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  • Author: Ai-Quan Jia x
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Treatment of Ru(acac)3 with 2-cyano-pyridine and 3,5-dimethyl-pyridine in the presence of zinc dust as reducing agent in refluxing THF afforded the ruthenium(II) complexes cis-[RuII(acac)2(2- CN-py)2] (1) and cis-[RuII(acac)2(3,5-Me2-py)2] (2), respectively. Interaction of Ru(acac)3 with 3- Me-pyridine and 3,5-Me2-pyridine in the presence of Br2 in refluxing THF gave the ruthenium(III) complexes [RuIII(acac)Br2(3-Me-py)2] (3) and [RuIII(acac)Br2(3,5-Me2-py)2] (4), respectively. The four complexes have been spectroscopically and electrochemically characterized, and their crystal and molecular structures have been established by X-ray crystallography

Abstract

Treatment of [(arene)Ru(μ-Cl)Cl]2 with Ph2P(S)NH(2-py) in the presence or absence of base gave two arene-ruthenium(II) complexes [(η 6-p-cymene)Ru{κ 2-N,N-Ph2P(S)N(2-py)}Cl] (1) and [(η 6-benzene)Ru{κ 1-N-Ph2P(S)NH(2-py)}Cl2] (2), which have been characterized by infrared, nuclear magnetic resonance spectroscopies, and mass spectrometry along with microanalyses. Crystal structures of Ph2P(S)NH(2-py) · ¼C6H14, 1 and 2 · ½CH2Cl2 were determined by single-crystal X-ray diffraction. Two arene-ruthenium(II) complexes were tested as precatalysts for the transfer hydrogenation of acetophenone to give 1-phenyl ethanol.

Abstract

The synthesis of three neutral bis-cyclometalated iridium(III) complexes [Ir(pba)2(S^S)] (pbaH=4-(2-pyridyl)benzaldehyde; S^S=Et2NCS2 (1), iPrOCS2 (2), (nPrO)2PS2 (3)) from [{Ir(μ-Cl)(pba)2}2] and the corresponding sodium or potassium dithiolates in methanol-dichloromethane is described. The composition of complexes 1–3 is discussed on the basis of 1H NMR, 13C NMR, IR, and mass spectroscopy, and the crystal structures of 1 and 3 were determined by X-ray crystallography. The absorption and emission spectra show that the [Ir(pba)2(S^S)] complexes may be effective candidates as green-emitting phosphorescent materials. The stability of the three cyclometalated iridium(III) complexes towards different transition metal ions was also investigated in acetonitrile-water solvent.

Abstract

Co-crystallization of C-propyl-pyrogallol[4]arene (PgC3) with 4,4′-bipyridine (bpy) in ethanol afforded a multi-component complex (PgC3) · 3(bpy) ·(EtOH) (1) that consists of a one-dimensional brick-wall framework, which was formed by four pyrogallol[4]arene molecules and two juxtaposed bpy molecules, entrapping two other bpy molecules as guests within each cavity. Heating a mixture of PgC3 and trans-1,2-bis-(4-pyridyl)ethylene (bpe) in an ethanol-water mixed solvent allowed the isolation of a multi-component complex (PgC3) ·(bpe) · 2(EtOH) ·(H2O) (2), which has a two-dimensional wave-like polymer structure with the bpe molecules embedded in the wave trough between two PgC3 molecules. Single-crystal X-ray crystallography was utilized to investigate the hydrogen bonding networks of the multi-component complexes 1 and 2.

Abstract

Interaction of AgCl with bis(diphenylphosphino)methane (dppm) in THF/MeCN in the presence of K[PF6] or [Et4N]Br afforded typical trinuclear cationic trigonal-bipyramidal complexes [Ag3(μ 3-Cl)2(μ-dppm)3][PF6] (1) or [Ag3(μ 3-Br)2(μ-dppm)3][AgBr2] (2), respectively. Treatment of AgBr with bis(diphenylphosphino)ethane (dppe) in THF/MeCN in the presence of [Et4N]Br gave a polymeric complex {[Et4N][Ag2(μ-Br)3(μ-dppe)]}n (3) with a dinuclear {Ag2(μ-Br)3} core. The reaction of AgCl with dppe or bis(diphenylphosphino)propane (dppp) in THF/MeCN in the presence of [Et4N]Cl resulted in the isolation of a dinuclear anionic complex [Et4N]2[(AgCl2)2(μ-dppe)] (4) with one μ-dppe bridge or a dinuclear neutral complex [(AgCl)2(μ-dppp)2] (5) with two μ-dppp bridges and a 12-membered ring, respectively. The structures of complexes 1–5 with the bidentate phosphine ligands were determined by single-crystal X-ray diffraction.

Abstract

The reaction of [PPh4]2[WS4] in CH3CN with excess n-propylbromide or n-butylbromide gave alkylthiolatotrithiotungstate complexes, [PPh4][WS3(SR)] (1: R=n-propyl; 2: R=n-butyl). The analogous reaction with 1-bromomethyl-4-chloromethyl-benzene afforded a benzylthiolatotrithiotungstate complex, [PPh4][WS3(SCH2C6 H4CH2Cl-4)] (3), whereas the reaction with 1,4-bis-bromomethyl-benzene led to isolation of a dinuclear complex [PPh4]2[WS3(μ-SCH2C6H4CH2S)WS3] (4). Complexes 1–4 were characterized spectroscopically and the crystal structures of 1/2·½C6H6 and 3 have been determined by X-ray diffraction.

Abstract

Treatment of [Ru(acac)3] (acac=acetylacetonate) with (2,4,5-Me3C6H2)MgBr, followed by column chromatography in air, afforded the homoleptic tetraaryl-ruthenium(IV) complex [Ru(2,4,5-Me3C6H2)4] (1) in moderate yield. The product was characterized by proton NMR spectroscopy and microanalyses. Its crystal structure has also been established by X-ray crystallography.

Abstract

Treatment of cis-[RuCl2(phen)2]·2H2O (phen=1,- 10-phenanthroline) with 1-(2,6-diisopropylphenoxy)-4-phenylphthalazine (HL1) or 1-(2,6-dimethylphenoxy)-4-phenylphthalazine (HL2) in the presence of AgPF6 afforded two cyclometalated ruthenium(II) complexes, [Ru(κ 2-C,N-L1)(phen)2](PF6) (1) and [Ru(κ 2-C,N-L2)(phen)2](PF6) (2), respectively. The two complexes have been characterized by UV–vis and luminescence spectroscopy. The structure of 1·1.5H2O has been determined by single-crystal X-ray diffraction.

Abstract

Interaction of (NH4)6Mo7O24·4H2O with tris-(3,5-di-tert-butyl-2-hydroxy-benzylidene)triaminoguanidinium chloride [H6 tBu6L]Cl in DMF-H2O resulted in isolation of a neutral dinuclear Mo(VI) complex [Mo2O4(OH2)(DMF)(HtBu6L)]·3DMF. The C 3-symmetric-type ligand HtBu6L is coordinated to two cis-{MoO2}2+ moieties via phenolic-oxygen, guanidine nitrogen and azomethine nitrogen atoms, and the remaining sixth coordination sites of the molybdenum centers are occupied by the oxygen atoms from the solvent molecules.

Abstract

A self-assembly reaction of Cd(NO3)2 · 4H2O, 3-ferrocenyl-5-(2-pyridyl)-pyrazole (Hfcpp), [Ag(SePh)]n, and Et3N in a mixed acetone-water solvent resulted in the formation of a heterometallic complex [Cd2{Ag(SePh)}2 (μ 3-OH2)2(μ 2,η 3-fcpp)4] · 2C3H6O (1) with a phenylselenolate ligand. The two cadmium and two silver centers are linked by four [μ 2,η 3-fcpp] ligands and two μ 3-OH2 water molecules. Each Cd atom is in a slightly distorted octahedral coordination environment, while each Ag atom shows a distorted tetrahedral coordination geometry, which is composed of two pyrazolyl nitrogen atoms, one selenium atom, and one oxygen atom.