Ternary compounds and solid-state phase equilibria in Mg-rich side of Mg-Zn-Ca system at 300 ℃

The phase equilibria and compositions in Mg-rich side at 300 ℃ were investigated in Mg-Zn-Ca ternary system through the equilibrated alloy method by using scanning electron microscopy,electron probe microanalysis,X-ray diffraction and transmission electron microscopy.The results show that two ternary compounds T1 and T2 can be in equilibrium with the Mg-based solid solution in Mg-Zn-Ca system.T1 phase is a linear compound with the composition region（molar fraction） of 15% Ca,20.5%-48.9% Zn and balanced Mg at 300 ℃.Its hexagonal structure parameters decrease with increasing Zn content,i.e.a=0.992-0.945 nm,c=1.034-1.003 nm.T2 phase has hexagonal structure with the composition region of 26.4%-28.4% Mg,63.2%-65.5% Zn and 7.1%-8.4% Ca.At 300 ℃,the solubility of Zn in the Mg-based solid solution increases for the addition of Ca,the maximum solubility of Zn is 3.7%.Three-phase fields consisting of--Mg＋Mg2Ca＋T1,--Mg＋T1＋T2,--Mg＋T2＋MgZn and MgZn＋T2＋Mg2Zn3 exist in the Mg-Zn-Ca system at 300 ℃.

Tuning of the textural features and acidic properties of sulfated mesoporous lanthana-zirconia solid acid catalysts for alkenylation of diverse aromatics to their corresponding α-arylstyrenes

The textural features and acidic properties of sulfated mesoporous lanthana‐zirconia solid acids （SO42？/meso‐La0.1Zr0.9Oδ） were efficiently tuned by modifying the conditions used to prepare the meso‐La0.1Zr0.9Oδcomposites, such as the molar ratio of the template to La and Zr metal ions （Nt/m）, molar ratio of ammonia to La and Zr metal ions （Na/m）, hydrothermal temperature （Thydro）, and hy‐drothermal time （thydro）. The effect of the textural features and acidic properties on the catalytic performance of solid acid catalysts for alkenylation of p‐xylene with phenylacetylene was investi‐gated. Various characterization techniques such as N2 physisorption, X‐ray diffraction, NH3 temper‐ature‐programmed desorption, and thermogravimetric analysis were employed to reveal the rela‐tionship between the nature of catalyst and its catalytic performance. It was found that the catalytic performance significantly depended on the textural features and acidic properties, which were strongly affected by preparation conditions of the meso‐La0.1Zr0.9Oδcomposite. Appropriate acidic sites and high accessibility were required to obtain satisfactory catalytic reactions for this reaction. It was also found that the average crystallite size of t‐ZrO2 affected by the preparation conditions had significant influence on the ultrastrong acidic sites of the catalysts. The optimized SO42？/meso‐La0.1Zr0.9Oδcatalyst exhibited much superior catalytic activity and coke‐resistant stabil‐ity. Moreover, the developed SO42？/meso‐La0.1Zr0.9Oδcatalyst demonstrated excellent catalytic per‐formance for alkenylation of diverse aromatics with phenylacetylene to their correspondingα‐arylstyrenes. Combining the previously established complete regeneration of used catalysts by a facile calcination process with the improved catalytic properties, the developed SO42？/meso‐La0.1Zr0.9Oδ solid acid could be a potential catalyst for industrial production ofα‐arylstyrenes through clean and atom efficient solid‐acid‐mediated Friedel‐Crafts alkenylation of diverse aromatics with phenylacetylene.

Synthesis of a New Series of Chalcone Derivatives and Their Antifungal Activities

To study the antifungal effect of chalcone derivatives. Methods Sixteenchalcone derivatives were synthesized and confirmed by ~1H NMR and IR spectra, and tested forantifungal activity against four common pathogenic fungi. Their structure-activity relationship isdiscussed. Results Among 16 title compounds, there were 5 new compounds, which have not beenreported before. The preliminary antifungal test showed that all title compounds exhibitedantifungal activities to a certain extent. The activity of compound 8 against Trichophyton rubrumhad a potency equal to that of fluconazole, with a MIC of 4 μg·mL^(-1) . Conclusion Sixteenchalcones were prepared and their antifungal activities against four common pathogenic fungi invitro were examined. Some of them exhibited antifungal activities to a certain extent.

Synthesis and Crystal Structure of Methyl(7,7-Dimethyl-2-amino-4-(4-chlorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-benzo-[b]-pyran-3-yl)Carboxylate

The title compound methyl (7,7-dimemyl-2-amino-4-(4-chlorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-benzo-[b]-pyran-3-yl) carboxylate (C19H20ClNO4, Mr = 361.81) was synthesized and crystallized. The crystal belongs to triclinic, space group P 1 with a = 8.519(2), b = 10.346(2), c = 11.481(3) A, α = 108.16(1), β = 107.78(2), γ= 91.83(2)°, Z = 2, V = 906.5(3) A3, Dc = 1.326 g/cm3, μ(MoKα) = 0.234 mm-1, F(000) = 380, R = 0.0467 and wR = 0.1270 for 3142 observed reflections (I > 2σ(I)). X-ray analysis reveals that the C(7), C(8), C(9), O(1), C(10) and C(11) atoms form a six-membered ring which adopts a boat conformation. In the ring, the distances of C(8)-C(9) and C(10)-C(11) are 1.332(3) and 1.357(3) A, respectively, which indicates that they are C=C double bonds. Another six-membered ring (C(8)-C(9)-C(15)-C(14)-C(13)-C(12)) adopts the half-chair confonnation. In addition, there are intermolecular hydrogen bonds in the crystal structure.

Synthesis and Structure of Copper(Ⅱ) Complex [Cu(C_5H_5N)_2(H_2O)(C_6H_5COO)_2]

At room temperature, the reaction of dibenzoyl peroxide with metallic copper powder in the presence of pyridine affords the copper(Ⅱ) complex [Cu(C 5H 5N) 2(H 2O)\|(C 6H 5COO) 2]. Crystal is monoclinic, M r =483.002, space group Cc with parameters: a=6\^078(4), b=15.879(4), c=23.091(3), β=97.61(2)°, V=2209.1(2) 3, Z=4, D c =1\^464g/cm 3, μ =10.279 cm -1 , F(000)=996, R=0\^031, R w =0.036, 1595 reflections with I≥3σ(I ) were considered to be observed. Each copper(Ⅱ) ion is coordinated by two monodentate benzoate ligands, two pyridines and one water molecule. The complex is also characterized by its IR, XPS and thermal properties.

Synthesis and Crystal Structure of (1,3-~tBu_2C_5H_3)_2Sm( μ-Cl)_2Li(THF)_2

Anhydrous SmCl 3 reacts with two equal of Li(1,3 tBu 2C 5H 3) to give a complex (1,3 tBu 2C 5H 3) 2Sm( μ Cl) 2Li(THF) 2(C 34 H 58 Cl 2LiO 2Sm, M r =726.99), monoclinic, space group P2 1/n, a=10.615(2), b=21.037(4), c=17.166(3), β=93.60(3)°, V=3825\^7(13) 3, Z=4, D c =1.262Mg/m 3, μ =1.699mm -1 and F (000)=1508, final R= 0.0387 and wR =0.0741 for 5320 observed[ I2σ(I)] reflections. The average Sm-C distance is 2\^73. Sm-Cl1 and Sm-Cl2 distances are 2\^719(2) and 2.697(2), respectively. Two 1,3 tBu 2C 5H 3 ring centroids and two μ 2 bridging chloride atoms around Sm atom form a distorted tetrahedron.

Design and Synthesis of Novel Fluorine-containing Acrylates

A series of novel fluorine-containing acrylates 6a-6g were synthesized via the condensation of ethyl cyanoacetate and trifluoroacetic anhydride, followed by chloridization and the coupling reaction with amines. These new compounds exhibited some biological activity as preliminary bioassay indicated. A plausible reaction mechanism was outlined and discussed.

Formation kinetics and transition mechanism of CaO·SiO2 in low-calcium system during high-temperature sintering

The crystal structure,formation kinetics and micro-morphology of CaO·SiO2 during high-temperature sintering process were studied in low-calcium system by XRD,FT-IR,Raman and SEM-EDS methods.When the molar ratio of CaCO3 to SiO2 is 1.0,β-2CaO·SiO2 forms firstly during the heating process,and then CaO·SiO2 is generated by the transformation reaction of pre-formed 2CaO·SiO2 with SiO2.3CaO·SiO2 and 3CaO·2SiO2 do not form either in the heating or sintering process.Rising the sintering temperature and prolonging the holding time promote the phase transition of 2CaO·SiO2 to CaO·SiO2,resulting in the sintered products a small blue shift and broadening in Raman spectra.The content of CS can reach 97.4%when sintered at 1400℃ for 1 h.The formation kinetics of CaO·SiO2 follows the second-order chemical reaction model,and the corresponding apparent activation energy and pre-exponential factor are 505.82 kJ/mol and 2.16×10^14 s^−1 respectively.

Preparation of tricalcium silicate and investigation of hydrated cement

Tricalcium silicate cement(TSC)has been widely used in dental materials because of its self-setting behavior,good bioactivity,biocompatibility,osteoinductivity,and antibacterial effect.Tricalcium silicate(C3S)powder was prepared by Pechini technique with a calcining temperature of 1300℃ for 3 h.The influence of liquid/powder(L/P)rate on the setting time and the mechanical property of TSC was studied.Characterization methods including XRD,FTIR,SEM-EDS,TEM,and ICP-AES were utilized to study the properties of C3S powder and its hydrated cement.The bioactivity and biocompatibility of the cement were investigated by soaking test and cell culture,respectively.The results show that the L/P rate plays an important role in the setting time and the compressive strength of TSC.The surface of TSC was covered by hydroxyapatite deposition during the immersion experiment and the cells attachment on the surface of TSC was well,which indicated that TSC has good bioactivity and biocompatibility.In addition,TSC has excellent antibacterial properties against Staphylococcus aureus.In conclusion,TSC is a promising candidate for root canal filling materials.

π-π Stacking Force in the Solid Structure of Mixed-Metal Complexes: Zn(phen)_2MS_4 (M=W, Mo)

The inter-diffusion of N,N-dimethylformamide solution of Zn(phen)2Cl2 and (NH4)2MS4 (M = W, Mo) in an H-shape tube produced crystals of Zn(phen)2WS4 1 and Zn(phen)2MoS4 2 (phen = 1,10-phenanthroline). The structures of isomorphous complexes 1 and 2 have been determined by X-ray single-crystal structure analyses. Four nitrogen atoms from the phenanthroline ligands and two sulfur atoms from the MS42- anion forming a distorted octahedron coordinate each zinc atom. Through p-p interactions of adjacent aromatic rings of the phenanthroline ligands, a quasi one-dimensional zigzag-stacking column is formed in each complex. Complex 1 crystallizes in monoclinic space group C2/c, with a = 10.447(8), b = 22.016(9), c = 12.824(8) ? b = 103.56(6)? V = 2867.7(8) 3, Z = 4, C24H16N4S4WZn, Mr=737.90, Dc = 1.71 g/cm3, F(000) = 1424, m = 5.25 mm-1, the final R = 0.054 and Rw = 0.075 for 2315 observations with I > 3s (I). Complex 2 crystallizes in monoclinic space group C2/c, with a = 10.410(6), b = 22.095(7), c = 12.830(6) ? b = 103.19(8)? V = 2873.1(5) 3, Z = 4, C24H16MoN4S4Zn, Mr=649.99, Dc = 1.50 g/cm3, F(000) = 1296, m = 1.58 mm-1, the final R = 0.072 and Rw = 0.100 for 1631 observations with I > 3s(I).

Self-assembly of Polyaniline： Mechanism Study

Anisotropic polyaniline （PAni） plates decorated with self-aligned nanofiber arrays were synthesized under the hydrothermaI conditions. The formation mechanism of the self-assembled structures was investigated by studying the effect on PAni micro-structure with additive electrolyte in reaction system, and numerical simulation for dependence of systematic electrostatic energy on cross angles of self-assembled nanofiber arrays in grid textured PAni plates. It is proposed that the electrostatic interaction based on ionic doping charges plays an important role in the formation of the self-assembled PAni structures.

Synthesis,algal inhibition activities and QSAR studies of novel gramine compounds containing ester functional groups

2,5,6-Tribromo-l-methylgramine （TBG）, isolated from bryozoan Zoobotryon pellucidum was shown to be very efficient in preventing recruitment of larval settlement. In order to improve the compatibility of TBG and its analogues with other ingredients in antifouling paints, structural modification of TBG was focused mainly on halogen substitution and N-substitution. Two halogen-substitute gramines and their derivatives which contain ester functional groups at N-position of gramines were synthesized. Algal inhibition activities of the synthesized compounds against algae Nitzschia cIosterium were evaluated and the Median Effective Concentration （EC50） range was 1.06-6.74 lag ml^-1. Compounds that had a long chain ester group exhibited extremely high antifouling activity. Quantitive Structure Activity Relationship （QSAR） studies with multiple linear regression analysis were applied to fred correlation between different calculated molecular descriptors and biological activity of the synthesized compounds. The results show that the toxicity （log （I/EC50）） is correlated well with the partition coefficient log P. Thus, these products have potential function as antifouling agents.

Synthesis and Structure of a New Dinuclear Molybdenum (I) Compound with Cyclohexanthiolate Ligand, [Mo_2(SC_6H_(11))_2(CO)_8]

Molybdenum(I) -compound [Mo2(SC6H11)2(CO)8]1,crystallizes in monoclinic,space group P21/c with a=9.5863(9),b=9.4469(9),c=13.869(1)A,β=99.697(2)°,V=1238.1(2)A^3,Z=2,Dc=1.734g/cm^3 ,μ=12.23cm^-1 and F(000)=644.The final R=0.0455 and wR=0.1159 for 1590 observed reflections with I>2ó(I).1 possesses a rhombic bimetallic core MoS2Mo with the Mo-Mo bond length of 2.975(1) and Mo-S of 2.485(2)A。

Synthesis and Structure of Dimolybdenum(I) Carbonyl Compound with Thiolate and Carboxylate Mixed-tri-bridging Ligands [Bu_4N][Mo_2(CO)_6(SC_6H_4Cl-p)_2(CF_3COO)]

The crystal of the title compound with formula C36H44Cl2F3Mo2NO8S2 (Mr = 10002.62) crystallized in monoclinic, space group P21/n, with a = 9.6184(1), b = 22.3476(2), c = 20.7758(2) ?, ( = 90.172(1)(, V = 4465.70(7) ?3, Z = 4, Dc = 1.491 g/cm3, F(000) = 2032, ( = 0.833 mm－1, Final R = 0.0665 and wR = 0.1650 for 5044 reflections with I >2.0( (I). The crystal structure revealed that the Mo2S2 core is planar, and the trifluoroacetic group acts as a bidentate bridging ligand and coordinates to two Mo atoms forming a five-membered ring plane, in which the Mo-Mo bond distance is 2.9222(9) ? and the O-C-O angle is 131.8(7)

Synthesis and Crystal Structure of 2-(Diphenylphosphine oxide)-3-(diphenylphosphine oxide ethynyl) spiro [bicyclo[2.2.1]hepta-2,5-diene-7,1'-cyclopropane]

The Diels-Alder reaction of bis(diphenylphosphine oxide)butadiyne (BDPPOB) with spiro[2.4]hepta-4,6-diene affords the title compound, 2-(diphenylphosphine oxide)-3-(diphen- ylphosphine oxide ethynyl)spiro[bicyclo[2.2.1] hepta-2,5-diene-7,1-cyclopropane] (DDSHC, C35H28O2P2, Mr = 542). Its crystal structure belongs to monoclinic system, space group P21/n with a =12.708(3), b = 14.666(4), c = 15.048(4) ? = 93.903(5) ? V = 2798.1(13) ?, Z = 4, Dc = 1.288g/cm3, F(000)=1136, (MoK? = 0.187mm-1, final R = 0.0626 and wR= 0.1422 for 4685 independent reflections with I > 2(I). Structural analyses reveal that the title compound is nonplanar and the dihedral angles between two phenyl rings around each phosphorus atom are 71.7(2) and 70.7(3)? respectively.

Investigation of the Aroma Profile of Green Tea Leaves Using Organic Synthesis and Conventional Analytical Techniques

Although many aroma components have been identified in green tea leaves, the aroma compounds contributing to green tea＇s characteristic odor have not yet been reported. The authors recently reported that aroma components with a matcha-like odor are present in both green tea and black tea prepared from the Sayamakaori tea cuttivar. This matcha-like odor is similar to the odor of commercial available matcha （high-quality powdered green tea）, and is a specific odor feature of green tea leaves. At present, the green-tea odor is thought to arise from the combination of a large number of constituents. Recent reports indicate that a complex interaction between olfactory receptors and odorants is important for the evaluation of the odors. Taking into consideration these findings, the authors investigated the aroma profile of green tea, focusing on the characteristic molecular structures of the constituents that give matcha-like odor. Using a combination of organic synthesis and gas chromatography-mass spectrometry plus gas chromatography-olfactometry, the authors identified aroma components with matcha-like odors in five other tea cultivars. This investigation also revealed that several compounds with a formyl group were important constituents of the aroma of green tea leaves, although the odor of each constituent was not individually similar to the tea＇s overall aroma. The authors found for the first time a group of key components that have the matcha-like odor.

Synthesis and Single Crystal Structure of RbEr_2Cu_3Se_5

Single crystals of a new quaternary rare-earth selenide RbEr2Cu3Se5 have been isolated through the RbCl flux reaction in the RE-Cu-Se system. The title compound crystallizes in an orthorhombic system, space group Cmcm with a = 4.089(2), b = 14.498(6), c = 16.977(2) Angstrom, V = 1006.5(7) Angstrom(3), Z = 4, D-c = 6.63 g/cm(3), F(000) = 1720 and mu(MoKalpha) = 45.51 mm(-1). The final R = 0.0498 and wR = 0.0734 for 1401 observed reflections with I > 3 sigma(1). The structure of RbEr2Cu3Se5 is a three-dimensional tunnel structure composed of ErSe6 and CuSe4 polyhedra with the charge-balanced Rb+ cations stuffing into the one-dimensional channels along the a direction. In the Er2RbCu3Se5 structure, the (1)(infinity) [Er2Se(1)(4/2)SE(2)(2)Se(3)(4/2)] double-octahedral chains are linked into a (2)(infinity) [Er2Cu2Se6] layer in the a-b plane via sharing Se(1)-Se(3) edges with the (1)(infinity) [Cu(2)(2)Se(1)(2)Se(3)(4/2)] double tetrahedral chains, and (2)(infinity)[Er2CU2Se6] layers are further interconnected along the c direction by sharing Se(1)-Se(2) edges with the (1)(infinity) [Cu(1)Se(1)(2)Se(2)(2/2)] tetrahedral chains, forming a three-dimensional framework with the channels along the a axis accommodated by Rb+ ions.

Synthesis and Crystal Structure of Pd(AETYF)Cl_2CH_2Cl_2 [AETYF = 4'5'Diaza-9' (4,5-bis(ethylthio)-1,3-dithiole-2-ylidene)-fluorene]

A stable Pd(II) compound Pd(AETYF)Cl2CH2Cl2 (AETYF = 4?5?diaza-9? (4,5-bis(ethylthio)-1,3-dithiole-2-ylidene)-fluorene) has been synthesized and its crystal structure was determined by X-ray crystallography. The crystal is of monoclinic, space group P21/c with a = 15.249(6), b = 8.619(3), c = 19.078(7) ? b = 106.932(8), C19H18Cl4N2PdS4, Mr = 650.79, V = 2398.6(16) 3, Z = 4, Dc = 1.802 g/cm3, F(000) = 1296, m = 1.579 mm-1, Npar = 268, the final R = 0.0538 and wR = 0.1282 for 5068 observed reflections with I > 2s(I). The crystal structure determi- nation shows that the atoms of the molecule, except two ethyl-groups, are conjugated in a quasi- plane and these molecules are further stacked or contacted via plane to plane or edge to edge p-p interactions, forming parallel molecular chains along the b axis.

Crystal Structure of A Novel Ionic Organotin Complex:{[Ph_(2)Sn]_(2)[2,6-(O_(2)C)_(2)C_(5)H_(3)N]_(3)H_(2)O}^(2-)[HNEt_(3)]_(2)^(+)

A novel ionic organotin complex{[Ph_(2)Sn]_(2)[2,6-(O_(2)C)_(2)]C_(5)H_(3)N}_(3)H_(2)O}^(2-)[HNEt_(3)]^(2+)has been unexpectedly obtained by the reaction of Ph_(3)SnCl and 2,6-pyridine dicarboxylic acid in 1:1 molar ratio in the presence of organic base Et_(3)N.Possible dephenylation mechanism was illustrated.The X-ray diffraction study has shown that the title complex consists of cation moiety[HNEt_(3)]^(+)and anion moiety{[Ph_(2)Sn]_(2)[2,6-(O_(2)C_(2))C_(5)H_(3)N]_(3)H_(2)O}^(2-)with tin(IV)in a pengonal bipyramidal coordination geometry.