd

103Rh NMR spectroscopy and its application to rhodium chemistry.

The rhodium(III) complex mer,cis-[RhCl3(PPh2py-P,N)(PPh2py-P)] (1) (PPh2py = diphenyl (2-pyridyl)phosphine) has been prepared from RhCl3·3H2O and PPh2py and converted to the trans,cis-[RhCl2(PPh2py-P,N)2]PF6 (2) in acetone solution by treatment with Ag+ and PF6-. Ruthenium(III) and ruthenium(II) compounds with PPh2py, mer,cis-[RuCl3(PPh2py-P,N)(PPh2py-P)] (3) and mer-[RuCl(PPh2py-P,N)2(PPh2py-P)]Cl (5) have been obtained from DMSO precursor complexes. In a chloroform solution, complex (5) isomerizes to fac-[RuCl(PPh2py-P,N)2(PPh2py-P)]Cl (fac-5). All compounds have been characterized by MS, UV−vis, IR, and 1H and 31P{1H} NMR spectroscopy, and the Ru(III) compound has been characterized by EPR spectroscopy as well. The crystal structures of 1, 2, 3, and fac-5 have been determined. In all compounds under investigation, at least one pyridylphosphine acts as a chelate ligand. The 31P chemical shifts for chelating PPh2py-P,N depend on the Ru−P bond lengths.

Syntheses and molecular structure of some Rh and Ru complexes with the chelating diphenyl (2-pyridyl)phosphine ligand.

Complexes of Distibinomethane Ligands. 1. Iron, Cobalt, Nickel, and Manganese Carbonyl Complexes

The complexes [AgL4]BF4 (L = SbMe3, SbEt3, SbMe2Ph, SbMePh2, SbPh3, SbMe2(o-C6H4Br)) and [Ag{R2Sb(CH2)3SbR2}2]BF4 (R = Me, Ph) have been prepared and studied by variable-temperature 1H and 109Ag NMR spectroscopy. The structure of [Ag(SbPh3)4]BF4 is reported.

Synthesis and 109ag nmr studies of homoleptic silver(i) stibines

Substituted Group 6 carbonyl complexes of the distibinomethane ligands Ph2SbCH2SbPh2 (dpsm) and Me2SbCH2SbMe2 (dmsm) of types [M(CO)5(η1-dpsm)] (M = Cr, Mo or W), [(OC)5M(µ-dpsm)M(CO)5] (M ≠ Mo), [(OC)5M(µ-dmsm)M(CO)5], [(OC)4M(µ-dpsm)2M(CO)4], [(OC)4M(µ-dmsm)2M(CO)4] and fac-[M(CO)3(η1-dpsm)3] have been isolated and characterised by chemical analysis, IR, NMR (1H, 13C-{1H}, 95Mo) spectroscopy and FAB mass spectrometry. The crystal structures of [W(CO)5(dpsm)], [{W(CO)5}2(dpsm)], [{W(CO)4(dpsm)}2] and [{W(CO)4(dmsm)}2] have been determined. Complexes of η1-dmsm have been observed but are too unstable to isolate in a pure state. Both the ligands function as monodentate or bridging bidentates in the complexes characterised, but no examples with chelated distibinomethanes have been prepared. Comparisons are drawn with complexes of related diphosphine ligands.

Chromium, molybdenum and tungsten carbonyl derivatives of distibinomethane ligands†

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)

Rhodium(III) ditertiary stibine complexes

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