Synthesis and Crystal Structure of 4-Arylamino-6-chloropyrido[3,2-d]pyrimidine

The title compounds 4a～c were synthesized and characterized by IR,NMR and MS.The crystal structure of C16H13ClN4O2·HBr·H2O(I),the quaternary ammonium salt of 4c,was determined by X-ray diffraction analysis.I crystallizes in triclinic,space group P1 with a = 8.3121(8),b = 9.3885(8),c = 13.2903(12),α = 106.788(2),β = 95.204(3),γ = 110.871(2)o,V = 905.81(14)3,Z = 2,C16H16BrClN4O3,Mr = 427.68,Dc = 1.568 g/cm3,F(000) = 432.00,μ = 2.446 mm-1,R = 0.0496 and wR = 0.127.X-ray analysis reveals that C(15) in the BrCH2COOH molecule binds to the N(1) of pyrimidine ring to form the quaternary ammonium salt.Two adjacent I molecules are connected by hydrogen bonds through carboxylate oxygen,water molecule and hydrobromic acid.     

Synthesis and Crystal Structure of a New Coordination Polymer: {[AgL]ClO_4}_n(L = 2,5-Bis(3-pyridinylmethylthio)-l,3,4-thiadiazole)

The title complex {[AgL]ClO4}n(L=2,5-bis(3-pyridinylmethylthio)-1,3,4-thiadiazole) was synthesized by the reaction of Ag(I) salt and a novel flexible ligand L.Its structure was determined by X-ray crystallography with the following data:monoclinic,space group P21/n,a=16.5068(13),b=7.6548(4),c=16.5521(13),β=115.119(3)o,V=1893.7(2)3,Z=4,Dc=1.893 g/cm3,μ=1.565 mm-1,F(000)=1072,C14H12AgClN4O4S3,Mr=539.78,T=293(2) K,S=1.067,the final R=0.0342 and wR=0.0870.The silver ion in the complex is in a trigonal coordin...     

Syntheses and Crystal Structures of （PySe）2 and Bi2（PySe）6（HPySe=2-Pyridineselenol N-Oxide）

The title compounds(PySe)2 1(HPySe=2-pyridineselenol N-oxide,(PySe)2= bis(2-pyridine-N-oxide) diselenide) and Bi2(PySe)6 2 were prepared by the reaction of 2-bromine-N-oxide with NaHSe and Bi(NO3)3·5H2O with HPySe,and the crystal structure of 2 was studied.Compound 2 crystallizes in the monoclinic space group P21/n with a=9.840(2),b=10.204(2),c=18.395(2),β=102.926(2)°,V=1800.0(5)3,Dc=2.2687 g/cm3,Z=2,the final R=0.0319 and wR=0.0646.The Bi atoms are coordinated by four selenium and four oxygen atoms from four PySe ligands to form a slightly distorted four-column geometry.     

Synthesis and Crystal Structure of a New Coordination Polymer：{[AgL]ClO4}n （L=2,5-Bis（3-pyridinylmethylthio）-1,3,4-thiadiazole）

The title complex {[AgL]ClO4}n(L=2,5-bis(3-pyridinylmethylthio)-1,3,4-thiadiazole) was synthesized by the reaction of Ag(I) salt and a novel flexible ligand L.Its structure was determined by X-ray crystallography with the following data:monoclinic,space group P21/n,a=16.5068(13),b=7.6548(4),c=16.5521(13),β=115.119(3)o,V=1893.7(2)3,Z=4,Dc=1.893 g/cm3,μ=1.565 mm-1,F(000)=1072,C14H12AgClN4O4S3,Mr=539.78,T=293(2) K,S=1.067,the final R=0.0342 and wR=0.0870.The silver ion in the complex is in a trigonal coordination geometry to link three different L.Meanwhile,each L connects three different silver ions by its N coordination sites to form a two-dimensional layer structure.     

A One-dimensional Coordination Polymer of Copper(Ⅱ) and Bis(4,6-dimethyl-2-pyrimidinethiolato)methane

Reaction of bis(4,6-dimethyl-2-pyrimidinethiolato)methane(bpytm) with CuCl2·4H2O in a mixed methanol/dichloromethane solution gave a one-dimensional coordina-tion polymer [CuCl2(μ-bpytm)]n which was characterized by single-crystal X-ray diffraction.It crystallizes in monoclinic,space group P21/c with a=16.9433(5),b=13.6986(4),c=7.8434(2),β=100.371(2)°,V=1790.71(9)3,Z=4,Mr=426.86,Dc=1.583 g/cm3,μ(MoKα)=1.751mm-1,F(000)=868,S=1.025,the final R=0.0399 and wR=0.0924 for 2538 observed reflections with Ⅰ2σ(Ⅰ) and 206 variables.The neutral coordination polymer is constructed by the bidentate thioether ligands to link adjacent copper atoms.Each copper atom is bridged by two adjacent nitrogen atoms of bpytm ligands and terminally bonded by two chloride atoms to form a squareplanar coordination geometry.The average Cu-N and Cu-Cl bond lengths are 2.025(2) and 2.234(1),respectively.     

Unexpected Synthesis and Crystal Structure of Macrocyclic Nickel Complex Involving Rare S-Cl Bond

A novel complex of [NiL(OOCNH2C2H3SClO3)]·H2O was obtained unexpectedly by the reaction of [Ni(rac-L)](ClO4)2 with l-cysteine (L=5,5,7,12,12,14-hexamethyl-1,4,8,11-tetra- azacyclotetradecane), and characterized by EA, IR, ESI-MS and single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group P212121 with a=9.211(12), b=14.942(19), c=19.002(2), Mr=563.80, V=2615.3(6)3 , Z=4, Dc=1.432 g/cm3 , F(000)=1204, μ=0.966 mm-1 , the final R=0.0565 and wR=0.1515. The central nickel(Ⅱ) ion displays a distorted six-coordinate octahedral coordination geometry by coordination with four nitrogen atoms of L, and one oxygen and one nitrogen atoms of l-cysteine. The sulfur atom of l-cysteine instead of oxygen atom links directly with the chlorine atom of perchlorate. The title complex is the first example of perchlorate salt involving the sulfur atom.     

Preparation,Crystal Structure,Thermal Decomposition and Explosive Properties of K2（tza）2（H2O） （tza=Tetrazole-1-acetic Acid）

A new energetic compound based on the tetrazole-1-acetic acid (tza) and potassium(I) salt, K2(tza)2(H2O), was synthesized and characterized by elemental analysis and FT-IR spectrum. Its crystal structure was determined by single-crystal X-ray diffraction analysis. The results show that the crystal belongs to the orthorhombic system, space group Pna21 with a = 1.11972(17) nm, b = 0.46647(7) nm, c = 2.5158(4) nm, V = 1.3140(3) nm3, K2C6H8N8O5, Mr = 350.40 g·mol-1, Dc = 1.771 g·cm-3, μ(MoKα) = 0.759 mm-1, F(000) = 712, Z = 4, R = 0.023 and wR = 0.0527 for 2961 observed reflections (I > 2σ(I)). The K(I) cation is six-coordinated with four O atoms from three carboxylate groups, one O atom from one H2O molecule and one N atom from tetrazolyl ring, in which each tza is coordinated in a tridentate chelating bridging coordination mode. The thermal decomposition mechanism of the title complex was studied by DSC and TG-DTG techniques. Under nitrogen atmosphere at a heating rate of 10 K·min-1, the thermal decomposition of the complex contains one main exothermic process between 191.7 and 243.8 ℃ in the DSC curve. Its combustion heat was mensurated by oxygen bomb calorimetry. The non-isothermal kinetics parameters were calculated by the Kissinger's method and Ozawa-Doyle's method, respectively. The sensitivity properties of K2(tza)2(H2O) were also determined with standard methods, which was very sensitive to flame.     

Synthesis and Crystal Structure of a New Potassium Yttrium Diphosphate Dihydrate KYP_2O_7·2H_2O

The dihydrated potassium yttrium diphosphate=KYP2O7·2H2O=has been synthe- sized for the first time. Single-crystal XRD study has allowed the determination of its structure and correct formula. It crystallizes in the monoclinic system=space group P21/c=with the cell parameters a=7.7069(3)=b=10.5801(4)=c=10.0204(5)=β=93.24(3)°=V=815.76(6)3=Z=4=Mr=337.98=F(000)=656=Dc=2.752 g/cm3 and μ=8.073 mm-1. The single-crystal structure was solved from 1856 unique reflections with the final R=0.0365 and wR=0.0772=refined with 119 parameters. The atomic arrangement of KYP2O7·2H2O is built by the P2O7 groups=the YO7 and the KO10 polyhedrons which are connected by corner and edge-sharing to form a three- dimensional framework. Water molecules are directly bonded to the Y and K atoms=and they are located in channels running along the a direction.     

A Novel Potassium Complex Based on the Taurine-salicylaldehyde Schiff Base:Synthesis, Crystal Structure and Spectroscopy

A novel two-dimensional self-assembly network formulated as [K(TSSB)]n (TSSB= taurine-salicylaldehyde Schiff base) has been synthesized via the reaction of salicylaldehyde with taurine at the presence of potassium hydroxide in water-methanol solution,and was structurally characterized by elemental analysis,IR,UV-VIS spectra and X-ray diffraction.It crystallizes in the monoclinic system,space group P21/c with a=20.245(3),b=7.2905(9),c=7.5458(10),β= 94.1920(10)o,V=1110.8(2)3,Mr=267.34,Z=4,Dc=1.599 g/cm3,μ(MoKα)=0.663 mm-1 and F(000)=552.The units of K[TSSB] are linked into a one-dimensional double chain structure via the sulfonic groups from the taurine-salicylaldelyde Schiff base,and such chains are further extended through O-K-O bond interactions resulting in a two-dimensional supramolecular architecture.In the complex,the K(I) ion displays a slightly distorted dodecahedral geometry with an eight-coordination number.     

[（n-C4H9）3SnO2C（CH2）2CO2Sn（C4H9-n）3]：A Novel Three-dimensional Framework Structure of Organotin Complex

The bis(tributyltin) ester of succinic acid was synthesized by the reaction of disodium salt of succinic acid with tributyltin chloride in a molar ratio of 1:2. The crystal structure was determined by X-ray single-crystal diffraction. It belongs to orthorhombic with space group Pccn, a = 20.949(3), b = 17.470(3), c = 20.345(3)A, V= 7446(2)A^3, Z= 8, Dc = 1.242 g/cm^3, μ=1.365 mm^-1, F(000) = 2864, R = 0.0544 and wR = 0.1417. The tin atom is of five-coordination in a trigonal bipyramidal structure by bridging two carboxylate groups in different directions and the resulting structure which contains straight twist large ring channels along the axes of a, b and c is a three-dimensional framework polymer containing two different tin atoms.     

Synthesis,Crystal Structure,and Thermal Stability of a Dibutyltin Complex {[4-Et2NC6H3（O）C=NC6H3（O）- 5-NO2]（n-Bu2Sn）}2 and Its Interaction with DNA

The Schiff base organotin(IV) complex {[4-Et2NC6H3(O)C=NC6H3(O)-5-NO2](nBu2Sn)}2 has been synthesized via the reaction between 4-(diethylamino) salicylaldehyde-2-amino-4-nitrophenol Schiff base(H2L) and dibutyltin oxide. Complex C1 has been characterized by IR, 1H NMR, 13 C NMR spectra, and elemental analysis, and its crystal structure was determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n with a = 15.6559(8), b = 9.1657(5), c = 18.8351(10) , β = 107.3440(10)°, Z = 4, V = 2579.9(2) 3, Dc = 1.442 Mg·m-3, μ(MoKα) = 1.025 mm-1, F(000) = 1152, R = 0.0250 and wR = 0.0633. The central Sn atom is coordinated in a hexadentate manner to assume a distorted octahedral configuration. Complex C1 was studied by TGA analysis in air atmosphere. The interaction between complex C1 and the herring sperm DNA was realized through the intercalation of the complex based on the studies by EB fluorescent probe.     

Synthesis and Characterization of Titanium-doped Ordered Mesoporous Alumina

Titanium-doped ordered mesoporous alumina with specific structural properties has been prepared by the evaporation induced self-assembly sol-gel method. The results show that the doped titanium helps to stabilize the ordered mesoporous alumina material without influencing the ordered mesoporosity. The textural properties of the obtained sample are related to the amount of doped titanium. When the molar ratio of aluminum to titanium(n(Al)/n(Ti)) is controlled as 10.2, the titanium-doped ordered mesoporous alumina exhibits high surface area(up to 218 m2 g-1), large pore volume(0.42 cm3 g-1) and narrow pore diameter(6.1 nm) after treating at 900 ℃, showing high thermal stability. Moreover, the obtained sample calcined at 900 ℃ still maintains ordered mesoporous structure and exhibits high thermal stability.     

Structural,Pasting, and Thermal Properties of Ultra-high Pressure-treated Lotus Seed Starch

Lotus seed starch(15%, w/w) was subjected to ultra-high pressure(UHP) at 500 MPa for 10~60 min. The effects of UHP on the structural, pasting, and thermal properties of starch were investigated using solid-state 13C CP/MAS NMR, differential scanning calorimetry(DSC), HPSEC-MALLS-RI, and a rapid visco analyzer. The 13C CP/MAS NMR results revealed a reduction in the relative crystallinity and peak intensity of the crystalline state with increasing the UHP time. The molecular weight of native starch was 1.433 × 107 Da, which was higher than that of the UHP-treated starch. Viscograms of UHP-treated starch revealed an increase in paste viscosity, peak time, and pasting temperature and a reduction in breakdown and setback viscosity compared to the native starch. Furthermore, the DSC results showed a reduction in gelatinization temperature and gelatinization enthalpy with increasing the UHP time.     

Syntheses,Crystal Structures and Thermal Properties of Two Dicadmiun（Ⅱ） Complexes CdeLeX2 （HL = N-（3-Methoxylsalicylidene）-3- dimethylaminopropylamine,X = Cl （1）, NCS （2））

Two Cd（Ⅱ） complexes, Cd2L2Cl2 （1） and Cd2L2（NCS）2 （2） （HL = N-（3-methoxylsalicylidene）-3-dimethylaminopropylamine） were synthesized and determined by EA, IR, TG and single-crystal X-ray diffraction. The crystallographic data are as follows： monoclinic, space group P21/n, a = 9.2710（9）, b = 18.0069（18）, c = 18.5562（19） A^°, β= 99.741（4）°, V = 3053.1（5）, Z = 4,μ = 1.605, F（000） = 1536, R = 0.0264 and wR = 0.0699 for 1; orthorhombic, space group Pca21, a = 16.196（3）, b = 11.506（2）, c = 36.126（7） A^°, V = 6732（2）, Z = 8,μ = 1.428, F（000） = 3264, R = 0.0376 and wR = 0.0877 for 2. There are two geometrically different octahedral Cd（Ⅱ） atoms, with N4O2 and O4Cl2 donor sets for 1 while N4O2 and N2O4 for 2. In the dinuclear Cd（Ⅱ） centers, the Cd（Ⅱ） atoms are held together by two deprotonted phenolate oxygen atoms from tetradentate L^- ligands. The thermal gravity data show two step decompositions with the residues of CdO for two complexes.     

Synthesis,Crystal Structure and Properties of a New Zn(II) Coordination Polymer Constructed from 2,3-Pyridine Dicarboxylic Acid and 1,1′-(1,4-Butanediyl)bis(imidazole)

A new coordination polymer, namely [Zn(pdc)(bbi)]n {H2 pdc = 2,3-pyridine dicar- boxylic acid, bbi = 1,1-(1,4-butanediyl)bis(imidazole)}, has been prepared under hydrothermal conditions and characterized by elemental analysis, IR, and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21 /n with a = 8.436(3), b = 16.988(5), c = 12.106(4), β = 92.204(5)°, V = 1733.6(9)3, Z = 4, C17 H17 N5 O4 Zn, Mr = 420.73, Dc = 1.612 g/cm3, F(000) = 864, μ(MoKa) = 0.452 mm-1, the R = 0.0672 and wR = 0.1645. In the mononuclear complex, each Zn(II) is five-coordinated by one carboxylate O and one pyridyl N atoms from one pdc anion, one carboxylate O atom from another pdc anion, and two N atoms from two bib ligands. The Zn(II) ions are connected by pdc ligands to form skeleton chains, and bbi ligands further link them to construct a 2D framework. The thermal and luminescence properties of the complex were also investigated.     

Crystal Structure and Thermal Stability Properties of a New 1D Chain Cu（ll） Coordination Polymer with 2,3-Pyridinedicarboxylic Acid as the Ligand

A new 1D chain copper coordination polymer [CuE（H2L）2（C10HsN2）（HEO）2]n＇3n（H20） with 2,3-pyridinedi carboxylic acid （H2L） and 2,2＇-bipyridine （2,2＇-bipy） as ligands has been synthesized in the mixed ethanol and water solvents. Crystal data for this complex are as follows： monoclinic, space group P2Jc, a = 7.7713（7）, b = 27.478（3）, c = 13.2621（13）/1,, fl = 100.6940（10）, V= 2782.8（5） A3, Dc = 1.722 g/cm3, Z = 4, p = 1.61 mm-1, F（000） = 1472, the final R = 0.0363 and wR = 0.0933. In the crystal structure, the whole molecule consists of two cooper ions, two H2L, one 2,2＂-bipy molecule and six water molecules. Each central copper ion is coordinated with three oxygen atoms from two H2L and one water molecule, two nitrogen atoms from one 2,2＇-bipy molecule and two H2L, giving a distorted tetragonal pyramidal geometry. Thermal stability properties of the complex were investigated.     

Improved Photovoltaic Performance of MEH-PPV/PCBM Solar Cells via Incorporation of Si Nanocrystals

We have studied the effect of silicon nanocrystals （SiNCs） as a third component on performance of organic bulk heterojunction solar cells composed of poly[2-methoxy,5-（2＇-ethylhexyloxy）-l,4-phenylene vinylene] （MEH- PPV）：[6,6]-phenyI-C61-butyric acid methyl ester （PCBM） blend film. By adding suitable amounts of SiNCs into MEH-PPV：PCBM blend, the device performance such as external quantum efficiency, short circuit current density （Js（）, and power conversion efficiency （PCE） improved. Incorporation of 2.5% SiNCs in the blend led to 13.6% improvement of Jsc, which in turn resulted in 18% improvement of PCE up to 2.28%. The improved performance was mainly due to the improvements both in the charge generation from the interface of MEH-PPV/SiNCs and the charge collection at the cathode.     

Investigation of the Interaction between Isoflavonoids and Bovine Serum Albumin by Fluorescence Spectroscopy

The interactions of bovine serum albumin （BSA） with three structurally related isoflavonoids, genistein, puerarin and daidzein, were studied under physiological conditions by fluorescence spectroscopic technique. The quenching mechanism of these compounds with BSA was suggested as static quenching and the binding constants were determined at different temperatures based on the fluorescence quenching results. The transfer efficiency of energy and distance between the acceptor and BSA were investigated on the basis of the mechanism of the Forster energy transference. According to the thermodynamic parameters it has been suggested that the acting force be mainly hydrophobic force. The comparison of binding potency of the three isoflavonoids to BSA showed that the substitution by 5-OH and 8-Glc could enhance the binding affinity. All these obtained in the work can make us better understand the mode of the action and pharmacological activities of the isoflavonoids.     

Synthesis and Crystal Structure of Tianagliflozin Triacetate

The title compound tianagliflozin triacetate 1 was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic system(C27H31ClO8,Mr = 518.97),space group P21 with a = 5.3913(11),b = 16.137(2),c = 15.411(3) ,β = 94.15(3)°,V = 1337.3(5) 3,Z = 2,Dc = 1.289 g/cm3,F(000) = 548,μ = 0.190 mm-1,the final R = 0.0374 and wR = 0.0809 for 3981 observed reflections(I 2σ(I)).The structure of 1,triacetate of a highly potent SGLT2 inhibitor tianagliflozin,was unambiguously determined by single-crystal X-ray diffraction,which helped to confirm the desired β configuration at the anomeric center and the position where the deoxylation occurred.The two benzene rings in the lattice are basically orthogonal to each other.There are four intermolecular hydrogen bonds in the crystal,which helps to further stabilize the crystal.     

Fe48Co52 Alloy Nanowire Arrays： Effects of Magnetic Field Annealing

The effects of magnetic field annealing on the properties of Fe48Co52 alloy nanowire arrays with various interwire distances （Di=30-60 nm） and wire diameters （Dw=22-46 nm） were investigated in detail. It was found that the array＇s best annealing temperature and crys- talline structure did not show any apparent dependence on the treatment of applying a 3 kOe magnetic field along the wire during the annealing process. For arrays with small Dw or with large Di, the treatment of magnetic field annealing also had no obvious influence on their magnetic performances. However, such a magnetic field annealing constrained the shift of the easy magnetization direction and improved the coercivity and the squareness obviously for arrays with large Dw or with small Di. The difference in the intensity of the effective anisotropic field within the arrays was believed to be responsible for this different variation of the array＇s magnetic properties after magnetic field annealing.