Synthesis and Crystal Structure of（E）-Ethyl 2-（5-（3-methyl-2-butenyloxy）-2-（3-（4-（3-methyl-2-butenyloxy）phenyl）acryloyl）phenoxy）acetate

The title compound,(E)-ethyl 2-(5-(3-methyl-2-butenyloxy)-2-(3-(4-(3-methyl-2-butenyloxy)phenyl) acryloyl) phenoxy)acetate(1),has been synthesized and characterized by FT-IR and 1H-NMR spectroscopy,ESI-MS,and X-ray single-crystal diffraction.FT-IR,1H-NMR and ESI-MS confirm the functional groups,particularly the ethyl groups in the ester moiety,of the compound.The single-crystal X-ray diffraction has revealed a monoclinic structure,space group P21/n with a = 14.6832(14),b = 7.7581(7),c = 23.075(2),β = 101.670(2)o,V = 2574.2(4) ?3,Z = 4,Dc = 1.235 g/cm,μ = 0.085 mm-1,and F(000) = 1024.The skeleton of chalcone in the molecular structure is coplanar.     

CRYSTAL AND MOLECULAR STRUCTURE OF {Fe_6Mo_2S_8(S-t-Bu)_6(OMe)_3}(Et_4N)_3

<正> Introduction. The title compound has been synthesized by reaction of {(SR)_2FeMoS_4}2-with {Fe_4(SR) 10}~2- (R=t-Bu) in methanol. It is interesting to note that the complex, which involves two {Fe_3MoS_4}cubane-like clusters, is generally regarded as the best model compound for molybdenum center of nitrogenase. The synthesis and property of {Fe_6Mo_2S_8(S-tBu)_6(OMe)_3}~3- have been discribed. Although it has previously been noted that the structure of this complex is similar to its tungsten analog, the detail structural report of the title compound has not yet been given.     

Synthesis and Crystal Structure of a New Mixed-ligand Nickel（Ⅱ） Coordination Polymer： [Ni（L）（cis-1,4-chdc）]n·1.25nH2O

A new one-dimensional Ni(II) coordination polymer [Ni(L)(cis-1,4- chdc)]n?1.25nH2O has been synthesized under hydrothermal conditions by using 1,4-cyclohexanedicarboxylic acid (1,4-H2chdc) and 2-(3-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline (L). Crystallographic data for the compound: triclinic, space group P with a=8.777(2), b=10.662(2), c=13.799(3), α=89.480(4), β=73.933(3), γ=81.980(4)°, V=1228.2(5)3, Z=2, C27H22.50FN4NiO5.25, Mr=568.70, Dc=1.527 g/cm3, F(000)=583, μ(MoKa)=0.846 mm-1, R=0.0634 and wR=0.1465. Neighboring Ni(II) atoms are linked by the cis-1,4-chdc ligands to generate a one-dimensional chain structure. The π-π interactions between the L ligands of neighboring chains led to the formation of a two-dimensional supramolecular layer. The elemental analysis, IR spectrum and TG of the compound have been studied.     

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Novel Mo(V) Phosphate [Zn(Mo~v_6P_4O_(31)H_(10))_2(C_4H_(14)N_3)_2]·2C_4H_(13)N_3·8H_2O

1 INTRODUCTION Hydrothermal synthesis of Mo(V) phosphates has allowed various structures, all characterized by the presence of identical clusters with the composition Mo12MP8X62 (X = O, OH) to be stabilized[1～6]. Many Mo(V) phosphates with such clusters have been iso- lated to date. The first compound was discovered by Haushalter and Lai[1] for M = Na with the formula (PPh4)2[(H3O)2NaMo6P4O24(OH)7]?5H2O. Recently, a second type of structure has been observed for M = Na (Na8(…     

Synthesis and Crystal Structure of 1-[（1＇-Phenyl-5＇-methyl-4＇-pyrazolcarbonyl）-3-methylthio-5-amino-1Hy l-1,2,4-triazole

The title compound (C14H14N6OS, Mr=314.37) has been synthesized and characterized by IR, ^1H NMR and X-ray single-crystal diffraction techniques.The crystal structure shows the presence of a dimmer with intermolecular N(4)H(4)…N(3) hydrogen bonds.     

1，4-双(1′-苯基-3′-甲基-5′-氧代吡唑-4′-基)丁二酮-(1，4)合双铜(Ⅱ)配合物的合成、表征、非等温热分解反应动力学及电化学性质

The paper reported the synthetic procedure and character of Copper(Ⅱ) binuclear coordination compound of 1,4-bis-(1′-phenyl-3′-methyl-5′-pyrazolone-4′)-1,4-butanedione. The non-isothermal kinetic of the thermal decomposition of the complex has been studied from the TG-DTG curves by means of the Achar et al and Coats-Redfern methods. The electrochemical characterization of the complex were studied by means of powder microelectrodes technique.     

Synthesis,Crystal Structure and Properties of a Novel Nickel Citrate Ni（H_2cit）（phen）（H_2O）·3H_2O（H_4cit = Citrate Acid,phen=1,10-Phenanthroline）

A new nickel citrate compound Ni(H2cit)(phen)(H2O).3H2O(H4cit = citrate acid,phen = 1,10-phenanthroline) has been synthesized and characterized by single-crystal X-ray diffraction.It crystallizes in the trigonal system,space group P31 with a = 13.8319(13),c = 10.425(2),V = 1727.3(4)3,Dc = 1.445 g/cm3,Mr = 501.09,F(000) = 780,μ = 0.901 mm-1,Z = 3,R = 0.0760 and wR = 0.1730 for 3859 observed reflections(I > 2σ(I)).In this compound,Ni2+ cation is chelated by a phen molecule,one H2cit2-anion and one H2O molecule.The citric acid coordinates to the Ni2+ center through three functional groups:α-hydroxyl,α-carboxylate and β-carboxylate while another α-carboxylate forms hydrogen bond with surrounding H2O molecule.And the citric acid is doubly protonated.The temperature-dependent magnetic susceptibility data revealed that the compound is a paramagnetic material.     

4-Amino-3-（p-chlorophenyl）-5-（p-methoxybenzyl）-4H-1,2,4-triazole：X-ray and DFT-calculated Structures

The title compound, 4-amino-3-(p-chlorophenyl)-5-(p-methoxybenzyl)-4H-1,2,4- triazole I , C16H15ClN4O), has been determined using X-ray diffraction techniques and the molecular structure has also been optimized at the B3LYP/6-31 G(d, p) level using density functional theory (DFT). The triazole ring exhibits dihedral angles of 41.61(15)o and 80.73(11)o with the phenyl rings. The molecules are linked principally by N–H…N hydrogen bonds involving the amino NH2 group and a triazole N atom, forming C(5) chains which are further linked to give a two-dimensional network of molecules. The N–H…N hydrogen bonding is supported by C–H…N hydrogen bond and C–H…π interaction. Intermolecular N–H…N and C–H…N hydrogen bonds produce R22(9), R44(10) and R44(20) rings.     

Synthesis, Crystal Structure and Biological Activities of N＇ - （ 4-Methoxybenzylidene ） -2- （ 1H-1, 2,4- triazol-1-yl） acetohydrazide

The title compound, N‘-( 4-methoxybenzylidene ) -2-( IH-1, 2,4-triazol-1-yl ) acetohydrazide, was synthesized and its structure was confirmed by means of IR, MS,^1H NMR and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test shows that the synthesized compound has a low antifungal activity.     

Synthesis and Crystal Structure of 2-Ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3（2H）-one

The crystal structure of the title compound 2-ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3(2H)-one(C15H15ClN2O4,Mr = 322.74) has been prepared and determined by single-crystal X-ray diffraction.The crystal is of orthorhombic,space group Pccn with a = 16.7246(10),b = 19.6626(12),c = 9.3013(6) ,V = 3058.7(3) 3,Z = 8,Dc = 1.402 g/cm3,μ = 0.269 mm-1,F(000) = 1344,the final R = 0.0506 and wR = 0.1464 for 2568 reflections with I 2σ(I).In addition,disordered C(14) and C(15) atoms exist in the crystal structure.     

Synthesis,Crystal Structure and Biological Activity of N-（2,6-Difluorobenzoyl）-N＇-[5-（4-trifluoromethyl-phenyl）-1,3,4-thiadiazol-2-yl]ure

The title compound N-(2,6-difluorobenzoyl)-N'-[5-(4-trifluoromethylphenyl)-1,3,4-thiadiazol-2-yl]urea(C17H9F5N4O2S,Mr = 428.34) has been synthesized by the reaction of 2-amino-5-(4-trifluoromethylphenyl)-1,3,4-thiadiazole with 2,6-difluorobenzoyl isocyanate,and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/n with a = 10.7316(13),b = 10.5617(13),c = 16.037(2) ,β = 106.408(2)°,V = 1743.6(4) 3,Z = 4,Dc = 1.632 g/cm3,μ = 0.260 mm-1,F(000) = 864,the final R = 0.0599 and wR = 0.1420 for 3467 observed reflections with I > 2σ(I).The urea group,which adopts a planar configuration mediated by the intramolecular N-H...O hydrogen bond,is nearly coplanar with the thiadiazole and 4-trifluoromethylbenzene rings.The title compound was found to exhibit good fungicidal activity against Rhizoctonia solani and Botrytis cinerea.     

Synthesis, Structure and Characterization of a New Iron Coordination Polymer： [Fe（L）（trans-l,4-chdc）]n

A novel Fe(Ⅱ) coordination polymer [Fe(L)(trans-1,4-chdc)]n has been hydrothermally synthesized by using 1,4-cyclohexanedicarboxylic acid (1,4-H 2 chdc) and 2-(2-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline (L). Crystallographic data: monoclinic, space group C2/c with a=14.571(5), b=32.389(6), c=10.948(5) , β=115.186(5)°, V=4676(3)3 , Z=8, C27H21FFeN4O4 , Mr=540.33, Dc=1.535 g/cm3 , F(000)=2224, μ(MoKa)=0.697 mm-1 , R=0.0462 and wR =0.1110. The two kinds of trans-1,4-chdc ligands link neighboring Fe(Ⅱ) atoms to yield a two-dimensional layer structure. The π-π interactions between the L ligands of neighboring layers result in a three-dimensional supramolecular architecture. The IR and UV-vis spectra of the compound have been investigated in detail.     

Synthesis,Crystal Structure and Band Structure of Tb3Co4Sn（13）

A new intermetallic compound,Tb3Co4Sn13,has been synthesized by solid-state reaction of the corresponding pure elements in a welded tantalum tube at high temperature.Its crystal structure was established by single-crystal X-ray diffraction.Tb3Co4Sn13 crystallizes in cubic,space group Pm3n(No.223) with a = 9.5072(2) ,V = 859.33(3) 3,Z = 2,Mr = 2255.45,Dc = 8.717 g/cm3,μ = 34.369 mm-1,F(000) = 1906,and the final R = 0.0140 and wR = 0.0312 for 199 observed reflections with I > 2σ(I).The structure of Tb3Co4Sn13 belongs to the Yb3Rh4Sn13 type.It is isostructural with RE3Co4Sn13(RE = La,Ce),featuring a 3D [Co4Sn12] framework based on [CoSn6] trigonal prisms.The [CoSn6] trigonal prisms are interconnected via corner-sharing and Sn-Sn bonds to form a 3D [Co4Sn12] framework.The other Sn and Tb atoms are located in the spacers of the 3D framework.Band structure calculations indicate that Tb3Co4Sn13 is metallic.     

Synthesis,Crystal Structure and Biological Activities of N-（4-Cyanopyrazole-3-yl）- α-（3,5-difluorophenyl）- O,O-diisopropyl- α-aminophosphonate

The title compound has been synthesized by the addition reaction of N-（4-cyanopyrazole-3-yl）-3,5-difluorophenyl-imine and diisopropyl phosphate. Its structure was confirmed by means of IR, ^1H NMR and elemental analysis. The single-crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in monoclinic, space group C2/c with a = 18.9959（14）, b = 9.2212（7）, c = 22.1108（16）A^°, β= 90.1540（10）°, V = 3873.0（5） A^°^3, Dc = 1.366 g/cm^3, Z = 8, μ = 0.185, F（000） = 1664, and the final R = 0.0503 and wR = 0.1539 for 2996 observed reflections （I 〉 2σ（I））. The results demonstrate that the dihedral angle between the pyrazole and benzene rings is 105.5°, and there is a full delocalized pyrazole system with sp^2 hydridization of N（3）. The crystal structure is stabilized by two intermolecular hydrogen bonds of N（1）-H（1）…O（3） and N（3）-H（3A）…N（4）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Synthesis,Crystal Structure and Antitumor Activities of Ethyl 5-methyl-4-morpholino- 2-（3-Methyl-phenylamino）-furo [2,3-d] pyrimidine-6-carboxylate

The title compound （C21H24N4O4, Mr = 396.44） has been synthesized by the func- tionalized ethyl 4-chloro-6-methyl-2-arylamino-furo[2,3-d]pyrimidine-5-carboxylates and mor- pholine. Its structure was confirmed by means of 1H NMR IR, MS and elemental analysis. The crystal structure of the title compound was determined by X-ray single-crystal diffraction. The compound crystallizes in triclinic system, space group P1, a = 7.9919（8）, b = 9.9312（1）, c = 12.9380（13） A, aα = 86.987（2）, β = 83.604（2）, γ = 89.641（2）°, V = 1019.08（18） A3, Z = 2, F（000） = 420, Dc = 1.292 g/cm3,μ = 0.091 mm-1, R = 0.0602 and wR = 0.1548 for 3943 independent （Rint = 0.0639） and 3414 observed （I 〉 2σ（I）） reflections, lntermolecular N-H…O and π-π stacking interactions contributed to the stability of the structure. The preliminary biological test indicated the title compound exhibited cytotoxicity against human lung cancer cell lines.     

Synthesis,Crystal Structure and Recognition Properties of 2-（5-（4-Chlorophenyl）-1-phenyl-4,5-dihydro-1H-pyrazol-3-yl）pyridine

The title compound 2-(5-(4-chlorophenyl)-1-phenyl-4,5-dihydro-1H-pyrazol-3-yl)- pyridine(C20H16ClN3, Mr = 333.81) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 10.9925(12), b = 11.0378(12), c = 14.2751(18) , β = 98.074(11)°, V = 1714.9(3)3, Z = 4, Dc = 1.293 g/cm3, μ(MoKα) = 0.228 mm-1, F(000) = 696, the final R = 0.0521 and wR = 0.1349 for 3495 observed reflections with I 2σ(I). Intermolecular C–H...π interactions and π-π stacking interactions stabilize the crystal structure. The binding study by fluorescence spectroscope titration showed that the title compound can selectively recognize Fe3+ in THF solution with fluorescence quenching.     

Crystal Structure and Antitumor Activity of Tri[2-[N-（4′-methyl-benzylsulfonyl）amino]ethyl]-amine

The crystal structure of the title compound (C27H38N4O7S3, Mr = 626.79) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pīwith a = 9.411(1), b = 11.645(2), c = 14.672(2) (A。), α = 91.80(1), β = 95.36(1), γ =104.56(1)o, V = 1547.0 (A。)3, Z = 2, Dc = 1.346 g/cm3, λ = 0.71073 (A。), μ(MoKα) = 0.289 mm－1 and F(000) = 664. The structure was refined to R = 0.0406 and wR = 0.1177 for 4103 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the title compound is a practically distorted tetrahedron and each molecule contains one lattice H2O by hydrogen bond. The antitumor activity of the title compound against HL-60 human leukemia cells has also been studied by MTT method.     

Synthesis and Crystal Structure of 4-[（1E）-（4-Hydroxy-3,5-dimethoxybenzylidene）-amino]-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one

The title compound (C20H21N3O4, Mr = 367.40) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 7.5143(15), b = 13.901(3), c = 18.545(4) , V = 1937.1(7) 3, Z = 4, Dc = 1.260 g/cm3, μ = 0.089 mm-1, F(000) = 776, the final R = 0.0616 and wR = 0.0912. X-ray diffraction reveals that the molecule adopts an E configuration about the central C=N double bond. The intermolecular O–H…O hydrogen bond stabilizes the crystal structure by causing the formation of a supramolecular architecture.     

Structure and Properties of a New Rare-earth Borate LiSrY_2（BO_3）_3

The structure of LiSrY2(BO3)3 has been solved by single-crystal X-ray diffraction analysis at 298 and 113 K on different diffractometers.It crystallizes in trigonal with space group P-3m1(No.164).The cell parameters at room temperature are as follows:a = 10.3345(9),c = 6.4049(11) ,V = 592.41(13) 3,Z = 3,Mr = 448.81,F(000) = 618,μ = 21.327 mm-1 and Dc = 3.774 g/cm3.The crystal structure consists of gear-like [BY6O33] groups which are linked together by corner-sharing to form a two-dimensional layer parallel to the ab plane.These layers are connected one after another by sharing oxygen atoms with B(2) atoms along the c direction to construct a three-dimensional framework.Li and Sr atoms just occupy the cavities formed by oxygen atoms.In addition,the vibrational spectroscopy of LiSrY2(BO3)3 and photoluminescence properties of the Eu3+ doped LiSrY2(BO3)3 were also studied.     

Synthesis and structures of novel octadecanuclear clusters [Cu_(12)RE_6(μ_3-OH)_(24)(pyb)_(12)(H_2O)_(18)(μ_(12)-ClO_4)]~(17+)(RE=Sm, Eu)

The novel octadecanudear Cu-RE cluster haw been isolated from the reaction system of aqueous Cu2+-RE3+-pyb (RE=Sm, Eu; pyb=pyridine betaine) and characterized by single-crystal structural analysis. The results show that the clusters comprise a [Cu12RE6(μ3-OH)24(μ12-ClO4)]17+ octahedral core, which encapsulates a ClO4- ion and has 18 water molecules and 12 bridging pyb carboxylato ligands as external ligands.