An X-ray photoelectron spectroscopic study of some nickel (II) amine complexes

Roe, Stephen P.; Hill, J.O.; Liesegang, J.; Lee, A.R.

doi:10.1016/0368-2048(85)80047-5

Cited by 14 publications

(4 citation statements)

References 38 publications

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“…Compound 3 (BF 4 ) showed the characteristic peak of chloride ,, at 197.04 eV (Cl 2p 3/2 ) and at 198.40 eV (Cl 2p 1/2 ) (Figure e). Additionally, a comparison of the peaks of Ni 2p 3/2 and Ni 2p 1/2 at 854.52 and 872.06 eV for 1 (BF 4 ) 2 and 854.52 and 872.02 eV for 3 (BF 4 ) along with the corresponding satellite peaks at 860.14 and 877.54 eV for 1 (BF 4 ) 2 and 860.26 and 877.50 eV for 3 (BF 4 ) in the X-ray photoelectron spectrum of 1 (BF 4 ) 2 and 3 (BF 4 ), respectively, with the peak values reported in the literature, − confirms the oxidation state of Ni centers in both 1 and 3 to be +II. The solution magnetic moment of 1 (ClO 4 ) 2 was determined by the Evans method. , The room temperature effective magnetic moment of 4.63 μ B for 1 (ClO 4 ) 2 is very close to the spin only value of 4.89 μ B expected for an S = 2 system with ferromagnetic interaction between two high-spin Ni(II) centers.…”

Section: Resultsmentioning

confidence: 81%

Thiolate Coordination vs C–S Bond Cleavage of Thiolates in Dinickel(II) Complexes

2021

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A detailed study for the synthesis of dinickel(II)–thiolate and dinickel(II)–hydrosulfide complexes and the complete characterization of the relevant intermediates involved in the C–S bond cleavage of thiolates are presented. Hydrated Ni(II) salts mediate the hydrolytic C–S bond cleavage of thiolates (NaSR/RSH; R = Me, Et, n Bu, t Bu), albeit inefficiently, to yield a mixture of a dinickel(II)–hydrosulfide complex, [Ni2(BPMP)(μ-SH)(DMF)2]2+ (1), and the corresponding dinickel(II)–thiolate complexes, such as [Ni2(BPMP)(μ-SEt)(ClO4)]1+ (2) (HBPMP is 2,6-bis[[bis(2-pyridylmethyl)amino]methyl]-4-methylphenol). A systematic study for the reactivity of thiolates with Ni(II) was therefore pursued which finally yielded 1 as a pure product which has been characterized in comparison with the dinickel(II)–dichloride complex, [Ni2(BPMP)(Cl)2(MeOH)2]1+ (3). While the reaction of thiolates with anhydrous Ni(OTf)2 in dry conditions could only yield [Ni2(BPMP)(OTf)2]1+ (5) instead of the expected dinickel(II)–thiolate compound, the C–S bond cleavage could be suppressed by the use of a chelating thiol, such as PhCOSH, to yield [Ni2(BPMP)(SCOPh)2]1+ (6). Finally, with the suitable choice of a monodentate thiol, a dinickel(II)–monothiolate complex, [Ni2(BPMP)(SPh)(DMF)(MeOH)(H2O)]2+ (7), was isolated as a pure product within 1 h of reaction, which after a longer time of reaction yielded 1 and PhOH. Complex 7 may thus be regarded as the intermediate that precedes the C–S bond cleavage and is generated by the reaction of a thiolate with an initially formed dinickel(II)–solvento complex, [Ni2(BPMP)(MeOH)2(H2O)2]3+(4). Selected dinickel(II) complexes were explored further for the scope of substitution reactions, and the results include the isolation of a dinickel(II)–bis(thiolate) complex, [Ni2(BPMP)(μ-SPh)2]1+ (8).

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Section: Resultsmentioning

confidence: 81%

Thiolate Coordination vs C–S Bond Cleavage of Thiolates in Dinickel(II) Complexes

2021

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“…Ex situ FT-IR is employed to provide further evidence for the reversible adsorption/desorption process of ClO 4 – in NNH electrode. In the ex situ FT-IR spectra of the NNH electrode (Figure f), the peak at 1100 cm –1 belonging to ClO 4 – gradually enhances in the charge process . During the discharge process, it changes weaker gradually.…”

Section: Resultsmentioning

confidence: 96%

“…− gradually enhances in the charge process. 48 During the discharge process, it changes weaker gradually. Simultaneously, the ex situ XRD of the NNH electrode (Figure S3) shows that the crystal structure of NNH does not change.…”

Section: Acs Applied Energy Materialsmentioning

confidence: 99%

All-Climate Aqueous Dual-Ion Hybrid Battery with Ultrahigh Rate and Ultralong Life Performance

Nian

Liu

et al. 2019

ACS Appl. Energy Mater.

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Aqueous sodium ion batteries (ASIBs) with the characteristics of long cycling life, all-climate compatibility, and low cost need to be developed urgently. Herein, a novel dual-ion battery baesd on Na+ and ClO4 – electrochemistry is proposed, consisting of an nano/microstructured Ni(OH)2 (NNH) cathode, a carbon-coated NaTi2(PO4)3 (NTP@C) anode, and 2 M NaClO4 aqueous (aq.) electrolyte. In a charging process, sodium ions are inserted into NaTi2(PO4)3 to form Na3Ti2(PO4)3, and ClO4 – is stored in the electric double layers of the NNH cathode; in a reverse process, the Na+ is extracted from Na3Ti2(PO4)3 to form NaTi2(PO4)3, and the adsorption ClO4 – is released into the electrolyte. Because of the mechanism of the dual-ion reaction, the aqueous sodium-ion-based dual-ion hybrid battery (ASDHB) displays excellent rate performance, with a capacity of 82.3 mA h g–1 anode even at the ultrahigh rate of 50 C. Moreover, the ASDHB displays an ultralong cycling life at a wide temperature range (i.e., from −20 to 50 °C), even at a low temperature of −20 °C, the capacity retention is still as high as 85% after 10 000 cycles at the rate of 10 C. At the same time, it shows a high energy density of 40.1 Wh kg–1 total and power density of 257.7 W kg–1 total, indicating the potential application on electrial energy storage.

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“…21 The material 3 was also characterized by X-ray photoelectron spectroscopy (XPSFigure S3). The Ni 2p spectrum shows a peak at 854.5 eV for Ni2p 3/2 and at 872.3 eV for Ni 2p 1/2 , which is in agreement with other reported Ni(II) compounds 22 and fits well with the XANES results. Furthermore, such spectral features are also found for the starting material 1 (854.8 eV for Ni 2p 3/2 Figure S4).…”

Section: ■ Results and Discussionmentioning

confidence: 99%

Well-Defined, Silica-Supported Homobimetallic Nickel Hydride Hydrogenation Catalyst

et al. 2021

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There is an increasing interest to replace precious metal-based catalysts by earth-abundant nonprecious metals due to higher costs, toxicity, and declining availability of the former. Here, the synthesis of a well-defined supported nickel hydrogenation catalyst prepared by surface organometallic chemistry is reported. For this purpose, [LNi(μ-H)] 2 (L = HC-(CMeNC 6 H 3 ( i Pr) 2 ) 2 ) was grafted on partially dehydroxylated silica to give a homobimetallic H-and O(silica)-bridged Ni 2 complex. The structure of the latter was confirmed by infrared spectroscopy, X-ray absorption near-edge structure, and extended X-ray absorption fine structure analyses as well as hydride titration studies. The immobilized catalyst was capable of hydrogenating alkenes and alkynes at low temperatures without prior activation. As an example, ethene can be hydrogenated with an initial turnover frequency of 25.5 min −1 at room temperature.

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An X-ray photoelectron spectroscopic study of some nickel (II) amine complexes

Cited by 14 publications

References 38 publications

Thiolate Coordination vs C–S Bond Cleavage of Thiolates in Dinickel(II) Complexes

Thiolate Coordination vs C–S Bond Cleavage of Thiolates in Dinickel(II) Complexes

All-Climate Aqueous Dual-Ion Hybrid Battery with Ultrahigh Rate and Ultralong Life Performance

Well-Defined, Silica-Supported Homobimetallic Nickel Hydride Hydrogenation Catalyst

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