An Efficient Palladium-catalyzed Coupling Reaction for the Preparation of Biaryls and Polyaryls

In the case of Pd(Ph3)4 as catalyst and toluene as reaction solvent,the desired biaryls and polyaryls were synthesized in excellent yield and on a large scate.     

Cu（OAc）2/Pyrimidines-Catalyzed Cross-coupling Reactions of Aryl Iodides and Activated Aryl Bromides with Alkynes under Aerobic, Solvent-free and Palladium-free Conditions

Excellent results have been achieved in the Cu（OAc）2-catalyzed Sonogashira cross-couplings of aryl iodides and activated aryl bromides utilizing TBAF （tetrabutylammonium fluoride） as the base and 4,6-dimethoxypyrimidin-2-amine as the ligand. It is noteworthy that the reaction is conducted under aerobic, solvent-free and palladium-free conditions.     

Synthesis and Single Crystal X-ray Studies of 3-（3,5-Bis（trifluoromethyl）phenyl） Quinoline and 3-（4-Fluoro-3-methyiphenyl） Quinoline

The title compounds 3-（3,5-bis（trifluoromethyl）phenyl）quinoline （1） and 3-（4- fluoro-3-methylphenyl）quinoline （2） were synthesized through Suzuki-Miyaura Cross coupling reaction of 3-bromoquinoloine with aryl boronic acids. The title compounds were characterized by single-crystal X-ray diffraction, 1H NMR, 13C NMR, El-MS, elemental analysis and IR. The crystals of 3-（3,5-bis（trifluoromethyl）phenyl）quinoline （C17H9F6N, Mr = 341.25） belongs to the monoclinic system, space group P21n, a = 12.3072（13）, b = 4.9378（6）, c = 24.493（2） A, V= 1473.1（3） A3, Z = 4, Dc = 1.539 Mg m-3, 2 - 0.71073A, μ = 0.144 mm^-1, F（000） = 688, the final R = 0.0715 and wR = 0.1873 for 1875 obserwed reflections with I 〉 2σ（I） and the crystal of 3-（4-fluoro-3- methylphenyl）quinoline （C16H12FN, Mr= 237.27） belongs to the orthorhombic system, space group Pca21, a = 23.794（2）, b = 3.9094（3）, c = 25.669（2） A, V = 2387.7（4） A3, Z = 8, D, = 1.320 Mg m-3, 2 = 0.71073 A, μ = 0.088 mm-1, F（000） = 992, the final R = 0.0534 and wR = 0.1188 for 2270 observed reflections with I 〉 2σ（I）.     

Synthesis and self-assembly of phthalocyanines bearing sulfur-containing substituents简

Asymmetrically substituted phthalocyanines with sulfur-containing substituents for fabrication of selfassembled monolayers were synthesized. Phthalocyanine 7, bearing a disulfide group, was synthesized from phthalocyanine with a hydroxyl group, which was prepared via mixed condensation of the corresponding substituted phthalonitriles. Phthalocyanine 10, bearing an acetyl protected thiol group, was synthesized through the Pd-catalyzed coupling reaction of an iodophthalocyanine. Their selfassembling behavior on gold substrates was further studied by UV–vis spectroscopy.     

Synthesis, Structure and Physical Properties of a Barium（II） Complex with 5-Sulfoisophthalic Acid Sodium

An alkaline earth metal-organic framework [Ba(Hsip)(H2O)4]n (1, NaH2sip = 5-sulfoisophthalic acid sodium) has been constructed, and characterized by single-crystal X-ray diffraction. In complex 1, each Ba(II) atom coordinates to one ligand Hsip3- and four water molecules with a distorted nine-coordinated monocapped tetragonal antiprism geometry. Each Hsip2- anion acts as a μ3-bridging ligand, in which two carboxylate groups adopt the same bidentate chelating coordinating model and the sulfonate group takes a monodentate coordinating model, resulting in a wave-like two-dimensional network with a (6, 3) topological structure. The two-dimensional networks are further linked by O-H···O to form a three-dimensional structure. Luminescent property and thermal stability of complex 1 are investigated. 1 belongs to the orthorhombic system, space group Pna21 with a = 7.3333(2), b = 16.7044(3), c = 10.4817(2), Z = 4, V = 1283.99(5)3, Mr = 453.58, Dc = 2.346 g/cm3, F(000) = 880, μ = 3.314 mm-1, the final R = 0.0261 and wR = 0.0592 for 2425 observed reflections with I > 2σ(I).     

A Novel Complex of Na（I）-Nitronyl Nitroxide [Na（NIT- 1＇-MeBzIm）3]ClO4： Synthesis and Crystal Structure

A novel complex [Na（NIT-1＇-MeBzIm）3]ClO4 （NIT-1＇-MeBzIm = 2-{2＇-[（1＇- methyl）benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide） has been prepared and structurally characterized by elemental analysis, IR spectra and X-ray diffraction methods. The title complex crystallizes in trigonal, space group P3 and Z = 2. Crystal data： C45H57ClN12NaO10, Mr = 984.47, a = 13.9411（8）, b = 13.9411（8）, c = 14.8622（16） A, γ= 120°, V= 2501.5（3） A^3, Dc = 1.307 g/cm^3, μ（MoKα） = 0.152 mm^-1, F（000） = 1038, R = 0.0637 and wR = 0.1813 for 1957 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the Na（I） ion is six-coordinated with three NIT-1＇-MeBzlm radicals. As we know, three radicals coordinating to the Na（I） ion in the main group by a chelate way is the first example. The Na（I） ion resides in a distorted octahedron with a facial configuration. Meanwhile, the intermolecular weak interactions result in a 2-D double layer conformation where the uncoordinated perchlorate anions are inserted in the packing space and take part in the H-bond interactions, and each complex is connected with six neighboring complexes and three perchlorate anions.     

Zinc Complexes Supported by N,N-Dimethylaniline-arylamido Ligands： Synthesis,Characterization and Catalytic Properties for Ring-opening Polymerization of L-Lactide

The reaction of bidentate N,N-dimethylaniline-arylamido ligands,o-C6H4NMe2（CH2NHAr）（Ar =Ph,1a;2,6-Me2C6H3,1b; 2,6-Et2C6H3,1c; 2,6-ipr2C6H3,1d） with ZnEt2 yields the complexes o-C6H4（NMe2）（CH2NAr）ZnEt （2a-2d）,respectively.All the complexes were characterized by 1H and 13C NMR spectroscopy and elemental analyses.It was found that all the zinc complexes were efficient catalysts for the ring-opening polymerization of L-lactide in the presence of benzyl alcohol with good molecular weight control and narrow polydispersity.     

Sodium Holmium Polyphosphate NaHo（PO3）4 with [P4O12]4- Spiral Chains： Synthesis,Crystal Structure,and Luminescent Properties

Sodium holmium polyphosphate crystal, NaHo（PO3）4, has been synthesized by the high temperature solution reaction and characterized by X-ray diffraction analysis, EDX, IR, UV-vis-NIR, and PL spectra. The structure belongs to the monoclinic system, space group P21/n with Z = 4, α = 7.181（3）, b = 13.059（5） and c = 9.730 （4） ？. It is described as a three-dimensional （3D） architecture made up of [P4O12]4- anionic spiral chains and HoO8 polyhedra by corner-sharing. The 8-coordinated sodium atoms are located in infinite tunnels. The results of EDX and IR spectrum are in good agreement with the crystallographic analysis. In addition, NaHo（PO3）4 exhibits visible light emission in the solid state at room temperature.     

An Environmentally Benign System for Synthesis of β-Hydroxylketones： L-Histidine Asymmetrically Catalyzed Direct Aldol Reactions in Aqueous Micelle and Water-like Media

The first histidine catalyzed direct aldol reactions of ketones with nitrobenzaldehydes in water and in poly（ethylene glycol） （PEG） were reported. It reveals that histidine is a good aldol catalyst for synthesis of β-hydroxylketones in water and in PEG, giving good to excellent yields of the respective products. Better enantioand regioselectivity were achieved using low molecular weight PEG as the media. The results show that histidine and PEG-200 or -300 may constitute a promising environmentally benign system for asymmetric synthesis of β-hydroxylketones.     

Hydrothermal Synthesis and Crystal Structure of a Manganese（Ⅱ） Coordination Polymer with 1,1＇-Biphenyl-2,2＇,6,6＇-tetracarboxyl Acid and 2,2＇：6,2＇-Terpyridine Ligands

The title compound {[Mn（H2BPTC）（tpy）（H2O）]·（H2O）3}, （1, H4BPTC = 1,1＇- biphenyl-2,2＇,6,6＇-tetracarboxylic acid, tby = 2,2＇：6,2＇-terpyridine） has been synthesized by the hydrothermal reaction, and its s...     

A New Method of Synthesis of Azo Schiff Base Ligands with Azo and Azomethine Donors： Synthesis of N-4-Methoxybenzylidene-2-（3-hydroxyphenylazo）-5-hydroxyaniline and Its Nickel（Ⅱ） Complex

A new method for the synthesis of azo Schiff an base ligand in which the azo and azomethine groups are coordination sites was developed through a Schiff base precursor. The precursor, N-4-methoxybenzylidene-3-hydroxyphenylamine （SB） derived from 3-aminophenol was regioselectively coupled with a diazonium ion para to the hydroxyl group of the amine component of the Schiff base. The para selectivity was controlled by the directing effect of the hydroxyl group. The ligand and its nickel（Ⅱ） complex were characterized by elemental analyses, IR and UV-Vis spectroscopy. The analytical and spectral data supported the mononuclear formulation of the complex with metal to ligand ratio （M ： L = 1 ： 2） and suggested a square planar geometry for the complex.     

Hydrothermal Synthesis and Crystal Structure of a Novel Selenite-chloride：[Cd4（SeO3）2Cl4（H2O）]n with a Three-dimensional Framework

A novel three-dimensional(3-D) compound [Cd4(SeO3)2Cl4(H2O)]n(1) was prepared from a hydrothermal reaction and structurally characterized.Compound 1 crystallizes in the space group Fmmm of the orthorhombic system with eight formula units in a cell:a = 15.5165(4),b = 17.5090(9),c = 7.3318(5) ,V = 1991.9(2) 3,Cd4Cl4H2O7Se2,Mr = 863.38,Dc = 5.758 g/cm3,S = 1.075,μ(MoKα) = 16.820 mm-1,F(000) = 3088,R = 0.0427 and wR = 0.1220.Compound 1 features a 3-D structure with the cadmium atoms having two different coordination environments,i.e.,six-and eight-coordination geometries.Two different chain-like structures of cadmium-oxo polyhedra are interconnect to each other to give a 2-D layer of [Cd4(SeO3)2(H2O)]n4n+.Between the [Cd4(SeO3)2(H2O)]n4n+ layers is a novel chloride layer.A 3-D framework is constructed from these [Cd4(SeO3)2(H2O)]n4n+ layers linked by the chloride layers.     

Hydrothermal Synthesis and Crystal Structure of a Nickel（Ⅱ） Polymer with a One-dimensional Chain Structure：[Ni（cbba）_2（bipy）（H_2O）_2]_n

A metal-organic coordination polymer formulated as [Ni(cbba) 2 (bipy)(H 2 O) 2 ] n 1 (H 2 cbba=2-(4-chlorine-benzoyl)benzoic acid,bipy=4,4-bipyridine) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum,TG and single-crystal X-ray diffraction.The title compound crystallizes in the triclinic system,space group P1 with a=5.4550(4),b=11.4099(8),c=15.3135(11),α=68.7680(10),β=81.3470(10),γ=79.3450(10)o,V=869.48(11) 3,C 38 H 28 Cl 2 N 2 NiO 8,M r=770.23,D c=1.471 g/cm 3,μ(MoKα)=0.768 mm 1,F(000)=396,Z=1,the final R=0.0456 and wR=0.1171 for 2477 observed reflections (I > 2σ(Ⅰ)).It exhibits a one-dimensional chain-like structure.