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Study of the conformationally flexible, wide bite-angle diphosphine 4,6-bis(3-diisopropylphosphinophenyl)dibenzofuran in rhodium(I) and palladium(II) coordination complexes

The diphosphine 4,6-bis(3-diisopropylphosphinophenyl)dibenzofuran (abbreviated as iPrDPDBFphos) was prepared and studied for its potential as a trans-chelating ligand in transition-metal coordination complexes. In the rhodium norbornadiene complex [(iPrDPDBFphos) Rh(NBD)]BF4, which has been characterized with multinuclear NMR spectroscopy, X-ray crystallography, and electrochemical studies, the ligand binds in cis fashion. In the bis(acetonitrile) complexes of rhodium and palladium [(iPrDPDBFphos)M(CH3CN)2](BF 4)n (M = Rh, Pd; n = 1, 2), the ligand adopts a trans coordination geometry. Density functional theory (DFT, M06-L) calculations predict that the trans conformer is energetically more favorable than the cis by 3.5 kcal/mol. Cyclic voltammograms of the bis(acetonitrile) Pd(II) and Rh(I) complexes contain reversible and quasi-reversible reduction events, respectively, which are preliminarily assigned as metal-based redox reactions.

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Reference£º
Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method

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Non-covalent synthesis of multiporphyrin systems

Non-covalent synthesis was used in the controlled assembly of metallodendrimers containing up to 12 porphyrins on the surface. A porphyrin containing four Pd-Cl complexes was synthesized to assemble dendrimers with a porphyrin in the nucleus. 1H NMR, ES-MS and MALDI-TOF mass spectrometry were used to characterize the nanometer-size assemblies.

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Reference£º
Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method

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Pinwheel motifs: Formation of unusual homo- and hetero-nuclear aggregates via bridging thiolates

The homohexanuclear complexes [Ni2{Ni(L1)} 4](BF4)4¡¤MeCN, 1, [Pd 2{Pd(L2)}4](BF4)4, 2, and the heteropentanuclear aggregate [Cu2{Ni(L3)} 3](PF6)2, 3, all adopt a ‘pinwheel’ type structural motif via thiolate bridging between square-planar Ni(II) or Pd(II) and between trigonal planar Cu(I) centres, respectively.

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Reference£º
Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method

In heterogeneous catalysis, the catalyst is in a different phase from the reactants. category: catalyst-palladium, At least one of the reactants interacts with the solid surface in a physical process called adsorption in such a way. 21797-13-7, name is Tetrakis(acetonitrile)palladium(II) tetrafluoroborate. In an article£¬Which mentioned a new discovery about 21797-13-7

Controlled assembly of nanosized metallodendrimers

Up to third-generation metallodendrimers can be constructed by a repetitive sequence of reactions with building blocks that contain two coordinatively unsaturated Pd centers (‘pie’ shape) and one labile, coordinating cyano group. The key steps of assembly are the displacement of the chloro ligands with AgBF4 and the in situ reaction with the cyano groups of the dendrimer building blocks to give the next generation. The resulting dendrimers have molecular masses of up to 25 kDa.

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Reference£º
Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method

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Chiral Self-Discrimination and Guest Recognition in Helicene-Based Coordination Cages

Chiral nanosized confinements play a major role for enantioselective recognition and reaction control in biological systems. Supramolecular self-assembly gives access to artificial mimics with tunable sizes and properties. Herein, a new family of [Pd2L4] coordination cages based on a chiral [6]helicene backbone is introduced. A racemic mixture of the bis-monodentate pyridyl ligand L1 selectively assembles with PdII cations under chiral self-discrimination to an achiral meso cage, cis-[Pd2L1P2L1M2]. Enantiopure L1 forms homochiral cages [Pd2L1P/M4]. A longer derivative L2 forms chiral cages [Pd2L2P/M4] with larger cavities, which bind optical isomers of chiral guests with different affinities. Owing to its distinct chiroptical properties, this cage can distinguish non-chiral guests of different lengths, as they were found to squeeze or elongate the cavity under modulation of the helical pitch of the helicenes. The CD spectroscopic results were supported by ion mobility mass spectrometry.

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Reference£º
Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method

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Alternative coordination modes in palladium(II)-diimino-bispyridine complexes with an axially chiral biphenyl backbone

The chiral biphenyl-bridged diimino-bispyridine ligands N,N?-(6,6?-dimethylbiphenyl-2,2?-diyl)bis(2-pyridylmethyl) -diimine(1)and N,N?-(6,6?-dimethylbiphenyl-2,2?-diyl)bis[(6- methyl-2-pyridyl)methyl]diimine (2) react with Pd(COD)Cl2 to give, depending on the reaction conditions, either mono- or binuclear PdCl2 complexes. In the binuclear complex 1-(PdCl2)2, the Pd nuclei are held at a distance of 3.37 A by the ligand backbone. N,N?-(6,6?-dimethylbiphenyl-2,2?-diyl) bis[(5-methyl-2-furyl) methyl]diimine (3), with furyl instead of pyridyl rings, gives mononuclear, C2-symmetric complexes only. Reactions of [Pd(NCCH3) 4]2+(BF4-)2 with ligand 1 or 3 give the C2-symmetric cations [1-Pd]2+or [3-Pd(NCCH3)2]2+, respectively, as their BF4- salts, Solid-state structures of the chloride complexes 1-PdCl2, 1-(PdCl2)2 and 3-PdCl 2, and of the complex cations [1-Pd]2+ and [3-Pd(NCCCH3)2]2+ with tetradentate and bidentate ligand coordination, respectively, all show square-planar coordination, with some distortion toward tedrahedral geometry due to the twisted biaryl-backbone. Preliminary observations on norbornene polymerization with the catalysts 1-PdCl2/MAO, 2-PdCl2/MAO and [(3-Pd(NCCH3)2]2+ suggest that a certain degree of stereoregularity of the polymers is induced by these chiral catalysts. Wiley-VCH Verlag GmbH & Co. KGaA, 2005.

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Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method

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Template-directed synthesis of a covalent organic capsule based on a 3 nm-sized metallocapsule

(Figure Presented) A 4 nm-sized covalent organic capsule having 24 pyridyl groups was synthesized in extremely high yield (43% in three steps) using an octahedron-shaped metallocapsule as a template molecule. The entity was fully characterized by NMR and MALDI-TOF MS measurements. N-Methylation of the 24 pyridyl groups of the organic capsule produced a 5 nm-sized polycationic capsule, which is larger than the neutral precursory capsule because of the electrostatic repulsion between the positive charges on the pyridinium groups of the capsule.

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Reference£º
Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method

Chemistry is an experimental science, and the best way to enjoy it and learn about it is performing experiments. Formula: C8H12B2F8N4Pd. Introducing a new discovery about 21797-13-7, Name is Tetrakis(acetonitrile)palladium(II) tetrafluoroborate

m-carborane-based chiral NBN pincer-metal complexes: Synthesis, structure, and application in asymmetric catalysis

We have succeeded in synthesizing m-carborane-based chiral NBN-pincer ligands, 1,7-bis(oxazolinyl)-1,7-dicarba-closo-dodecaborane (Carbox) (7-9). The combination of bis(hydroxyamides) and 3 equiv of diethylaminosulfur trifluoride (DAST) is a key step for cyclization to form oxazoline rings in excellent yields. X-ray crystal structures of these ligands confirmed three donor sites, one central B and two flanking N atoms in fixed positions. The electrophilic halogenation of the Carbox pincer ligands with iodine and a catalytic amount of Lewis acid led to ring-opening of the oxazolines and afforded bis(haloamides) (13 and 14). The air- and moisture-stable Carbox pincer complexes of rhodium(III), nickel(II), and palladium(II) were synthesized by the oxidative addition of RhCl3¡¤3H2O, Ni(COD)2, and Pd(CH3CN)4[BF4]2 to the Carbox pincer ligands (7-9), respectively. The catalytic activity of the rhodium(III) complexes (18-20) was examined for the asymmetric conjugate reduction of alpha,beta-unsaturated esters and reductive aldol reaction. Among these catalysts, [(S,S)-Carbox-iPr]Rh(OAc)2¡¤H2O (18) showed the highest enantioselective catalytic ability for both asymmetric conjugate reduction and reductive aldol reaction.

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Reference£º
Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method

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Ligand Aspect Ratio as a Decisive Factor for the Self-Assembly of Coordination Cages

It is possible to control the geometry and the composition of metallasupramolecular assemblies via the aspect ratio of their ligands. This point is demonstrated for a series of iron- and palladium-based coordination cages. Functionalized clathrochelate complexes with variable aspect ratios were used as rod-like metalloligands. A cubic FeII8L12 cage was obtained from a metalloligand with an intermediate aspect ratio. By increasing the length or by decreasing the width of the ligand, the self-assembly process resulted in the clean formation of tetrahedral FeII4L6 cages instead of cubic cages. In a related fashion, it was possible to control the geometry of PdII-based coordination cages. A metalloligand with a large aspect ratio gave an entropically favored tetrahedral PdII4L8 assembly, whereas an octahedral PdII6L12 cage was formed with a ligand of the same length but with an increased width. The aspect ratio can also be used to control the composition of dynamic mixtures of PdII cages. Out of two metalloligands with only marginally different aspect ratios, one gave rise to a self-sorted collection of PdII4L8 and PdII6L12 cages, whereas the other did not.

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Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method

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Electrochemical reduction of CO2 catalyzed by [Pd(triphosphine)(solvent)](BF4)2 complexes: Synthetic and mechanistic studies

The free radical addition of phosphorus-hydrogen bonds to carbon-carbon double bonds has been used to prepare a number of new tridentate ligands containing phosphorus. Reactions of these tridentate ligands with [Pd(CH3CN)4](BF4)2 yield the corresponding [Pd(tridentate)(CH3CN)](BF4)2 complexes. These complexes catalyze the electrochemical reduction of CO2 to CO in acidic dimethylformamide or acetonitrile solutions if the tridentate ligand is a linear triphosphine ligand. Complexes in which one or more of the phosphorus atoms of the tridentate ligand have been substituted with a nitrogen or sulfur heteroatom do not catalyze the electrochemical reduction of CO2. Kinetic studies on [Pd(etpC)(CH3CN)](BPh4)2 (where etpC is bis[(dicyclohexylphosphino)ethyl]phenylphosphine) show that, at acid concentrations above 1.0 ¡Á 10-2 M, the reaction is first order in catalyst. First order in CO2, and independent of acid concentration. At acid concentrations less than 4.0 ¡Á 10-3 M, the catalytic rate is first order in catalyst, second order in acid, and independent of CO2. The rate is also solvent dependent. A mechanism is proposed to account for these data. Comparison of the rate constants for catalysts with different alkyl and aryl substituents on the terminal phosphorus atoms indicates that the rate of reaction of the palladium(I) intermediates with CO2 increases with the electron-donating ability of the R groups, and that steric interactions are of less importance. In contrast, the rate constants decrease with increasing steric bulk for substituents on the central phosphorus atoms of the triphosphine ligand. Other relationships between ligand structure and catalyst activity, selectivity, and stability are also discussed. An X-ray diffraction study of the catalytic decomposition product [Pd(etp)]2(BF4)2 (where etp is bis[(diphenylphosphino)-ethyl]phenylphosphine) has been carried out. [Pd(etp)]2(BF4)2 crystallizes in the monoclinic space group P21/n with a = 13.842 (6) A, b = 28.055 (8) A, c = 19.596 (7) A, beta = 95.80 (3), v = 7571 (5) A3, and Z = 4. The structure was refined to R = 0.057 and Rw = 0.0809 for 10352 independent reflections (F > 6sigma(F)). This Pd(I) dimer is bridged by two triphosphine ligands. A dihedral angle of 67 exists between the two nearly square planar PdP3 fragments of [Pd(etp)]2(BF4)2. This dimer can be reoxidized to regenerate the catalytically active complexes.

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Reference£º
Chapter 1 An introduction to palladium catalysis,
Palladium/carbon catalyst regeneration and mechanical application method