In Situ Hydrogenation and Crystal Chemistry Studies of Co2Si Type Compounds MgPd2 and Pd2Zn

The hydrogenation properties of the intermetallic compounds MgPd₂ and Pd₂Zn, crystallizing in the Co₂Si type, were studied by in situ thermal analysis (DSC) under hydrogen pressure. Pd₂Zn does not show any reaction with hydrogen while MgPd₂ reversibly forms the hydride MgPd₂H. Neutron diffraction on the deuterides reveals the compositions MgPd₂D_0.861(6) (ambient) and MgPd₂D_0.97(1) [308(2) K, 2.56(5) MPa deuterium] with hydrogen (deuterium) occupying distorted [MgPd₅] octahedral voids. Quantum mechanical calculations support the structure models and show the hydrogenation to be exergonic for MgPd₂ and endergonic for Pd₂Zn. MgPd₂H releases hydrogen under normal conditions or vacuum. Heating under hydrogen pressure leads first reversibly to MgPd₂H_≈0.2 and subsequently irreversibly to MgPd₃H_≈1 and MgH₂. MgPd₂, Pd₂Zn, and MgPd₂H were classified in a structure map. Trends of axial ratio changes upon hydrogenation of TiNiSi type and ZrBeSi type compounds are discussed.     

DMTADAT光度法钴、钯同时测定的研究

本文提出,在高氯酸介质中,以5-(4,5-二甲基噻唑偶氮)-2.4-二氨基-甲苯(简称DMTADAT)作为显色剂进行钴,钯同时测定的新方法。在实验条件下,钴、钯与试剂形成配合物的摩尔吸光系数为ε_(CoL2)~(605)=9.3×10~4,ε_(PdL)~(610)=5.4×10~4。钴在0～10μg/25ml,钯在0～35μg/25ml浓度范围内服从比尔定律。所拟方法已成功地应用于矿样中钴、钯的同时测定。     

High-throughput quantification of palladium in water samples by ion pair based-surfactant assisted microextraction

A novel method for the determination of palladium as a metal ion model was developed by ion pair based surfactant-assisted microextraction (IP-SAME) and inductively coupled plasma-optical detection (ICP-OES). In this methodology, a cationic surfactant was used in extraction process. It has two fundamental functions: (1) the formation of an emulsified phase and (2) the ion pair formation with Pd(II) in the presence of iodide ions and making PdI₄²⁻$\text{Pd}{{\text{I}}_4}^{2-}$ extractable into organic phase (active microextraction). The effective parameters on the extraction recovery such as the types of extraction solvent and the surfactant, surfactant concentration, KI amount and HCl concentration of the sample were investigated and optimized. In the proposed approach, tetradecyl trimethyl ammonium bromide (TTAB) was used as emulsifier and ion pairing agent, and 1-octanol was selected as extraction solvent. Under the optimum conditions, the enhancement factor as large as 146 was obtained. The detection limit for palladium was 0.2 μg L⁻¹, and the relative standard deviation (RSD) was 4.1% (n = 5, C = 10.0 μg L⁻¹). The proposed method was applied for extraction and determination of palladium in different water samples.     

Synthesis,spectroscopic studies,and preliminary antibacterial assays of a palladium(II) complex with 2-mercaptothiazoline

In this article, synthesis of a palladium(II) complex with 2-mercaptothiazoline in aqueous solution is presented. Composition of the complex was defined as 1?:?2 (metal?:?ligand). Infrared and solid-state nuclear magnetic resonance indicate ligand coordination to Pd(II) through nitrogen of thiazole ring and sulfur of thiol. ESI–QTOF–mass spectrometric analysis shows primarily the dimeric form in solution. An antibiogram assay of the complex was performed by the disc diffusion method. The compound did not show antibacterial activity against the considered bacterial cells in the tested concentrations.     

Pd(thiosaccharinato)2·H2O,the first thiosaccharinato complex of a platinum-group metal

A Pd(II) complex of the thiosaccharinato (tsac) anion, of stoichiometry Pd(tsac)₂·H₂O was prepared by interaction of Na₂PdCl₄ with thiosaccharin in methanol and characterized by infrared and ¹H and ¹³C NMR spectroscopy. These spectral studies confirmed interaction of the metal center with the thiosaccharinate acting as a bidentate ligand through its thiol group and the N-atom. NMR measurements also confirmed that in solution thiosaccharin is mainly present in its thiolate tautomeric form.     

Suzuki-Miyaura cross-coupling reaction of aryl chlorides with aryl boronic acids catalyzed by a palladium dichloride adduct of N-diphenylphosphanyl-2-aminopyridine

One palladium dichloride adduct of a phosphine-pyridine ligand N-diphenylphosphanyl-2-aminopyridine (L₁) [(L₁)PdCl₂] (1) has been prepared and structurally characterized. Compound 1 can be used as an effective catalyst for the Suzuki-Miyaura cross-coupling reactions of unreactive aryl chlorides with aryl boronic acids, and worked much better than its mono- or bidentate phosphine ligands. The reactions with a wide scope of substrates proceeded to give desired products in good to excellent yields.     

Palladium(0) nanoparticles-catalyzed ligand-free direct arylation of benzothiazole via C-H bond functionalization

Palladium nanoparticles, generated in situ efficiently catalyzes direct 2-C-H arylation of benzothiazole without requirement of any ligand. A wide range of substituted aryl and heteroaryl iodides participate in this reaction producing a series of 2-aryl/heteroaryl-benzothiazoles in high yields.