Cu K-Edge EXAFS Characterisation of Copper(I) Arenethiolate Complexes in both the Solid and Liquid State: Detection of CuCu Coordination

Tromp, Moniek; Bokhoven, Jeroen A. van; Arink, Anne M.; Bitter, Johannes H.; Koten, Gerard van; Koningsberger, D.C.

doi:10.1002/1521-3765(20021216)8:24<5667::aid-chem5667>3.0.co;2-o

Cited by 32 publications

(36 citation statements)

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“…The fit was evaluated in all weightings ( k n with n =0, 1, 2, and 3) to unravel anti‐phase behaviour, which can easily lead to the non‐detection of a particular contribution when only one particular weighting is used 34. 40, 41 Details of the fitting procedure in relation to supported vanadium oxides have been described in previous papers by our group 28. 34…”

Section: Methodsmentioning

confidence: 99%

Application of AXAFS Spectroscopy to Transition‐Metal Oxides: Influence of the Nearest and Next Nearest Neighbour Shells in Vanadium Oxides

Keller

Weckhuysen

Koningsberger

2007

Chemistry A European J

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IntroductionMany parameters affect the catalytic properties of transition-metal oxide catalysts, for example, metal oxide loading, pre-treatment conditions, molecular structure, electronic structure, and the nature of the supporting oxide. [1][2][3][4][5][6][7] Various researchers have investigated the activities and selectivities of metal oxide catalysts. However, little is known about the parameters that are truly responsible for the catalytic action of transition-metal oxides.To study the effect of the support on the catalytic performance, one has to find a tool that is capable of probing the influence of the local environment (e.g., the support or promoters) on the properties of the catalytically active species, that is, a metal particle or metal oxide cluster. Metal-A C H T U N G T R E N N U N G (oxide)-support interactions can be ascribed to a structural (particle/cluster size and shape) effect, but can also have an electronic origin. For supported metal particles, the effect of the support on the catalytic properties has been determined by several techniques, for example, XPS, FT-IR analysis of adsorbed CO, and newly developed delta XANES and atomic XAFS (AXAFS) techniques. [8][9][10][11][12][13][14][15] In particular, the application of AXAFS has, in our opinion, led to a better understanding of metal-support interaction effects. [8,[15][16][17] AXAFS is sensitive to changes in the potential around the X-ray absorbing atom. The potential field around an atom is mainly determined by the first and second coordination spheres. O Grady et al. have shown for Pt/Ru alloys that the AXAFS intensity changes systematically with the composition of the alloy. [18] Thus, when the number of Ru atoms around a Pt atom increases, the intensity of the FT AXAFS peak increases and the peak centroid shifts to lower values of R. Comparison of these effects with the effects observed for a Pt electrode as a function of the applied voltage suggests that the first coordination shell of the Pt in the Pt/Ru alloy influences the electronic properties (inter-A C H T U N G T R E N N U N G atomic potential) of the Pt atom. [18,19] The effect of changes in the coordination around the absorber atom has been further illustrated for Pt by van Dorssen et al., who compared the AXAFS of a Pt foil with that of bulk Na 2 Pt(OH) 6 . The AXAFS intensity was found to be significantly higher in the Abstract: The influence of changes in coordination number, interatomic distances, and oxidation state on the intensity and centroid position of the Fourier transform (FT) of the atomic X-ray absorption fine structure (AXAFS) peak of vanadium oxide bulk model compounds and aluminasupported vanadium oxide clusters has been investigated. Using Na 3 VO 4 and V 2 O 5 as model compounds, it has been shown that the nearest neighbour shells have a pronounced influence on the AXAFS intensity; specifically, a 40 % decrease in intensity was observed between these two compounds. Secondly, the influence of partial reduction of the vanadium oxide species has been dete...

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Section: Methodsmentioning

confidence: 99%

Application of AXAFS Spectroscopy to Transition‐Metal Oxides: Influence of the Nearest and Next Nearest Neighbour Shells in Vanadium Oxides

Keller

Weckhuysen

Koningsberger

2007

Chemistry A European J

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“…XAS is a well-established technique which can provide information on the oxidation state, site symmetry, and coordination environment of a selected analyte in the gas, liquid or solid phase [2,6,8,[3][4][5]7,32,33,126,128,127,129,130]. Transmission XAS experiments are the most direct way to measure the absorption as it does not suffer from self-absorption effects, where the latter is the case in most fluorescence yield detected XAS (FY-XAS) experiments [33,131,132].…”

Section: Xas Backgroundmentioning

confidence: 99%

“…Nowadays X-ray spectroscopy is employed in almost every thinkable field of technology and research. To give just a few examples, applications range from fundamental research in chemistry [3][4][5][6][7][8], physics [9][10][11][12][13][14][15] and material science [16,17], to environmental research [18,19], architecture [20], art [19,21,22], archeology [19,[23][24][25] and industrial applications [19], to even forensics [19], security systems [26,27] and astronomy [28][29][30][31]. In a scientific context X-ray spectroscopy is also known as core-level-or core-spectroscopy [32,33] and it has become an essential tool for the study of a vast number of systems.…”

Section: Introductionmentioning

confidence: 99%

Modern X-ray spectroscopy: XAS and XES in the laboratory

Zimmermann

Peredkov

Abdala

et al. 2020

Coordination Chemistry Reviews

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147

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X-ray spectroscopy is an important tool for scientific analysis. While the earliest demonstration experiments were realised in the laboratory, with the advent of synchrotron light sources most of the experiments shifted to large scale synchrotron facilities. In the recent past there is an increased interest to perform X-ray experiments also with in-house laboratory sources, to simplify access to X-ray absorption and X-ray emission spectroscopy, in particular for routine measurements. Here we summarise the recent developments and comment on the most representative example experiments in the field of in-house laboratory X-ray spectroscopy. We first give an introduction and some historic background on X-ray spectroscopy. This is followed by an overview of the detection techniques used for X-ray absorption and X-ray emission measurements. A short paragraph also puts related high energy resolution and resonant techniques into context, though they are not yet feasible in the laboratory. At the end of this section the opportunities using wavelength dispersive X-ray spectroscopy in the laboratory are discussed. Then we summarise the relevant details of the recent experimental laboratory setups split into two separate sections, one for the recent von Hamos setups, and one for the recent Johann/Johansson type setups. Following that, focussing on chemistry and catalysis, we then summarise some of the notable X-ray absorption and X-ray emission experiments and the results accomplished with in-house setups. In a third part we then discuss some applications of laboratory X-ray spectroscopy with a particular focus on chemistry and catalysis.

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“…23 was selectively formed by mixing mesitylcopper and copper aminoarenethiolate in 1:1 M ratio and then transferred to 23 by addition of one equivalent of PPh 3 (mimicking the addition of an electrophilic substrate to the cuprate intermediate), see Fig. 12 [33,35]. To summarize: the reaction of MgIMe with a diethyl ether solution of benzylideneacetone and 3 mol% of [CuSAr*] (providing the "dummy", non-transferable anion), at 0 C gives rise to the formation of the 1,4-addition product in 57% ee [33,35,36].…”

Section: 2mentioning

confidence: 99%

“…12 [33,35]. To summarize: the reaction of MgIMe with a diethyl ether solution of benzylideneacetone and 3 mol% of [CuSAr*] (providing the "dummy", non-transferable anion), at 0 C gives rise to the formation of the 1,4-addition product in 57% ee [33,35,36]. This preliminary result (later improved to 76%) represented, to the best of our knowledge, one of the first reported examples of the catalytic use of a copper salt with a chiral auxiliary in an enantioselective 1,4-addition reaction of self-assembled cuprate reagents.…”

Section: 2mentioning

confidence: 99%

Highlights of 45 years of research: A personal account

Koten

2017

Journal of Organometallic Chemistry

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a b s t r a c tThis part of my biosketch, which I prepared on invitation by the Editors, made me realize again how entangled my interest for doing research and teaching and management have been over the years. Working together with my students and colleagues has always been a strong motivation and pleasure for me and I hope that this sketch of our research reflects our common enthusiasm for what we achieved.In hindsight, trying to overlook almost 45 years of research, various main themes can be discerned that marked my fundamental research in the subsequent periods at TNO Utrecht (1968e1977), University of Amsterdam (1977e1986) and University of Utrecht (1986e2007). Overarching has been my preference and fascination for working with nitrogen based ligands (culminating in the design and use of the NCNpincer ligand platform, vide infra), the study of synthetic routes for organometallics (most importantly trans-and cyclo-metallation routes), the use of NMR for the study of the stereochemistry of organometallics (cf. the early use of 107,109 Ag NMR for detecting and following the formation of coordination compounds with helical structures), chemistry involving organometallic radicals (cf. organozinc and aluminum a-diimine chemistry, development of b-lactam synthesis routes), self-assembly of organometallics to discrete aggregated species (cf. organo-Cu, -Li and cuprate chemistry), the development of palladium complexes and homogeneous metal catalysts with simple amine ligands, the synthesis of, and catalysis with, dendrimers decorated with organometallic catalysts, mimicking the active center of metallo-enzymes as well as the synthesis of organometal-lipase hybrids for catalysis.Being educated in an "eco"-system of contract research, in concert with fundamental research, the results of the above outlined items were not only published in journals with peer review (>850) but also in the patent literature (>40). Most important were the results reported in over 85 PhD theses that I had the privilege to supervise as PI. The references refer to key-papers describing this body of work. The respective reference numbers are given at the heading of each paragraph. The full list of publications in peer reviewed Journals can be found in http://www.gerardvankoten.nl and www.uu.nl/staff/GvanKoten.© 2017 The Author. Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/). GeneralAs indicated above, nitrogen ligands fascinated me throughout my research career, right from the very beginning. Whereas in my early days ligands with phosphorous donor atoms were the dominating "privileged" ligands in inorganic and organometallic chemistry; they have remained so up until now. However, my interest for nitrogen-containing ligands was fortified for a number of reasons; i, Nitrogen is one of the smallest donor atoms. This results in short N-metal bond distances thus affecting/interfering with its (N)R-substituents (also because of the short N-C bonds, viz. N-cone angle c...

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Cu K-Edge EXAFS Characterisation of Copper(I) Arenethiolate Complexes in both the Solid and Liquid State: Detection of CuCu Coordination

Cited by 32 publications

References 55 publications

Application of AXAFS Spectroscopy to Transition‐Metal Oxides: Influence of the Nearest and Next Nearest Neighbour Shells in Vanadium Oxides

Application of AXAFS Spectroscopy to Transition‐Metal Oxides: Influence of the Nearest and Next Nearest Neighbour Shells in Vanadium Oxides

Modern X-ray spectroscopy: XAS and XES in the laboratory

Highlights of 45 years of research: A personal account

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