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Articles by Ingo Krossing
Redox Potentials for the Synthesis of Cationic Transition Metal Complexes from the Metal and Weak Ligands: A Computational Methodology for Practical Oxidant Choice
1 Introduction The conceptually simplest way to generate a cationic complex is the removal of an electron from a neutral precursor by deelectronation [1]. Consequently, a wide range of cationic species, including transition-metal carbonyl complexes [2, 3] and organic (di)cations [4, 5], have been prepared in recent years via deelectronation of their neutral counterparts.
A Bridged Copper(I) Diiodine Complex
Filename Description ejic70352-sup-0001-SuppData-S1.pdf1,010.1 KB The electronic supporting information contains the general synthetic methods and characterization techniques used for this work together with the experimental procedures. Additional figures such as NMR and Raman spectra are presented, including the crystallographic data of the isolated salt and details of the quantum chemical calculations.
Finding the Perfect Match: Investigation of 1,2-Diketone-Based Materials for Use as Cathode Active Material in Rechargeable Magnesium Batteries
1 Introduction Electrochemical energy storage methods, such as lithium-ion batteries (LIB), play a key role in the energy transition [1, 2]. Their high round-trip efficiency exceeding 90% makes them ideal candidates for a versatile alternative to pumped hydro storage [2, 3]. However, high production costs, safety concerns, and limited lithium resources motivate the development of more sustainable battery systems based on abundant metals such as aluminum, calcium, or magnesium [4-6].
Fluorinated CuO/ZnO/MgO Catalyst Systems for the Direct CO2 Hydrogenation to DME
1 Introduction In order to combat the effects of climate change, it is essential to implement technologies that facilitate the capture and utilization of carbon dioxide (CCU) and those that enable the conversion of electrical energy into other forms (Power-to-X, PtX). Especially, since the European Parliament has committed EU member countries to the European Green Deal to reduce their greenhouse gas emissions to net-zero by 2050 (European Parliament, 2020) [1].
First Heterodinuclear Transition Metal Carbonyl Cation [MnFe(CO)10]+
Dr. Malte Sellin and Professor Ingo Krossing, Albert-Ludwigs-Universität Freiburg, Germany discuss the synthesis, characterization, and bonding of the heterodinuclear cation [MnFe(CO)₁₀]⁺, along with the preparation of the isoelectronic anion [CrMn(CO)10]− What did you do? Dimetal decacarbonyl complexes like Mn₂(CO)₁₀ are fundamental to organometallic chemistry and essential for teaching the subject to chemistry majors.
Isolation and Characterization of the Dimetal Decacarbonyl Dication [Ru2(CO)10]2+ and the Metal-Only Lewis-Pair [Ag{Ru(CO)5}2]+
Isolation and Characterization of the Dimetal Decacarbonyl Dication [Ru2(CO)10]2+ and the Metal-Only Lewis-Pair [Ag{Ru(CO)5}2]+ The reaction of Ag+ with Ru3(CO)12 in CO atmosphere under concommittant irradiation with UV-light yields a salt of the metal-only Lewis-pair [Ag{Ru(CO)5}2]+.
Reaction Mechanisms of High‐Rate Copper Electrochemical Machining in Nitrate Electrolytes
Supporting Information As a service to our authors and readers, this journal provides supporting information supplied by the authors. Such materials are peer reviewed and may be re-organized for online delivery, but are not copy-edited or typeset. Technical support issues arising from supporting information (other than missing files) should be addressed to the authors.
Reaction Mechanisms of High‐Rate Copper Electrochemical Machining in Nitrate Electrolytes
Introduction Electrochemical machining (ECM) is a non-traditional metal shaping technique known and applied since the middle of the last century. Industrially, it is mainly used for shaping difficult-to-machine metals and alloys and complex shapes, e.g., turbine blades, parts for aerospace1 and automotive industry2 or biomedical industry.3 Characteristics are the polished surfaces and the unconventionally high current densities (>100 A cm−2) applied for controlled anodic metal oxidation.
The Ether‐Adduct of a Lewis Superacidic, Dicoordinate Aluminum Hydride Cation and the Ion Affinities of Solvent‐Adducts
Supporting Information As a service to our authors and readers, this journal provides supporting information supplied by the authors. Such materials are peer reviewed and may be re-organized for online delivery, but are not copy-edited or typeset. Technical support issues arising from supporting information (other than missing files) should be addressed to the authors.
Does Direct Dimethyl Ether Synthesis from Carbon Dioxide and Hydrogen Yield More Valuable Products than the Equivalent Methanol Production? A Review on Recent Work
1 Introduction The share of fossil fuels in the global energy mix has been constantly high, about 80 %, for decades [1]. Even though governments and societies of nearly every country increase their effort to upgrade their renewable energy infrastructure, the share of fossil fuels like coal, oil, and natural gas are not expected to drop below 60 % by 2050 [1]. This use of fossil fuels resulted in a global energy-related CO2 emission of ca.
In situ formation of reactive (di)gallenes for bond activation - Nature Synthesis
Abstract Access to reactive low-valent main-group complexes capable of bond activation commonly requires multistep syntheses, limiting options for electronic or steric fine-tuning. Here we present a one-pot synthesis of highly reactive Ga(I) complex cations for the activation of strong bonds that works analogously to the in situ generation of active transition-metal catalysts.
Gold carbonyl cations and beyond: homoleptic gold(I) complexes with P4 and P4S3 and the half-sandwich cation [Au(C6H6)(CO)]+
Gold carbonyl cations and beyond: homoleptic gold(i) complexes with P4 and P4S3 and the half-sandwich cation [Au(C6H6)(CO)]+† Oxidation of Au0 with the synergistic Ag+/0.5 I2 system in the commercial organic solvent 1,2,3,4-tetrafluorobenzene led to the perfluoroalkoxyaluminate salt of the [Au(CO)2]+ cation known from superacid chemistry.
Synthesis and Characterization of a Stable Nickelocenium Dication Salt
In 1951 two groups independently published the synthesis of the famous ferrocene molecule and thus opened the door to the rich chemistry of the metallocenes.1 Fischer, Woodward and Wilkinson proposed the—at that time revolutionary—π-bonding between the η5-Cp-ligands and the central iron atom, which was later confirmed by single crystal XRD and was eventually awarded the Nobel prize.2 Since then, many metallocene derivates have been synthesized spanning from transition metals to p-block...
Homoleptic Transition Metal Carbonyl Cations: Synthetic Approaches, Characterization and Follow-Up Chemistry
Conspectus Carbon monoxide, CO, is one of the most important ligands in organometallic chemistry. It is an excellent π-acceptor and a moderate σ-donor. Therefore, most of the known transition metal carbonyls (TMCs) exhibit a zerovalent or even negative metal oxidation state (OS) of up to −4.
The Best of Both Worlds: Combining the Power of MICs and WCAs to generate Stable and Crystalline CrI‐tetracarbonyl Complexes with Accepting Ligands
Graphical Abstract The isolation of two isomeric pyridyl-MIC chromium(I) tetracarbonyl complexes, which were fully characterized by IR- and EPR-spectroscopy and compared with their electrochemical-generated analogues is presented. Furthermore, theoretical calculations were conducted to get detailed information about the electronic structure of these rare complexes. This is the first time Cr(I) complexes with π-acceptor ligands have been isolated and crystallographically characterized.
Coordination versus Insertion: On the Interaction of 5 d‐Transition Metal Carbonyl Clusters with Silver(I)
Graphical Abstract Feeding M−M bonds: The transition metal carbonyls Re2(CO)10 and Ir4(CO)12 form adducts with silver(I) cations, leading to the respective monocationic 2 : 1 cluster ions. Yet the structural motifs differ: insertion and bent-coordination for Re but edge-coordination for Ir. Both are discussed and further analyzed with computational methods.
Teaching old tricks to new dogs - rational synthesis of multi-decker complexes featuring cyclo-P5 decks
Teaching old tricks to new dogs – rational synthesis of multi-decker complexes featuring cyclo-P5 decks† Christoph Riesinger,a David Röhner,b Ingo Krossing b and Manfred Scheer *a Abstract A rational synthetic pathway towards a series of cyclo-P5-bearing multi-decker complexes was developed.
Cationic dialanes with fluxional π-bridged cyclopentadienyl ligands
Cationic dialanes with fluxional π-bridged cyclopentadienyl ligands† Philipp Dabringhaus, a Silja Zedlitza and Ingo Krossing*a Abstract Unique π-cyclopentadienyl bridged dialanes are synthesized as complex salts with aluminate anions by comproportionation of aluminocenium cations [AlIII(Cp)(Cp*)]+/[AlIIICp2]+ with [(AlICp*)4]. Very short Al–Al bond lengths occur in positively charged Al24+ fragments.
Cationic Dialanes with Fluxional π-Bridged Cyclopentadienyl Ligands
Cationic Dialanes with Fluxional π-Bridged Cyclopentadienyl Ligands Philipp Dabringhaus, Silja Zedlitz and Ingo Krossing Abstract Unique π-cyclopentadienyl-bridged dialanes are synthesized as complex salts with aluminate anions by comproportionation of alu-minocenium cations [AlIII(Cp)(Cp*)]+ /[AlIIICp2]+ with [(AlICp*)4]. Very short Al–Al bond lengths occur in the positively charged Al24+ fragments.
From mixed group 13 cations [M(AlCp*) 3 ] + (M = Ga/In/Tl) to an Al 4 + cluster
From mixed group 13 cations [M(AlCp*)3]+ (M = Ga/In/Tl) to an Al4+ cluster Abstract AlCp*-complexes with transition metals have shown to be highly reactive and enable C–H or Si–H bond activation. Yet, complexes of AlCp* with low-valent main-group metals are scarce. Here, we report the syntheses of [M(AlCp*)3][Al(ORF)4] (RF = C(CF3)3) with M = Ga, In, Tl, which include the first covalent Al–In and Al–Tl bonds.
Synthesis of a low-valent Al4+ cluster cation salt - Nature Chemistry
Abstract Low-valent aluminium compounds are very reactive main-group species and have therefore been widely investigated. Since the isolation of a stable molecular Al(I) compound in 1991, [(AlCp*)4] (Cp* = [C5Me5]–), a variety of highly reactive neutral or anionic low-valent aluminium complexes have been developed. By contrast, their cationic counterparts have remained difficult to access.
Oxidative Addition, Reduction and Reductive Coupling: The Versatile Reactivity of Subvalent Gallium Cations.
Oxidative Addition, Reduction and Reductive Coupling: The Versatile Reactivity of Subvalent Gallium Cations. Intrigued by the successful oxidative addition of a P-H bond to univalent Ga[Al(ORF)4] giving the unprecedented dicationic gallium hydride complex [H-Ga(PPh3)3][Al(ORF)4]2 (ORF = OC(CF3)3), the oxidative addition of E-Cl containing substrates was investigated.
Strong Lewis and Brønsted Acidic Sites in the Borosulfate Mg3[H2O→B(SO4)3]2
Abstract Borosulfates provide fascinating structures and properties that go beyond a pure analogy to silicates. Mg3[H2O→B(SO4)3]2 is the first borosulfate featuring a boron atom solely coordinated by three tetrahedra. Thus, the free Lewis acidic site forms a Lewis acid–base adduct with a water molecule. This is unprecedented for borosulfate chemistry and even for borates.
Extending the chemistry of weakly basic ligands: solvates of Ag+ and Cu+ stabilized by [Al{OC(CF3)3}4]− anion as model examples in the screening for useful weakly-interacting solvents
Extending the chemistry of weakly basic ligands: solvates of Ag+ and Cu+ stabilized by [Al{OC(CF3)3}4]− anion as model examples in the screening for useful weakly-interacting solvents Weakly Coordinating Anions (WCAs) facilitate formation of exotic “naked” cationic species. However, feasibility of the respective synthetic approaches may be limited by the basicity of solvent utilized, as the latter is one of the most important factors determining solvation ability.
A Simple Homoleptic Gallium(I) Olefin Complex: Mimicking Transition‐Metal Chemistry at a Main‐Group Metal?
Abstract The earth‐metal olefin complex [GaI(COD)2]+[Al(ORF)4]− (COD=1,5‐cyclooctadiene; RF=C(CF3)3) constitutes the first homoleptic olefin complex of any main‐group metal accessible as a bulk compound. It is straight forward to prepare in good yield and constitutes an olefin complex of a main‐group metal that—similar to many transition‐metals—may adopt the +1 and +3 oxidation states opening potential applications.
A Highly Lewis Acidic Strontium ansa‐Arene Complex for Lewis Acid Catalysis and Isobutylene Polymerization
Abstract The potential of a dicationic strontium ansa‐arene complex for Lewis acid catalysis has been explored. The key to its synthesis was a simple salt metathesis from SrI2 and 2 Ag[Al(ORF)4], giving the base‐free strontium‐perfluoroalkoxyaluminate Sr[Al(ORF)4]2 (ORF=OC(CF3)3). Addition of an ansa‐arene yielded the highly Lewis acidic, dicationic strontium ansa‐arene complex.
Building blocks for the chemistry of perfluorinated alkoxyaluminates [Al{OC(CF3)3}4]−: simplified preparation and characterization of Li+−Cs+, Ag+, NH4+, N2H5+, N2H7+ salts
Building blocks for the chemistry of perfluorinated alkoxyaluminates [Al{OC(CF3)3}4]−: simplified preparation and characterization of Li+−Cs+, Ag+, NH4+, N2H5+, N2H7+ salts Przemysław Jan Malinowski, Tomasz Jaroń, Małgorzata Domańska, John M. Slattery, Manuel Schmitt and Ingo Krossing Abstract Advanced weakly coordinating anions (WCAs) significantly facilitate synthesis of various exotic chemical compounds and novel, potentially useful materials.
Innocence is Bliss: Synthesis and Application of a very strong Perfluorinated Ammoniumyl Radical Cation in Deelectronation Chemistry.
Research Article Ingo Krossing Corresponding Author E-mail address: krossing@uni-freiburg.de Albert-Ludwigs Universität Freiburg, Institut für Anorganische und Analytische Chemie, Albertstr.
Soft Interactions with Hard Lewis acids: Generation of Mono- and Dicationic Alkaline-Earth Metal Arene-Complexes by Direct Oxidation.
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Stable Salts of Heteroleptic Iron Carbonyl/Nitrosyl Cations - A New Class of Iron Carbonyl Complexes
Communication Ingo Krossing Corresponding Author E-mail address: krossing@uni-freiburg.de Albert-Ludwigs Universität Freiburg, Institut für Anorganische und Analytische Chemie, Albertstr.
Oxidative Fluorination of Cu/ZnO Methanol Catalysts.
Communication Oxidative Fluorination of Cu/ZnO Methanol Catalysts. Ingo Krossing Corresponding Author E-mail address: krossing@uni-freiburg.de Albert-Ludwigs Universität Freiburg, Institut für Anorganische und Analytische Chemie, Albertstr. 21, 79104 Freiburg, GERMANY Search for more papers by this author PDF PDF Share Abstract The influence of a mild difluorine treatment on Cu/ZnO pre¬cata¬lysts for methanol synthesis was investigated.
Taming the Cationic Beast: Novel Developments in the Synthesis and Application of Weakly Coordinating Anions
As a service to our authors and readers, this journal provides supporting information supplied by the authors. Such materials are peer reviewed and may be re‐organized for online delivery, but are not copy‐edited or typeset. Technical support issues arising from supporting information (other than missing files) should be addressed to the authors. Please note: The publisher is not responsible for the content or functionality of any supporting information supplied by the authors.
Taming the Cationic Beast: Novel Developments in the Synthesis and Application of Weakly Coordinating Anions
As a service to our authors and readers, this journal provides supporting information supplied by the authors. Such materials are peer reviewed and may be re‐organized for online delivery, but are not copy‐edited or typeset. Technical support issues arising from supporting information (other than missing files) should be addressed to the authors. Please note: The publisher is not responsible for the content or functionality of any supporting information supplied by the authors.
Angewandte Chemie International Edition
This Review provides a unified view on Brønsted acidity. For this purpose, a brief overview of the concepts acidity, acid strengths, and pH value is given, including problems, proposed solutions, and the use of the pH / scale as a unifying concept. Thereafter, some examples of the accessibility and application of unified pH values are given. The Review is rounded off with the analogy of acid‐base chemistry to redox chemistry with the introduction of the unified redox scale pe .
Angewandte Chemie International Edition
This Review provides a unified view on Brønsted acidity. For this purpose, a brief overview of the concepts acidity, acid strengths, and pH value is given, including problems, proposed solutions, and the use of the pH / scale as a unifying concept. Thereafter, some examples of the accessibility and application of unified pH values are given. The Review is rounded off with the analogy of acid‐base chemistry to redox chemistry with the introduction of the unified redox scale pe .
Taming the Cationic Beast: Novel Developments in the Synthesis and Application of Weakly Coordinating Anions
This review gives a comprehensive overview of the most topical Weakly Coordinating Anions (WCAs) and contains information on WCA design, stability and applications. As an update to the 2004 review, developments in common classes of WCA are included. Methods for the incorporation of WCAs into a given system are discussed and advice on how to best choose a method for introduction of a particular WCA.
The Ideal Ionic Liquid Salt Bridge for the Direct Determination of Gibbs Energies of Transfer of Single Ions, Part I: The Concept
We describe a procedure for the thermodynamically rigorous, experimental determination of the Gibbs Energy of Transfer of single ions between solvents. The method is based on potential difference measurements between two electrochemical half cells with different solvents connected by an ideal Ionic Liquid Salt Bridge (ILSB). We discuss the specific requirements for the IL with regard to the procedure, ensuring that the Liquid Junction Potentials (LJP) at both ends of the ILSB cancel largely.
The Ideal Ionic Liquid Salt Bridge for the Direct Determination of Gibbs Energies of Transfer of Single Ions, Part II: Evaluation of the Role of Ion Solvation and Ion Mobilities - Ermantraut - 2017 - Angewandte Chemie International Edition - Wiley Online
An important intermediate goal to evaluate our concept for the assumption-free determination of single ion Gibbs transfer energies ?trG°(i, S1 > S2) is presented: We executed the crucial steps a) and b) of the methodology, described in Part I of this treatise, exemplarily for Ag+ and Cl? with S1 being water and S2 being acetonitrile.
Angewandte Chemie International Edition
We report on a unified view on Brønsted acidity introduced by our group in this journal in 2010, its perception in the view of a synthetic/materials chemist contrasted by that of a physical or a theoretical chemist, and the discrepancy between both views. For this purpose, we provide a brief overview of the concepts acidity, acid strengths, and pH value, including problems, proposed solutions, and the pH_abs/pH_abs^H2O scale as a unifying concept developed in our group.
Catalytic Use of Low-Valent Cationic Gallium(I) Complexes as π-Acids
Transformations of alkene and alkyne substrates relevant to ?-Lewis acid catalysis have been performed using low-valent Ga(I) species for the first time. [Ga(I)(PhF) ]+[Al(ORF) ]? and gallium dichloride (i.?e. [Ga(I)]+[GaCl ]?) proved to be efficient catalysts for cycloisomerizations, Friedel-Crafts reactions, transfer hydrogenations, and reductive hydroarylations. Their activity is compared to more common Ga(III) complexes.
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