Synthesis, Characterization, and Crystal Structures of Three cis/trans Pyridine - Cyclopalladated Ferrocenylimine Complexes, and Their Catalysis in Suzuki Reactions

2007 ◽  
Vol 60 (3) ◽  
pp. 190 ◽  
Author(s):  
Chen Xu ◽  
Jun-Fang Gong ◽  
Yan-Hui Zhang ◽  
Yu Zhu ◽  
Yang-Jie Wu
Keyword(s):  
Solid State ◽  
Ir Spectra ◽  
Single Crystal ◽  
1H Nmr ◽  
Elemental Analysis ◽  
Phenylboronic Acid ◽  
Suzuki Reaction ◽  
X Ray ◽  
Suzuki Reactions ◽  
Aryl Bromides

Three new pyridine–cyclopalladated ferrocenylimine complexes 2a–c have been easily prepared and characterized by elemental analysis, ESI-MS, 1H NMR, and IR spectra. Their detailed structures are determined by single-crystal X-ray analysis. Palladacycle 2a is found to be a cis complex in the solid state, while 2b and 2c are trans complexes. These complexes were found to be efficient for the Suzuki reaction of aryl bromides with phenylboronic acid. Typically, using 0.2 mol% of 2c in the presence of 1.5 equivalents of K2CO3 as base in toluene at 100°C provided the coupled products in good to excellent yields.

N-Heterocyclic Carbene-facilated Condensation of 3-Methylphenylboronic Acid to the Boroxine

2013 ◽  
Vol 68 (5-6) ◽  
pp. 453-457 ◽  
Author(s):  
Dongxiang Zhang ◽  
Jie Li ◽  
Xiao Dong ◽  
Xing Zhou ◽  
Zhi Yang ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
1H Nmr ◽  
Elemental Analysis ◽  
1H Nmr Spectroscopy ◽  
Phenylboronic Acid ◽  
X Ray Diffraction ◽  
X Ray

The adduct of (3-MeC6H4)3B3O3 with an N-heterocyclic carbene (NHC=1,3-diethyl-4,5- dimethylimidazol-2-ylidene) was prepared by reacting 2.5 equiv. of 3-methylphenylboronic acid with 1 equiv. of the NHC. This reaction shows a novel carbene-facilitated condensation of substituted phenylboronic acid monomers. The structure of the compound (3-MeC6H4)3B3O3(NHC) (1) has been characterized by 1H NMR spectroscopy, elemental analysis, and single-crystal X-ray diffraction studies

scholarly journals 1-[N-Methyl-N-(Phenyl)amino]-3- (4-Methylphenyl)Thiourea

Molbank ◽  
10.3390/m1052 ◽  
2019 ◽  
Vol 2019 (1) ◽  
pp. M1052 ◽  
Author(s):  
Chien Yeo ◽  
Edward Tiekink
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Title Compound ◽  
Molecular Conformation ◽  
Phenyl Hydrazine ◽  
X Ray ◽  
X Ray Crystallography

The title compound, 1-[N-methyl-N-(phenyl)amino]-3-(4-methylphenyl)thiourea (1), was synthesized by the reaction of 1-methyl-1-phenyl hydrazine and 4-tolyl isothiocyanate, and was characterized by spectroscopy (1H and 13C{1H} NMR, IR, and UV), elemental analysis as well as by single crystal X-ray crystallography. In the solid state, the molecule exists as the thioamide tautomer and features an anti-disposition of the thioamide–N–H atoms; an intramolecular N–H⋯N hydrogen bond is noted. The molecular conformation resembles that of the letter L. In the molecular packing, thioamide-N1–H⋯S1(thione) hydrogen bonds lead to centrosymmetric eight-membered {⋯HNCS}2 synthons. The dimers are assembled into a supramolecular layer in the bc-plane by phenyl- and methyl-C–H⋯π(phenyl) interactions.

N–O Bond Cleavage During the Deprotonation of N,O-Bis(trimethylsilyl)hydroxylamine

2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Bond Cleavage ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Potassium Hydride ◽  
Oxygen Atoms

The reaction of N,O-bis(trimethylsilyl)hydroxylamine with potassium hydride in pentane affords a product of the formula {K6[OSiMe3]4[ON(SiMe3)2]2}, resulting from deprotonation followed by N-O bond cleavage and 1,2-silylshift. The compound was characterised by elemental analysis and by single crystal X-ray diffraction. The aggregate consists of a K3O3 bis-cubane core, with N(SiMe3)2 groups at the oxygen atoms shared by the two cubes, andMe3Si groups attached to the four O vertices. Two weak K···N interactions are also detected in the solid state structure.

Room Temperature Suzuki Reactions in Aqueous Media under Air by Palladium(II) Complexes with Pyrazole Derived Ligands

2010 ◽  
Vol 63 (2) ◽  
pp. 315 ◽  
Author(s):  
Kai Xu ◽  
Xin-Qi Hao ◽  
Jun-Fang Gong ◽  
Mao-Ping Song ◽  
Yang-Jie Wu
Keyword(s):  
Aqueous Solution ◽  
13C Nmr ◽  
Room Temperature ◽  
Phenylboronic Acid ◽  
Aqueous Media ◽  
Palladium Complexes ◽  
Coupling Reactions ◽  
X Ray ◽  
Suzuki Reactions ◽  
Aryl Bromides

Two new palladium complexes with pyrazole derived ligands 2a–2b have been easily prepared and well characterized by elemental analysis, 1H NMR, 13C NMR, and IR spectra. Their detailed structures are determined by a single-crystal X-ray analysis of 2a. The two compounds were successfully applied to the Suzuki coupling reactions of aryl bromides with phenylboronic acid, in aqueous solution at room temperature under air, giving the desired coupled products in good to excellent yields with catalyst loadings as low as 0.01–0.05 mol-%.

Synthesis, characterization, and application of palladium complexes containing 8-quinolylphosphinite ligands

2010 ◽  
Vol 88 (2) ◽  
pp. 99-103 ◽  
Author(s):  
Earl Cook ◽  
Jason D. Masuda ◽  
Aibing Xia
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Phenylboronic Acid ◽  
Suzuki Coupling ◽  
Palladium Complexes ◽  
Aryl Halides ◽  
Coupling Reactions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid State Structures

Palladium complexes containing 8-quinolylphosphinite ligands have been synthesized and characterized. Their solid state structures were determined by single-crystal X-ray diffraction. They were found to be active catalysts for Suzuki coupling reactions of phenylboronic acid and various aryl halides.

Thermochromism in copper(II) complexes: thermal, spectroscopic, solid-state broadline 1H NMR and room-temperature single-crystal x-ray analysis of bis(N,N′-dimethyl-1,2-ethanediamine)copper(II) dinitrate

Polyhedron ◽  
1993 ◽  
Vol 12 (11) ◽  
pp. 1311-1317 ◽  
Author(s):  
Subratanath Koner ◽  
Ashutosh Ghosh ◽  
Nirmalendu Ray Chaudhuri ◽  
Alok K. Mukherjee ◽  
Monika Mukherjee ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
1H Nmr ◽  
Room Temperature ◽  
X Ray

Synthesis and solid-state molecular structures of bis- and mono-nitrosobenzene complexes of ruthenium porphyrins

2002 ◽  
Vol 80 (9) ◽  
pp. 1252-1258 ◽  
Author(s):  
Jonghyuk Lee ◽  
Brendan Twamley ◽  
George B Richter-Addo
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Ir Spectra ◽  
Single Crystal ◽  
Binding Mode ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Parallel Arrangement ◽  
Ruthenium Porphyrin

Bis-nitrosobenzene complexes of the form (por)Ru(PhNO)2 (por = TPP, TTP; TPP = tetraphenylporphyrinato dianion, TTP = tetratolylporphyrinato dianion) have been prepared in good yields from the reaction of the (por)Ru(CO) precursor with excess PhNO in dichloromethane. The IR spectra of the complexes (as KBr pellets) displayed new bands at ~1348 cm–1, due to υNO. The solid-state molecular structure of (TPP)Ru(PhNO)2 was determined by single-crystal X-ray diffraction, and revealed that the PhNO ligands are bound to the Ru center via the N-binding mode. Reactions of the (por)Ru(PhNO)2 complexes with excess 1-methylimidazole gave the mono-nitrosobenzene complexes (por)Ru(PhNO)(1-MeIm). The IR spectra revealed a lowering of υNO in these mononitrosobenzene derivatives by ~27 cm–1, a feature consistent with the replacement of one π-acid PhNO ligand with the more basic 1-MeIm ligand. The solid-state molecular structure of (TPP)Ru(PhNO)(1-MeIm) reveals, in addition to the N-binding of the PhNO ligand, an essentially parallel arrangement of the C-N-O (of PhNO) and imidazole planes; this is in contrast with the (TPP)Ru(PhNO)2 complex, in which the C-N-O planes (of PhNO) are essentially perpendicular.Key words: nitroso, X-ray, ruthenium, porphyrin, imidazole.

Synthesis, structure, fluorescence, and electrochemical properties of a binuclear Ag(I) complex with 1,4-bis(benzo[d]oxazol-2-yl)butane as a ligand

2020 ◽  
Vol 75 (4) ◽  
pp. 353-357
Author(s):  
Lixian Xia ◽  
Geng Zhang ◽  
Xinzhao Xia ◽  
Yagang Li ◽  
Jiao Wang ◽  
...  
Keyword(s):  
Solid State ◽  
Ir Spectroscopy ◽  
Oxygen Atom ◽  
Single Crystal ◽  
Electrochemical Properties ◽  
Elemental Analysis ◽  
Cyclic Voltammograms ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray

AbstractReaction of 1,4-bis(benzo[d]oxazol-2-yl)butane (BBO) with [Ag(CH3CN)4(ClO4)] afforded a new binuclear silver(I) complex, with composition [Ag2(BBO)2(ClO4)2], characterized by elemental analysis, UV/Vis and IR spectroscopy, and single-crystal X-ray diffraction. The results show that the Ag(I) complex consists of a centrosymmetric dimetallacyclic structure assembled from two Ag(I) atoms and two bridging BBO ligands. The coordination environment of silver(I) complex can be described as distorted trigonal planar, with one oxygen atom from a perchlorate anion and two nitrogen atoms from two BBO ligands. The luminescence properties of the ligand and the Ag(I) complex were studied in the solid state. The emission peaks of the Ag(I) complex are attributed to ligand-centered transitions. There is no effect of the complexation except for a partial quenching. The cyclic voltammograms of the Ag(I) complex indicated an irreversible Ag+/Ag couple.

Synthesis, X-ray characterization and DFT studies of bis-N-imidazolylpyrimidine salts: the prominent role of hydrogen bonding and anion–π interactions

CrystEngComm ◽  
2014 ◽  
Vol 16 (38) ◽  
pp. 9043-9053 ◽  
Author(s):  
Francisca Orvay ◽  
Antonio Bauzá ◽  
Miquel Barceló-Oliver ◽  
Angel García-Raso ◽  
Joan J. Fiol ◽  
...  
Keyword(s):  
Hydrogen Bonding ◽  
Solid State ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Dft Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Π Interactions ◽  
New Compounds

Five new compounds have been synthesized and characterized by elemental analysis, IR, NMR and single-crystal X-ray diffraction. They present interesting assemblies in the solid state dominated by H-bonding and anion–π interactions.

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