Synthesis and structural characterisation of unprecedented primary <i>N</i>-nitrosamines coordinated to iridium(<scp>iv</scp>)

Foi, Ana; Salvo, Florencia Di; Doctorovich, Fabio; Huck‐Iriart, Cristián; Ramallo‐López, José M.; Dürr, Maximilian; Stirnat, Kathrin; Garbe, Simon; Klein, Axel

doi:10.1039/c8dt02549e

Cited by 5 publications

(2 citation statements)

References 44 publications

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“…In the last decade, several reports using commercial or in-house built lab-based XAS and XES spectrometers have been published. These works have demonstrated the usefulness of lab-based XAS instrumentation for studying catalytic systems, in particular when complemented by other laboratory techniques or in certain cases with XAS data collected at synchrotron facilities [208,209,[227][228][229][230][231][232][233][234][235][236][237][238][239][240][241][242][243][244][245].…”

Section: Characterisation Opportunities In Laboratories To Allow For a More Efficient Synchrotron Beam Time Usagementioning

confidence: 99%

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

Zimmermann

Peredkov

Abdala

et al. 2020

Coordination Chemistry Reviews

162

140

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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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Section: Characterisation Opportunities In Laboratories To Allow For a More Efficient Synchrotron Beam Time Usagementioning

confidence: 99%

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

Zimmermann

Peredkov

Abdala

et al. 2020

Coordination Chemistry Reviews

162

140

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“…The important observation of slow magnetic relaxation for these salts compared to all the previously observed LRO magnets raises an important question of what are the limiting factors for this big difference. Moreover, Ir IV -based molecular materials have rarely been reported and the reports rarely include magnetic studies. − Therefore, it is well worth establishing magnetostructural correlation by developing Ir IV -based molecular magnetic materials.…”

Section: Introductionmentioning

confidence: 99%

Incorporating Paramagnetic Ir^IVCl₆^2– in H-Bonded Networks of Metal-Phosphonate Hydrate: Slow Magnetic Relaxation and Proton Conduction

Liu

Huang

Bao

et al. 2019

Crystal Growth & Design

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The large spin−orbital coupling and spatially extended valence orbitals of the Ir IV (5d 5 , S = 1/2 and L = 1) are parameters responsible for its interesting magnetism in addition to the geometrical arrangements in the crystals. In order to study the effect of the Ir•••Ir distance on the magnetic behavior of Ir IV Cl 6 2− species, we made use of diamagnetic supramolecular hosts of Co III Ca II (notpH x ) [notpH 6 = C 9 H 18 N 3 (PO 3 H 2 ) 3 ] to accommodate the guest anion of Ir IV Cl 6 2− . Controlling the protonation of the acid affects the Co:Ca ratio and the degree of hydration but does not affect its coordination or the geometry to the cobalt center. Consequently, three different salts have been isolated, [Co III 2 Ca II 2 (notpH 2 ) 2 (H 2 O) 8 ]-(Ir IV Cl 6 )•2H 2 O at pH 3.5 (1), [Co III 2 Ca II (notpH 3 ) 2 (H 2 O) 2 ](Ir IV Cl 6 )•4H 2 O at pH 2.5 (2), and [Co III 2 (notpH 4 ) 2 ](Ir IV Cl 6 )•6H 2 O at pH 1. 7 (3). The distance between the Ir IV Cl 6 2− anions varies in the sequence 3 < 1 < 2. Magnetic studies reveal that only 2 exhibits slow magnetic relaxation associated with Ir IV Cl 6 2− , which correlates with the large Ir•••Ir distance (9.428 Å) and the absence of a halogen bond between neighboring Ir IV Cl 6 2− (Cl•••Cl > 4.941 Å). Furthermore, the different degree of protonation in 1−3 also poses influences on their proton conductivities which increase with the protonation of the phosphonate groups under 95% RH and 25 °C.

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Spectroelectrochemistry

González‐Baró

Espino

Colina

et al. 2022

Springer Handbook of Inorganic Photochemistry

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Synthesis and structural characterisation of unprecedented primary N-nitrosamines coordinated to iridium(iv)

Cited by 5 publications

References 44 publications

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

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

Incorporating Paramagnetic Ir^IVCl₆^2– in H-Bonded Networks of Metal-Phosphonate Hydrate: Slow Magnetic Relaxation and Proton Conduction

Spectroelectrochemistry

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Synthesis and structural characterisation of unprecedented primary N-nitrosamines coordinated to iridium(iv)

Cited by 5 publications

References 44 publications

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

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

Incorporating Paramagnetic IrIVCl62– in H-Bonded Networks of Metal-Phosphonate Hydrate: Slow Magnetic Relaxation and Proton Conduction

Spectroelectrochemistry

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Incorporating Paramagnetic Ir^IVCl₆^2– in H-Bonded Networks of Metal-Phosphonate Hydrate: Slow Magnetic Relaxation and Proton Conduction