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Johannes G Vos

Publications and source records attributed to Johannes G Vos.

At least 19 recordsLinked to original sources

A density functional theory study of the electronic properties of Os(II) and Os(III) complexes immobilized on Au(111).

We present a density functional theory (DFT) study of an osmium polypyridyl complex adsorbed on Au(111). The osmium polypyridyl complex [Os(bpy)2(P0P)Cl]n+ [bpy is 2,2'-bipyridine, P0P is 4,4'-bipyridine, n = 1 for osmium(II), and n = 2 for osmium(III)] is bound to the surface through the free nitrogen of the P0P ligand. The calculations illuminate electronic properties relevant to recent comprehensive characterization of this class of osmium complexes by electrochemistry and electrochemical scanning tunneling microscopy. The optimized structures for the compounds are in close agreement with crystallographic structures reported in the literature. Oxidation of the complex has little effect on these structural features, but there is a substantial reordering of the electronic energy levels with corresponding changes in the electron density. Significantly, the highest occupied molecular orbital shifts from the metal center to the P0P ligand. The surface is modeled by a cluster of 28 gold atoms and gives a good description of the effect of immobilization on the electronic properties of the complexes. The results show that the coupling between the immobilized complex and the gold surface involves electronic polarization at the adsorbate/substrate interface rather than the formation of a covalent bond. However, the cluster is too small to fully represent bulk gold with the result that, contrary to what is experimentally observed, the DFT calculation predicts that the gold surface is more easily oxidized than the osmium(II) complex.

Algorithms↗

Mechanism of electrochemical charge transport in individual transition metal complexes.

We used electrochemical scanning tunneling microscopy (STM) and spectroscopy (STS) to elucidate the mechanism of electron transport through individual pyridyl-based Os complexes. Our tunneling data obtained by two-dimensional electrochemical STS and STM imaging lead us to the conclusion that electron transport occurs by thermally activated hopping. The conductance enhancement around the redox potential of the complex, which is reminiscent of switching and transistor characterics in electronics, is reflected both in the STM imaging contrast and directly in the tunneling current. The latter shows a biphasic distance dependence, in line with a two-step electron hopping process. Under conditions where the substrate/molecule electron transfer (ET) step is dominant in determining the overall tunneling current, we determined the conductance of an individual Os complex to be 9 nS (Vbias = 0.1 V). We use theoretical approaches to connect the single-molecule conductance with electrochemical kinetics data obtained from monolayer experiments. While the latter leave some controversy regarding the degree of electronic coupling, our results suggest that electron transport occurs in the adiabatic limit of strong electronic coupling. Remarkably, and in contrast to established ET theory, the redox-mediated tunneling current remains strongly distance dependent due to the electronic coupling, even in the adiabatic limit. We exploit this feature and apply it to electrochemical single-molecule conductance data. In this way, we attempt to paint a unified picture of electrochemical charge transport at the single-molecule and monolayer levels.

Journal Article↗

Ruthenium polypyridyl chemistry; from basic research to applications and back again.

Since the mid 1970's interest in the chemistry and applications of ruthenium polypyridyl complexes has increased steadily. In this perspective, the development of this area is tracked and discussed taking into account new scientific developments as well as novel applications. The interaction between basic and applied research is of particular importance and selected examples are highlighted.

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Derivatives of dipyrido[3,2-a:2',3'-c]phenazine and its ruthenium complexes, influence of arylic substitution on photophysical properties.

The synthesis and photophysical properties of a series of substituted dipyridophenazine (dppz) ruthenium complexes of the type [(tbbpy)2Ru(dppz-R2)]2+ (where tbbpy = 4,4-tert-butyl-2,2-bipyridine and dppz = dipyrido[3,2-a:2',3'-c]phenazine and R represents substitution at the 11 and 12 position with: Br, phenyl, 4-tert-butyl-phenyl and para-biphenyl) are described. The ligands could be obtained in high yields using Suzuki-type coupling reactions, an approach which also has been successfully applied to the analogous dppz-Br2 ruthenium complex. All compounds are fully characterised by NMR, MS and UV-vis spectroscopy. The solid state structures of dppz-bi-para-biphenyl and the ruthenium complex [(tbbpy)2Ru(dppz-Br2)]2+ are also reported. The investigation of the free ligands reveals a pronounced effect of the arylic substitution on absorption and emission properties. These properties are mirrored in the corresponding complexes, which possess emission lifetimes of up to 900 ns. The resonance Raman investigation of the complex [(tbbpy)2Ru(dppz-Br2)]2+ supports the assumption that the excited state properties of the substituted complexes are related to the parent [(bpy)2Ru(dppz)]2+ compound, but that important differences may be expected based on the differences observed in the lowest energy absorption band.

Crystallography, X-Ray↗

In situ scanning tunnelling spectroscopy of inorganic transition metal complexes.

Redox molecules with equilibrium potentials suitable for electrochemical control offer perspectives in nanoscale and single-molecule electronics. This applies to molecular but also towards higher sophistication such as transistor or diode function. Most recent nanoscale or single-molecule functional systems are, however, fraught with operational limitations such as cryogenic temperatures and ultra-high vacuum, or lack of electrochemical potential control. We report here cyclic voltammetry (CV) using single-crystal Au(111)- and Pt(111)-electrodes and electrochemical in situ scanning tunnelling microscopy (STM) of a class of Os(II)/(III)- and Co(II)/(III)-complexes, the former novel molecular electronics. The complexes are robust, with ligand groups suitable for linking the complexes to the Au(111)- and Pt(111)-surfaces via N- and S-donor atoms. The data reflect monolayer behaviour. Interfacial ET of the Os-complexes is fast, kET(0) > or = 10(6) s(-1), while the Co-complex reacts much more slowly, kET(0) approximately (1-3) x 10(3) s(-1). In STM of the Os-complexes shows a maximum in the tunnelling current/overpotential relation at constant bias voltage with up to 50-fold current rise. The peak position systematically the bias voltage and equilibrium potential, in keeping with theoretical frames for two-step electron transfer (ET) of in situ STM of redox molecules. The molecular conductivity behaves broadly similarly. The Co-complex also shows a tunnelling spectroscopic feature but much weaker than the Os-complexes. This can be ascribed much smaller interfacial ET rate constant, again caused by large intramolecular nuclear reorganization and weak electronic coupling to the substrate electrode. Overall the has mapped the properties of target molecules needed for stable electronic switching, possible importance in molecular electronics towards the single-molecule level, in room temperature condensed matter environment.

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Synthesis of mononuclear and dinuclear ruthenium(II) tris(heteroleptic) complexes via photosubstitution in bis(carbonyl) precursors.

A novel, and quite general, approach for the preparation of tris(heteroleptic) ruthenium(II) complexes is reported. Using this method, which is based on photosubstitution of carbonyl ligands in precursors such as [Ru(bpy)(CO)(2)Cl(2)] and [Ru(bpy)(Me(2)bpy)(CO)(2)](PF(6))(2), mononuclear and dinuclear Ru(II) tris(heteroleptic) polypyridyl complexes containing the bridging ligands 3,5-bis(pyridin-2-yl)-1,2,4-triazole (Hbpt) and 3,5-bis(pyrazin-2-yl)-1,2,4-triazole (Hbpzt) have been prepared. The complexes obtained were purified by column chromatography and characterized by HPLC, mass spectrometry, 1H NMR, absorption and emission spectroscopy and by electrochemical methods. The X-ray structures of the compounds [Ru(bpy)(Me(2)bpy)(bpt)](PF(6))x0.5C(4)H(10)O [1x0.5C(4)H(10)O], [Ru(bpy)(Me(2)bpy)(bpzt)](PF(6))xH(2)O (2xH(2)O) and [Ru(bpy)(Me(2)bpy)(CH(3)CN)(2)](PF(6))(2)xC(4)H(10)O (6xC(4)H(10)O) are reported. The synthesis and characterisation of the dinuclear analogues of 1 and 2, [{Ru(bpy)(Me(2)bpy)}(2)bpt](PF(6))(3)x2H(2)O (3) and [{Ru(bpy)(Me(2)bpy)}(2)bpzt](PF(6))(3) (4), are also described.

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Microscopy and spectroscopy of interactions between metallopolymers and carbon nanotubes.

The interaction between redox polymers, based on Ru- or Os-bis(2,2'-bipyridyl)-poly(4-vinylpyridine), and carbon nanotubes was investigated by spectroscopic and microscopic techniques. These metallopolymers were found to be excellent dispersants for nanotubes, as a result of a good wetting interaction between polymer and nanotubes. The results obtained show that well-coated individual nanotubes can be obtained. In addition, interactions between nanotubes and polymers did not significantly affect the electronic and electrochemical properties of the metallopolymers. On the basis of the electrochemical properties of the polymers this opens the possibility of adding functionality through interaction with nanotubes, either as redox active materials with enhanced mechanical properties or by using these modified nanotubes as nanosized electrochemical sensors.

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Elucidating excited state electronic structure and intercomponent interactions in multicomponent and supramolecular systems.

Rational design of supramolecular systems for application in photonic devices requires a clear understanding of both the mechanism of energy and electron transfer processes and how these processes can be manipulated. Central to achieving these goals is a detailed picture of their electronic structure and of the interaction between the constituent components. We review several approaches that have been taken towards gaining such understanding, with particular focus on the physical techniques employed. In the discussion, case studies are introduced to illustrate the key issues under consideration.

Chemical Phenomena↗

Ground- and excited-state electronic structure of an emissive pyrazine-bridged ruthenium(II) dinuclear complex.

The synthesis, characterization, and electrochemical, photophysical, and photochemical properties of the binuclear compounds [(Ru(H8-bpy)2)2((Metr)2Pz)](PF6)2 (1) and [(Ru(D8-bpy)2)2((Metr)2Pz)](PF6)2 (2), where bpy is 2,2'-bipyridine and H2(Metr)2Pz is the planar ligand 2,5-bis(5'-methyl-4'H-[1,2,4]triaz-3'-yl)pyrazine, are reported. Electrochemical and spectro-electrochemical investigations indicate that the ground-state interaction between each metal center is predominantly electrostatic and in the mixed-valence form only a low level of ground-state delocalization is present. Resonance Raman, transient, and time-resolved spectroscopies enable a detailed assignment to be made of the excited-state photophysical properties of the complexes. Deuteriation is employed to both facilitate spectroscopic characterization and investigate the nature of the lowest excited states.

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Transistor-like behavior of transition metal complexes.

Electron transport through semiconductor and metallic nanoscale structures, molecular monolayers, and single molecules connected to external electrodes display rectification, switch, and staircase functionality of potential importance in future miniaturization of electronic devices. Common to most reported systems is, however, ultrahigh vacuum and/or cryogenic working conditions. Here we introduce a single-molecule device concept based on a class of robust redox active transition metal (Os(II)/(III)) complexes inserted between the working electrode and tip in an electrochemical scanning tunneling microscope (in situ STM). This configuration resembles a single-molecule transistor, where the reference electrode corresponds to the gate electrode. It operates at room temperature in a condensed matter (here aqueous) environment. Amplification on-off ratios up to 50 are found when the redox level is brought into the energy window between the Fermi levels of the electrodes by the overpotential ("gate voltage"). The current-voltage characteristics for two Os(II)/(III) complexes have been characterized systematically and supported by theoretical frames based on molecular charge transport theory.

Electrochemistry↗

Assessment of intercomponent interaction in phenylene bridged dinuclear ruthenium(II) and osmium(II) polypyridyl complexes.

The synthesis and characterisation of [Ru(bipy)(2)(L1)](2+) and the homodinuclear complexes [M(bipy)(2)(L1)M(bipy)(2)](4+)(where M = Ru or Os), employing the ditopic ligand, 1,4-phenylene-bis(1-pyridin-2-ylimidazo[1,5-a]pyridine)(L1), are reported. The complexes are identified by elemental analysis, UV/Vis, emission, resonance Raman, transient resonance Raman and (1)H NMR spectroscopy, mass spectrometry and electrochemistry. The X-ray structure of the complex [Ru(bipy)(2)(L1)(bipy)(2)Ru](PF(6))(4) is also reported. DFT calculations, carried out to model the electronic properties of the compounds, are in good agreement with experiment. Minimal communication between the metal centres is observed. The low level of ground state electronic interaction is rationalized in terms of the poor ability of the phenyl spacer in facilitating superexchange interactions. Using the electronic and electrochemical data a detailed picture of the electronic properties of the RuRu compound is presented.

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Complexed nitrogen heterosuperbenzene: the coordinating properties of a remarkable ligand.

Tetra-peri-(tert-butyl-benzo)-di-peri-(pyrimidino)-coronene 1, the parent compound of the nitrogen heterosuperbenzene family N-HSB, is employed as a novel monotopic ligand in the formation of [Pd(eta3-C3H5)(1)]PF6 2 and [Ru(bpy)2(1)](PF6)2 (where bpy = 2,2'-bipyridine 3a and d8-2,2'-bipyridine 3b). These N-coordinated complexes are fully characterized by 1H NMR and IR spectroscopy and ESI-MS. Metal coordination has a profound effect on both the absorption and the emission properties of 1. Pd(II) coordination causes a red-shift in the low-energy absorptions, a decrease in the intensity of the n-pi absorptions, and a quenching of the emission. Ru(II) coordination causes absorption throughout the visible region and creates two new complexes that join an elite group of compounds known as "black" absorbers. 3a and 3b possess two discernible 1MLCT bands. The one of exceptionally low energy (lambda(max) = 615 nm) has an associated (3)MLCT emission (lambda(max) = 880 nm) due to the unprecedented electron delocalization and acceptor properties of the rigid aromatic N-HSB 1. Both Ru(II) complexes are near-IR emitters with unusually protracted emission lifetimes of 320 ns at 77 K. They are photochemically inert, and their electrochemical properties are consistent with the presence of a low-lying pi orbital on 1. The first two reversible reductions (E(1/2) (CH3CN), -0.54 V, -1.01 V vs SCE) are due to the stepwise reduction of 1 and are anodically shifted as compared to [Ru(bpy)3]2+. Temperature- and concentration-dependent NMR studies on 2 and 3a suggest extensive aggregation is occurring in solution.

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Energy transfer pathways in dinuclear heteroleptic polypyridyl complexes: through-space vs through-bond interaction mechanisms.

A series of homo- and heteronuclear ruthenium and osmium polypyridyl complexes with the bridging ligands 1,3-bis(5-(2-pyridyl)-1H-1,2,4-triazol-3-yl)benzene (H(2)mL) and 1,4-bis(5-(2-pyridyl)-1H-1,2,4-triazol-3-yl)benzene (H(2)pL) are reported. The photophysical properties of these compounds are investigated, and particular attention is paid to the heteronuclear (RuOs) compounds, which exhibit dual emission. This is in contrast to phenyl-bridged polypyridine Ru-Os complexes with a similar metal-metal distance, in which the Ru emission is strongly quenched because the nature of the bridging ligand allows for an efficient through-bond coupling. The results obtained for the compounds reported here suggest that energy transfer is predominantly taking place via a dipole-dipole, Förster type, mechanism, that may dominate when through-bond coupling is weak. This is in stark contrast to ground state interaction, which is found to be critically dependent on the nature of the bridging unit employed.

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Electronic and photophysical properties of a novel phenol bound dinuclear ruthenium complex: evidence for a luminescent mixed valence state.

A novel dinuclear ruthenium(II) complex bridged by dianionic bridge 3-(2-phenol)-5-(pyridin-2-yl)-1,2,4-triazole in which the ruthenium metal atoms are bound through N,N coordination to the pyridine and triazole and O,N coordination to the triazole and phenolate is described. The electrochemical, spectroscopic and photophysical behaviour of the dimer is compared with its associated N,N- and O,N-coordinated mononuclear complexes. The mixed valence complex was prepared electrochemically and a weak inter-valence charge transfer transition is observed which from Hush theory provides an electronic coupling matrix element of 666 cm(-1), suggesting the complex is weakly coupled and valence trapped. In its native state the dinuclear compound is essentially non-emissive but upon the oxidation of the O,N moiety luminescence from the complex is reversibly switched on at 0.3 V and reversibly switched off by application of 1.3 or 0 V. To our knowledge this is the first report of a luminescent mixed valence ruthenium complex.

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Synthesis and characterisation of ruthenium complexes containing a pendent catechol ring.

A series of [Ru(bipy)2L]+ and [Ru(phen)2L]+ complexes where L is 2-[5-(3,4-dimethoxyphenyl)-4H-1,2,4-triazol-3-yl]pyridine (HL1) and 4-(5-pyridin-2-yl-4H-1,2,4-triazol-3-yl)benzene-1,2-diol (HL2) are reported. The compounds obtained have been characterised using X-ray crystallography, NMR, UV/Vis and emission spectroscopies. Partial deuteriation is used to determine the nature of the emitting state and to simplify the NMR spectra. The acid-base properties of the compounds are also investigated. The electronic structures of [Ru(bipy)2L1]+ and Ru(bipy)2HL1]2+ are examined using ZINDO. Electro and spectroelectrochemical studies on [Ru(bipy)2(L2)]+ suggest that proton transfer between the catechol and triazole moieties on L2 takes place upon oxidation of the L2 ligand.

Catechols↗

Enhancement of luminescence lifetimes of mononuclear ruthenium(II)-terpyridine complexes by manipulation of the sigma-donor strength of ligands.

The synthesis and characterization of mixed ligand 2,2';6',2' '-terpyridine (tpy) ruthenium complexes with 2,6-bis([1,2,4]triazol-3-yl)pyridine, 2,6-bis(5-phenyl-[1,2,4]triazol-3-yl)pyridine, and 2,6-bis([1,2,3,4]tetrazol-5-yl)pyridine are reported. The species are characterized by HPLC, 1H NMR, UV/vis, and emission spectroscopy. The photophysical properties of the complexes are investigated as a function of temperature over the range 80-320 K. The emission lifetime observed for the fully deprotonated compounds at room temperature is about 80 ns. This increase by 2 orders of magnitude with respect to the parent "[Ru(tpy)2](2+)" complex is rationalized by an increase in the energy of the metal based dsigma orbital, rather than by manipulation of the pi* orbitals on the ligands. The acid-base and electrochemical properties of the compounds are reported also.

Journal Article↗

Isotope effects on the picosecond time-resolved emission spectroscopy of tris(2,2'-bipyridine)ruthenium (II).

The excited-state properties of the transition metal complexes tris(2,2'-bipyridine) ruthenium(II) and tris(4,7-diphenyl-1,10-phenanthroline) ruthenium(II) are examined using picosecond time-resolved luminescence spectroscopy. For both complexes, direct observation of a short-lived high-energy emission with a lifetime of less than 4 ps is reported. Upon deuteriation of the complexes the lifetime of the high-energy emission shows a marked increase with a biexponential decay (20 and approximately 300 ps components). Examination by time-resolved excited-state resonance Raman shows that for the perprotio complexes features attributable to the 3MLCT excited state are formed within 4 ps, while for the perdeuterio a rise time of approximately 20 ps is observed in the 3MLCT features. The results indicate that the emission in both cases may be 1MLCT in origin and are discussed with respect to heterogeneous electron transfer.

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