The distinction between valence electrons and essentially inactive core electrons is the basis of many classifying concepts in chemistry. However, it has recently been recognized that this is an oversimplification and should, at least in some areas of chemistry, be modified. Many cases are known where cations with closed d10 configurations are subject to homoatomic interactions that influence structure and properties. A characteristic and surprisingly uniform structural feature (e.g., of a number of compounds containing monovalent coinage metals) is a clusterlike assembly of d10 cations that corresponds in geometry and bond lengths to fragments of the metal structures themselves. Further evidence for a special type of bonding in such compounds is provided by their physical properties; for example, the absorption in the UV/VIS region shows a drastic redshift and the compounds are often conductors or semiconductors. The d electrons in such cases have obviously lost their pure “core” nature. All bonding models so far proposed for such systems involve mixing of higher orbitals.

Homoatomic d10–d10 Interactions: Their Effects on Structure and Chemical and Physical Properties

Homoatomare d10‐d10‐Wechselwirkungen — Auswirkungen auf Struktur‐ und Stoffeigenschaften

Oxocuprate wurden vor einigen Jahren einfach nur als chemische Stoffe wie unzahlige andere Verbindungen auch angesehen. Die Euphorie um die oxidischen Hochtemperatur (HTc)-Supraleiter und die inzwischen gewonnene Erkenntnis, das Kupfer eine essentielle Rolle in ihnen spielt, weckte weltweit das Interesse an kupferhaltigen oxidischen Substanzen. Synthese und Strukturaufklarung der Kupferoxometallate werden num nicht mehr von wenigen, sondern von vielen Wissenschaftlern betrieben. Da Supraleitung und Festkorperstruktur untrennbar miteinander verknupft sind, erwachte spontan das Interesse an der kristallchemischen Rolle des Kupfers in Festkorpern und fuhrte zu neuen Arbeiten uber Oxocuprate. Die interessante Chemie dieser Stoffgruppe wurde bisher uberwiegend fur individuelle Verbindungen publiziert. Durch die moderne Technik der dreidimensionalen Darstellung von Kristallstrukturen auf Graphic-Workstations eroffnet sich ein neues didaktisches Hilfsmittel, den komplizierten Aufbau von Festkorpern am Beispiel der Oxocuprate dem Leser in einer Ubersicht naher zu bringen.

Zur Kristallchemie von Kupferoxometallaten

Up to three or four years ago oxocuprates were a class of chemical compounds no more remarkable than countless others. Then, as a result of the euphoria surrounding the high-temperature oxide superconductors and the discovery that copper plays an essential role in these materials, there was a world-wide awakening of interest in copper-containing oxide compounds. The number of scientists engaged in the synthesis and structure determination of copper oxometalates has grown from just a few to very many. As superconductivity is inseparably connected with the structure of the solid state, there has been a spontaneous awakening of interest in the role of copper in the crystal chemistry of solid materials, leading to new research projects on this aspect of oxocuprates. Most of the work published so far on the interesting chemistry of this group of compounds has related to individual compounds. New aids in describing complex solid state structures are now available through the development of methods that give three-dimensional displays of crystal structures using computer graphics terminals, as this review illustrates for the example of the oxocuprates.

The Crystal Chemistry of Copper Oxometalates

Uniting the advantages of molecular and heterogeneous catalysts, a continuing effort in heterogeneous catalysis, has often proved to be challenging. This work introduces a facile strategy to obtain molybdenum-oxo functional groups strongly anchored on metallic copper support through in situ electrochemical reduction of a cuprous oxomolybdate thin film resulting from electroless plating. The oxomolybdate modified copper electrode exhibits enzyme-like activity and excellent stability for the hydrogen evolution reaction over the entire pH range, together with excellent mechanical properties and cost effectiveness that are needed for commercial applications, including seawater electrolysis. In situ Fourier transformed ac voltammetric study revealed two underlying MoIV/III and MoIII/II processes that are responsible for the high catalytic activity of the material. This study opens up a new avenue for designing advanced heterogeneous catalysts for a greener future using a broad range of oxometalates.

Oxomolybdate anchored on copper for electrocatalytic hydrogen production over the entire pH range

Einkristalle von Cu4Mo5O17 warden aus Cu2O und MoO3 unter Luftausschlus dargestellt. Rontgenbeugungsuntersuchungen fuhren zu trikliner Symmetrie (Raumgruppe P1, a = 6,782, b = 9,573, c = 10,948 A; α = 107,03, β = 88,40, γ = 111,02°; Z = 2). Cu4Mo5O17 unterscheidet sich kristallchemisch von den bisher bekannten CuII-Oxomolybdaten in der Koordination von Mo6+. Die Koordination von Cu+ ist nicht hantelformig, sondern tetraedrisch und oktaedrisch. Die Kristallstruktur wird beschrieben und diskutiert.



About a New Copper Molybdate: Cu4Mo5O17



Single crystals of Cu4Mo5O17 were prepared by solid state reaction of Cu2O and MoO3 in the absence of oxygen. Single crystal X-ray investigations lead to triclinic symmetry (space group P1, a = 6.782, b = 9.573, c = 10.948 A; α = 107.03, β = 88.40, γ = 111.02°, Z = 2). Cu4Mo5O17 shows crystal chemical differences in respect to the CuII-oxomolybdates. The differences concern the coordination of Mo6+. Cu+ formes not a linear OCuO group but is surrounded by oxygen tetrahedrally and octahedrally. The crystal structure is described and discussed.

Zur Kenntnis eines neuen Kupfermolybdats: Cu4Mo5O17

Die bisher unbekannte Verbindung Cu6Mo5O18 wurde in einkristalliner Form dargestellt und rontgenographisch untersucht (a = 18,884(19), b = 6,273(7), c = 15,259(23) A, β = 130,40(5)°, Raumgruppe C–C2/c, Z = 4). Die charakteristischen Strukturmerkmale werden beschrieben und im Zusammenhang mit Oxocupraten(I) diskutiert. Experimentelle und berechnete Pulverdiffraktogramme zeigen, das die fruher beschriebene Verbindung Cu6Mo4O15 tatsachlich die Zusammensetzung Cu6Mo5O18 besitzt.



Synthesis and Crystal Structure of Cu6Mo5O18



Single crystals of the hitherto unknown compound Cu6Mo5O18 were prepared and investigated by X-ray methods (a = 18.884(19), b = 6.273(7), c = 15.259(23) A, β = 130.40(5)°, space group C–C2/c, Z = 4). The typical features of the structure are described and compared with the crystal chemistry of oxocuprates(I). Observed and calculated powder patterns show that the correct composition of the earlier described compound Cu6Mo4O15 is Cu6Mo5O18.

Synthese und Kristallstruktur von Cu6Mo5O18

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Zur Kenntnis eines neuen Kupfermolybdats: Cu4Mo5O17

Synthese und Kristallstruktur von Cu6Mo5O18