Xian-Qiang Huang

Copper- and Palladium-Catalyzed Cross-Coupling Reactions for the Synthesis of N-Fused Benzo[4,5]imidazo[2,1-b]thiazole Derivatives via Substituted trans-1,2-Diiodoalkenes, 1H-Benzo[d]imidazole-2-thiols, and Halobenzenes

Two transition metal (Cu and Pd)-catalyzed C-S, C-N, and C-C bond cross-coupling reactions for the preparation of N-fused benzo[4,5]imidazo[2,1-b]thiazole derivatives were developed. A variety of 3-substituted and 2,3-disubstituted benzo[4,5]imidazo[2,1-b]thiazoles were efficiently and conveniently synthesized from the coupling reaction via trans-1,2-diiodoalkenes, 1H-benzo[d]imidazole-2-thiols, and halobenzenes in moderate to excellent yields.

4-(4-Chloro-phen-yl)-2,6-diphenyl-pyridine.

In the title compound, C23H16ClN, the crystal packing exhibits no significantly short intermolecular contacts. The benzene rings show a disrotatory arrangement and the angles between them and the pyridine ring range from 20.80 (3) to 37.56 (4)°. The Cl atom deviates by 0.01 (3) Å from the plane of the benzene ring to which it is attached.

Synthesis, crystal structure and luminescent properties of manganese 3,3′-dicarboxy-2,2′-bipyridine induced by hydrolysis of 1,10-phenanthroline-5,6-dione

The manganese coordination compound [Mn(dcb)(H2O)4] n has been obtained by hydrothermal synthesis by using Mn(CH3COO)2 · 2H2O and 1,10-phenanthroline-5,6-dione, where dcb = 3,3′-dicarboxy-2,2′-bipyridine. The results of X-ray single-crystal diffraction reveal that the title complex forms a chain-like 1D structure. The complex [Mn(dcb)(H2O)4] n crystallizes in the orthorhombic system, space group P2(1)2(1)2, with lattice parameters a = 13.896(3) Å, b = 6.3507(12) Å, c = 8.3745(15) Å, V = 739.1(2) Å3, D c = 1.659 Mg m−3, Z = 2, F(000) = 378, GOF = 0.999, R 1 = 0.0283, wR 2 = 0.0719. The photophysical properties have been investigated with fluorescence excitation and emission spectra.

A NEW METHOD TO SYNTHESIZE 3,5-DIARYLPYRAZOL DERIVATIVES

Twelve 3, 5-diarylpyrazoles have been synthesized by microwave-assisted condensation reaction in a short and concise manner using various aromatic aldehydes and aromatic ketones as starting materials. The corresponding products were obtained in good yields (87-96%). All products were identified by MS, 1H NMR, 13C NMR and elemental analysis. The advantages of this novel protocol include the excellent yield, operational simplicity, short time and the avoidance of the use of expensive catalysts.

(E)-N′-[1-(4-Chloro­phen­yl)ethyl­idene]-2-hydroxy­benzohydrazide

In the title compound, C15H13ClN2O2, the dihedral angle between the two benzene rings is 7.0 (1)°. An intramolecular N—H⋯O hydrogen bond is present and intermolecular O—H⋯O hydrogen bonds link the molecules into chains along [001].

2,4-Bis(4-chloro­benzo­yl)-1-(4-chloro­phen­yl)-3,5-di-2-thienylcyclo­hexa­nol methanol hemisolvate

The title compound, C34H25Cl3O3S2·0.5CH3OH, was synthesized by the reaction of thiophene-2-carbaldehyde with acetophenone and NaOH under solvent-free conditions, using tetrabutylammonium bromide as a phase-transfer catalyst. The central six-membered ring adopts a chair conformation with the bulky thiophene, 4-chlorophenyl and 4-chlorobenzoyl substituents in equatorial positions. The hydroxyl group is in an axial position and forms an intramolecular O—H⋯O hydrogen bond to the carbonyl group of an adjacent 4-chlorobenzoyl substituent. The methanol solvent molecules are disordered equally over two positions within one-dimensional channels, with site occupancy factors of 0.25.

A dimeric luminescent lanthanide complex [Eu(PAA)2(phen)(NO3)]2: hydrothermal synthesis, crystal structure and fluorescence

A lanthanide coordination complex [Eu(PAA)2(phen)(NO3)]2 (PAA = phenylacetic acid, phen = 1,10-phenanthroline) has been synthesized by the hydrothermal method. Single crystal X-ray diffractions show that it forms a dimeric molecular structure. The title complex crystallizes in the triclinic system, space group P 1, with lattice parameters a = 8.9473(8) Å, b = 13.3659(12) Å, c = 13.4745(12) Å, α = 60.7590(10)°, β = 89.5100(10)°, γ = 71.9850(10)°, V = 1317.3(2) Å3, D c = 1.675 Mg m−3, Z = 1, F(000) = 660, GOF = 1.003, R 1 = 0.0206, wR 2 = 0.0575. The fluorescence excitation and emission spectra have been investigated.

Tetrakis[(benzene-18-crown-6)potassium]bis[tris(thiocyanato)copper(I)].

The title complex, bis(μ-benzene-18-crown-6)-3κ6 O:4κO;4κ6 O:3κO-bis(benzene-18-crown-6)-1κ6 O,6κ6 O-tetra-μ-thiocyanato-1:2κ2 S:N;2:3κ2 N:S;4:5κ2 S:N;5:6κ2 N:S-dithiocyanato-2κN,5κN-2,5-dicopper(I)-1,3,4,6-tetrapotassium(I), [K4Cu2(NCS)6(C16H24O6)4] or {[K(C16H24O6)]4[Cu(NCS)3]2}, consists of four [K(benzene-18-crown-6)]+ cations and two [Cu(NCS)3]2− anions, forming a dimeric structure with site symmetry . In each [Cu(NCS)3]2− anion, the CuI atom is coordinated by three N atoms of thiocyanate ligands in a trigonal–planar coordination geometry. Each [Cu(NCS)3]2− anion bridges two [K(benzene-18-crown-6)]+ cations, with K—S distances of 3.317 (3) and 3.198 (3) Å, and two [K(benzene-18-crown-6)]+ cations are linked across a crystallographic centre of inversion, with K—O distances of 2.903 (5) Å.

1,1′-[o-Phenyl­enebis(nitrilo­methyl­idyne)]di-2-naphthol ethanol hemisolvate

The asymmetric unit of the title compound, C28H20N2O2·0.5C2H5OH, contains two independent molecules of 1,1′-[o-phenylenebis(nitrilomethylidyne)]di-2-naphthol, denoted A and B, and one ethanol solvent molecule. The hydroxy groups are involved in intramolecular O—H⋯N hydrogen bonds influencing the molecular conformations, which are slightly different in molecules A and B, where the two bicyclic systems form dihedral angles of 51.93 (9) and 58.52 (9)°, respectively. In the crystal structure, a number of short intermolecular C⋯C contacts with distances of less than 3.5 Å suggest the existence of π–π interactions, which contribute to the stability of the crystal packing.