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Karel Škoch, Ivana Císařová, Filip Uhlík, Petr Štěpnička
Isomeric phosphinoferrocene ligands, viz. 1'-(diphenylphosphino)-1-cyanoferrocene (1) and 1'-(diphenylphosphino)-1-isocyanoferrocene (2), show markedly different coordination behaviours. For instance, the reactions of 1 with [PdCl2(MeCN)2] and [(LNC)Pd(μ-Cl)]2 (LNC = [2-(dimethylamino-κN)methyl]phenyl-κC1) produced the "phosphine" complexes [PdCl2(1-κP)2] (7) and [(LNC)PdCl(1-κP)] (8), and the latter was converted into the coordination polymer [(LNC)Pd(μ(P,N)-1)][SbF6] (9). Conversely, the reaction of 2 with [(LNC)Pd(μ-Cl)]2 involved coordination of the phosphine moiety and simultaneous insertion of the isocyanide group into the Pd-C bond, giving rise to the P,η1-imidoyl complex [PdCl(Ph2PfcN[double bond, length as m-dash]CC6H4CH2NMe2-κ3C,N,P)] (10; fc = ferrocene-1,1'-diyl)...
October 10, 2018: Dalton Transactions: An International Journal of Inorganic Chemistry
Petre Flaviu Gostin, Owen Addison, Alexander P Morrell, Yue Zhang, Angus J M C Cook, Alethea Liens, Mihai Stoica, Konstantin Ignatyev, Steven R Street, Jing Wu, Yu-Lung Chiu, Alison J Davenport
Ti-based bulk metallic glasses are under consideration for implants due to their high yield strength and biocompatibility. In this work, in situ synchrotron X-ray diffraction (XRD) is used to investigate the corrosion products formed from corrosion of Ti40 Zr10 Cu34 Pd14 Sn2 bulk metallic glass in artificial corrosion pits in physiological saline (NaCl). It is found that Pd nanoparticles form in the interior of the pits during electrochemical dissolution. At a low pit growth potential, the change in lattice parameter of the Pd nanoparticles is consistent with the formation of palladium hydride...
September 16, 2018: Advanced Healthcare Materials
Sadeeq Ullah, Aftab Ahmad, Arifullah Khan, Jie Zhang, Muslim Raza, Aziz Ur Rahman, Muhammad Tariq, Usman Ali Khan, Shah Zada, Qipeng Yuan
Low cost and an easy technique for the synthesis of palladium nanoparticles (PdNPs) was developed. Glucosamine was used to stabilize palladium precursor (PdCl2 ) into palladium nanoparticles. Several analytical techniques were used for the determination of morphology, crystalline structure; size, capping, and composition of synthesize palladium nanoparticles. The UV-visible spectroscopy SPR peak (Surface Plasmon Resonance) at 284 nm revealed synthesis of PdNPs. Energy dispersive X-ray (EDX) and X-ray diffraction (XRD) studies proved the elemental composition and crystalline structure of the synthesized palladium nanoparticles respectively...
September 12, 2018: Microbial Pathogenesis
Yasunari Monguchi, Tomohiro Ichikawa, Tsuyoshi Yamada, Yoshinari Sawama, Hironao Sajiki
Microwave-assisted continuous-flow reactions have attracted significant interest from synthetic organic chemists, especially process chemists from practical points of view, due to a less complicated shift to large-scale synthesis based on simple and continuous access to products with low energy requirements. In this personal account, we focused on the Suzuki-Miyaura and Mizoroki-Heck reactions, both of which are significantly important cross-coupling reactions for the synthesis of various functional materials...
September 4, 2018: Chemical Record: An Official Publication of the Chemical Society of Japan ... [et Al.]
Tao Zhang, Guigang Deng, Hanjie Li, Bingxin Liu, Qitao Tan, Bin Xu
A palladium-catalyzed synthesis of dibenzothiophenes from 2-biphenylthiols is described. This highly efficient reaction employs a simple PdCl2 /DMSO catalytic system, in which PdCl2 is the sole metal catalyst and DMSO functions as an oxidant and solvent. This transformation has broad substrate scope and operational simplicity and proceeds in high yield. The synthetic utility was demonstrated by the facile synthesis of helical dinapthothiophene 3 and an eminent organic semiconductor DBTDT 4. Importantly, highly strained trithiasumanene 5, a buckybowl of considerable synthetic challenge, was observed under this catalytic system...
September 7, 2018: Organic Letters
Rena Simayi, Simone M Gillbard, Warren B Cross, Eric G Hope, Kuldip Singh, Gregory A Solan
The pyridylimine-substituted 1-naphthalenes, 2-(1-C10H7)-6-{CR[double bond, length as m-dash]N(2,6-i-Pr2C6H3)}C5H3N (R = Me HLMe, H HLH), react with Na2[PdCl4] in acetic acid at elevated temperature to afford either ortho-C-Hnaphthyl activated (LMe)PdCl (2ortho) or the unactivated adduct (HLH)PdCl2 (1b). Alternatively, 1b and its ketimine analogue (HLMe)PdCl2 (1a), can be prepared by treating (MeCN)2PdCl2 with either HLMe or HLH in chloroform at room temperature. Regio-selective ortho-C-H activation to form 2ortho can also be initiated by the thermolysis of 1a in acetic acid, while no reaction occurs under similar conditions with 1b...
August 21, 2018: Dalton Transactions: An International Journal of Inorganic Chemistry
Vnira Rakhimovna Akhmetova, Rozalia Akramovna Galimova, Nail Salavatovich Akhmadiev, Albina Midkhatovna Galimova, Ravil Akhmetzyanovich Khisamutdinov, Galiya Maratovna Nurtdinova, Eduard Feliksovich Agletdinov, Valery Alekseevich Kataev
Purpose: This research is devoted to designing the synthesis of sulfanyl-substituted 3,5-dimethylisoxazoles, which contain structural analogues of the SAM drug in the molecule. SAM (S-adenosyl-L-methionine), formed in the biosynthetic process, is used as an effective hepatoprotective drug. Complexation and hepatoprotective properties of the combinatorial series of bis(isoxazolylsulfanyl)ethane have been studied. Methods: Bis(isoxazol-4-ylmethylsulfanyl)alkanes were synthesized using the one-pot method. The structures of compounds were established by one-dimensional (1 H,13 C) and two-dimensional (COSY, HCQS, HMBC) NMR spectroscopy, mass-spectrometry and X-ray diffraction...
June 2018: Advanced Pharmaceutical Bulletin
Sheng Zhang, Hengmin Ma, Hon Eong Ho, Yoshinori Yamamoto, Ming Bao, Tienan Jin
A new and efficient Pd-catalyzed cascade cyclization of biaryl-tethered o-alkynylanilines for the formation of dibenzo[a,c]carbazole derivatives has been reported. The use of the alkyl-substituted tertiary anilines together with the combination of the PdCl2 catalyst with the MnO2 oxidant and PivOH is vital for giving rise to 5-endo cyclization, C-N bond cleavage, and C-H bond activation in a cascade manner to produce the corresponding products with structural diversity.
July 25, 2018: Organic & Biomolecular Chemistry
Sunit Kumar, Kishor G Thorat, Way-Zen Lee, Mangalampalli Ravikanth
A new nonaromatic selenabenziporphyrin was synthesized by (3 + 1) condensation of m-benzitripyrrane and 2,5-bis[( p-tolyl)hydroxymethyl] selenophene under mild trifluoroacetic acid-catalyzed reaction conditions. The selenabenziporphyrin was characterized by high-resolution mass spectrometry, one- and two-dimensional NMR spectroscopy, and X-ray crystallography. The crystal structure revealed that the macrocycle was planar with moderately tilted m-phenylene ring and that the phenylene ring completely blocks the macrocyclic π-delocalization...
August 6, 2018: Inorganic Chemistry
Oishi Jana, Ganesan Mani
2,6-Bis(3,5-dimethylpyrazoylmethyl)-4-methylphenol LH was readily synthesized by the reaction between 2,6-bis[(dimethylamino)methyl]-4-methylphenol and 3,5-dimethylpyrazole. The X-ray structure of the trisodium complex of LH showed the benzene-like planar Na3 O3 ring with alternative shorter (2.181-2.185 Å) and longer (2.244-2.263 Å) bonds. The reaction of anionic ligand L with [PdCl2 (COD)] yielded three Pd(II) complexes: [Pd{OC6 H2 (CH2 PzMe2 )2 -2,6-Me-4-κ N, O}2 ] (1), [PdCl{μ-OC6 H2 (CH2 PzMe2 )2 -2,6-Me-4-κ N, O, N}]2 (2), and [PdCl2 {μ-OC6 H2 (CH2 PzMe2 )2 -2,6-Me-4-κ N, O, N}2 Pd] (3) (PzMe2 = 3,5-dimethylpyrazole)...
July 2, 2018: Inorganic Chemistry
Ioannis Bratsos, Christos Tampaxis, Ioannis Spanopoulos, Nicola Demitri, Georgia Charalambopoulou, Dionisios Vourloumis, Theodore A Steriotis, Pantelis N Trikalitis
The targeted synthesis of metal-organic frameworks (MOFs) with open metal sites, following reticular chemistry rules, provides a straightforward methodology toward the development of advanced porous materials especially for gas storage/separation applications. Using a palladated tetracarboxylate metalloligand as a 4-connected node, we succeeded in synthesizing the first heterobimetallic In(III)/Pd(II)-based MOF with square-octahedron (soc) topology. The new MOF, formulated as [In3 O(L)1.5 (H2 O)2 Cl]·n(solv) (1), features the oxo-centered trinuclear clusters, [In3 (μ3 -O)(-COO)6 ], acting as trigonal-prismatic 6-connected nodes that linked together with the metalloligand trans-[PdCl2 (PDC)2 ] (L4- ) (PDC: pyridine-3,5-dicarboxylate) to form a 3D network...
June 18, 2018: Inorganic Chemistry
Pengfei Ai, Kirill Yu Monakhov, Jan van Leusen, Paul Kögerler, Christophe Gourlaouen, Moniek Tromp, Richard Welter, Andreas A Danopoulos, Pierre Braunstein
Selective copper(I) to palladium(0) transmetallation of P-donors from the rigid N,N'-diphosphanyl-imidazol-2-ylidene C3 H2 [NP(tBu)2 ]2 (PCNHC P) was observed when known [Cu3 (μ3 -PCNHC P,κP,κCNHC ,κP)2 ](OTf)3 was reacted with [Pd(PPh3 )4 ]. When 1.2 equivalents of [Pd(PPh3 )4 ] was used, the product [Cu2 Pd(μ3 -PCNHC P,κP,κCNHC ,κP)2 ](OTf)2 (2(OTf)2 ) was obtained, which features a CuI -CuI -Pd0 chain and appears to be the first linear heterotrinuclear complex with d10 -d10 interactions between Pd0 and CuI ...
June 21, 2018: Chemistry: a European Journal
Madhusudan K Pandey, Joel T Mague, Maravanji S Balakrishna
The synthesis of sterically demanding aminophosphine and phosphinite ligands Ar*NHPPh2 (1) and Ar*OPPh2 (2), based on 2,6-dibenzhydryl-4-methylphenyl core having bulky benzhydryl groups, and their RuII , PdII and PtII complexes is described. The reactions of 1 and 2 with [Ru(η6 - p-cymene)Cl2 ]2 in 2:1 molar ratios produced mononuclear complexes [RuCl2 {(η6 - p-cymene)PPh2 -EAr*}-κ1 -P] (E = NH (3) and O (4)). Interestingly, complexes 3 and 4, upon refluxing in chlorobenzene, displace the p-cymene ring by one of the phenyl rings of side arms, forming rare η6 -arene coordinated tethered complexes [RuCl2 {(PPh2 -EAr*)-κ1 -P-η6 -arene}] (E = NH (5) and O (6))...
June 18, 2018: Inorganic Chemistry
Austin Bonnette, Joel T Mague, Perumalreddy Chandrasekaran
A palladium(II) complex {systematic name: dichlorido[1,3-di- tert -butyl-2,4-bis( tert -butylamino)-1,3,2λ5 ,4λ5 -diazadiphosphetidine-2,4-diselone-κ2 Se , Se ']pal-ladium(II)}, cis -[PdCl2 { I }], ( II ), containing a bis-(selenium) ligand based on cyclo-diphosph(V)azane, cis -[( t BuNH)(Se)P(μ-N t Bu)2 P(Se)(NH t Bu)], ( I ), has been synthesized and structurally characterized. The crystal structure of complex II reveals that the ligand chelates through selenium donors with the natural bite-angle of 110...
February 1, 2018: Acta Crystallographica. Section E, Crystallographic Communications
Alexander G R Howe, Peter J Miedziak, David J Morgan, Qian He, Peter Strasser, Jennifer K Edwards
A series of 1 wt% supported Au, Pd and AuPd nanoalloy catalysts were prepared via microwave assisted reduction of PdCl2 and HAuCl4 in a facile, one pot process. The resulting materials showed excellent activity for the direct synthesis of hydrogen peroxide from hydrogen and oxygen, with a synergistic effect observed on the addition of Au into a Pd catalyst. Detailed electron microscopy showed that the bimetallic particles exhibited a core-shell morphology, with an Au core surrounded by an Au-Pd shell, with a size between 10-20 nm...
September 3, 2018: Faraday Discussions
Alexander S Mikherdov, Mikhail A Kinzhalov, Alexander S Novikov, Vadim P Boyarskiy, Irina A Boyarskaya, Margarita S Avdontceva, Vadim Yu Kukushkin
The reaction of cis-[PdCl2 (CNXyl)2 ] (Xyl = 2,6-Me2 C6 H3 ) with the aminoazoles [1 H-imidazol-2-amine (1), 4 H-1,2,4-triazol-3-amine (2), 1 H-tetrazol-5-amine (3), 1 H-benzimidazol-2-amine (4), 1-alkyl-1 H-benzimidazol-2-amines, where alkyl = Me (5), Et (6)] in a 2:1 ratio in the presence of a base in CHCl3 at RT proceeds regioselectively and leads to the binuclear diaminocarbene complexes [(ClPdCNXyl)2 {μ-C(N-azolyl)N(Xyl)C═NXyl}] (7-12; 73-91%). Compounds 7-12 were characterized by C, H, N elemental analyses, high-resolution ESI+ -MS, Fourier transform infrared spectroscopy, 1D (1 H, 13 C) and 2D (1 H,1 H-COSY, 1 H,1 H-NOESY, 1 H,13 C-HSQC, 1 H,13 C-HMBC) NMR spectroscopies, and X-ray diffraction (XRDn)...
June 4, 2018: Inorganic Chemistry
Magdalena Staniszewska, Stephan Kupfer, Julien Guthmuller
Time-dependent density functional theory calculations combined with the Marcus theory of electron transfer (ET) were applied on the molecular photocatalyst [(tbbpy)2 Ru(tpphz)PdCl2 ]2+ in order to elucidate the light-induced relaxation pathways populated upon excitation in the longer wavelength range of its absorption spectrum. The computational results show that after the initial excitation, metal (Ru) to ligand (tpphz) charge transfer (MLCT) triplet states are energetically accessible, but that an ET toward the catalytic center (PdCl2 ) from these states is a slow process, with estimated time constants above 1 ns...
August 1, 2018: Chemistry: a European Journal
Christian W Lopes, Jose L Cerrillo, Antonio E Palomares, Fernando Rey, Giovanni Agostini
The activation of precursor-dependent Pd nanoparticles was comprehensively followed by in situ X-ray absorption spectroscopy on two inorganic supports for rationalizing the final catalytic activity. Two series of Pd-based catalysts (7 wt% Pd) were prepared by impregnation of γ-Al2O3 and activated carbon supports varying the metal precursor (Pd(NO3)2, PdCl2 and Pd(OAc)2). The most relevant physicochemical properties of the studied catalysts were determined by several techniques including ICP-OES, XRD, N2 adsorption and XAS...
May 9, 2018: Physical Chemistry Chemical Physics: PCCP
Mi Yeon Byun, Ji Sun Kim, Dae-Won Park, Man Sig Lee
The increasing role of catalysis by noble metals coupled with their high price requires the development of cheaper and more effective catalysts, e.g., highly dispersed supported catalyst. Herein, Pd supported on Al2O3 catalysts prepared by deposition-precipitation under different conditions were subjected to X-ray diffraction, N2-physisorption, NH3/CO2 temperature programmed desorption, CO-chemisorption, and field-emission transmission electron microscopy analyses, which revealed that the size and distribution of Pd particles were influenced by Al2O3 support type (particle size and phase transition) and preparation conditions (metal precursor type, pH value, and solution temperature)...
September 1, 2018: Journal of Nanoscience and Nanotechnology
Yongyi Wei, Zhan Mao, Zhenzhong Li, Fang Zhang, Hexing Li
Heterogeneous organometallic catalysts with well-defined active sites and hierarchical pores hold tremendous promise for efficient and eco-friendly chemical processes. However, the simple and scalable preparation of these materials remains difficult to date, which has hampered a more broad application scope. Herein, we reported a low-cost, rapid, and scalable aerosol-assisted assembly approach for the synthesis of a well-defined PdDPP (PdCl2 (PPh2 (CH2 )2 ))_ complex-containing benzene-bridged organosilica-based catalyst with a hierarchical bimodal micro-macroporous structure...
April 25, 2018: ACS Applied Materials & Interfaces
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