Synthesis and Crystal Structure of 3,3 ＇-（2,2 ＇-（E thane- 1,2-diylbis（oxy） ） bis（ethane- 2,1- diyl））bis（2-（4-chlorophenylamino）quinazolin-4（3H）-one）

The title compound 3,3＇-（2,2＇-（ethane-1,2-diylbis（oxy））bis（ethane-2,1-diyl））bis（2- （4-chlorophenylamino）quinazolin-4（3H）-one） 3 （C34H30CI2N604, Mr = 657.54） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in space group P1 with a = 9.9185（8）, b = 10.6124（9）, c = 15.4064（13） A, α = 92.896（2）,β = 103.813（2）, γ= 94.635（2）°, V= 1565.5（2） A3, Z = 2, Dc = 1.395 g/cm^3,μ = 0.257 mm^-1, F（000） = 684, the final R = 0.0580 and wR = 0.1284 for 3400 observed reflections （I〉 2σ（I）. It remains triclinic in the crystal. Intra- and intermolecular N（3）-H（3A）…O（2）, N（6）-H（6A）…O（3） and C（19）-H（19A）…O（4） #1 （#1： 1-x, 1-y, -z） hydrogen bonds are observed in the title compound. A two-dimensional chain network is formed from the dimmers and intermolecular π-π interactions in the crystal structure. This open network has solvent-accessible voids （10A3）.     

Synthesis and Crystal Structure of （Z）-1- （3-Fluorobenzyl）-5-（（3-fluorobenzylimino）（2-hydroxy-4-methoxyphenyl）methyl）pyridin-2（1H）-one

The title compound （Z）-1-（3-fluorobenzyl）-5-（（3-fluorobenzylimino）（2-hydroxy-4- methoxyphenyl）methyl）pyridin-2（1H）-one （C27H22F2N2O3,Mr = 460.47） was synthesized and crystallized. The crystal belongs to the triclinic system,space group P1 with a = 9.951（6）,b = 10.059（6）,c = 12.927（7）A,α = 109.828（7）,β = 102.304（7）,γ = 104.898（7）°,Z = 2,V = 1110.2（11）A^3,Dc =1.377 Mg/m^3,μ（MoKα） = 0.102 mm^-1,F（000） = 480,the final R = 0.0449 and Rw = 0.1250 for 4595 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that both m-fluorobenzyl groups are diorientationally disordered because of the rotation of C–C single bond which was represented as F（1）,F（2） and F（1＇）,F（2＇）. The diorientational disorder was refined and gave the occupancies of 0.665（4） and 0.335（4） for F（1） and F（1＇）,0.631（3） and 0.369（3） for F（2） and F（2＇）. Hydrogen bonds existing in the cell link different components to stabilize the crystal structure. The active data proved that the title compound has good anti-HBV activity.     

人工神经网络分光光度法同时测定铜（Ⅱ）、镉（Ⅱ）、镍（Ⅱ）和锌（Ⅱ）

在pH 9.80的硼砂-氢氧化钠缓冲溶液、十六烷基三甲基溴化铵（CTMAB）存在下,铜（Ⅱ）、镉（Ⅱ）、镍（Ⅱ）和锌（Ⅱ）与二甲酚橙（XO）发生灵敏的显色反应,所形成的络合物吸收光谱严重重叠,各组分间相互干扰。采用人工神经网络结合分光光度法,设计不经分离同时测定铜（Ⅱ）、镉（Ⅱ）、镍（Ⅱ）和锌（Ⅱ）含量的方法。结果表明...     

（CeO_2）_（0．7－x）（MO）_x（La_2O_3）_（0．3）（M＝

合成了（ＣｅＯ＿２）＿（０．７－ｘ）（ＭＯ）＿ｘ（Ｌａ＿２Ｏ＿３）＿（０．３）（Ｍ＝Ｍｇ、Ｃａ、Ｓｒ）固体电解质。对其晶体结构、电导率、ＸＰＳ谱、离子迁移数及制成的燃料电池的Ｖ－Ｉ曲线进行了测定。（ＣｅＯ＿２）＿（０．７）（Ｌａ＿２Ｏ＿３）＿（０．３）中掺入Ｃａ￣（２＋）、Ｍｇ￣（２＋）或Ｓｒ￣（２＋），可使电解质的氧离子导电性能改善，从而使制成的燃料电他的开路电压输出功率也得到提高。     

Syntheses and Crystal Structures of （S）-Methyl 2-（4-R-phenylsulfonamido）-3-（1H-indol-3-yl）propanoate （R = H （1） and Cl （2））

The title compounds （S）-methyl-2-（4-R-phenylsulfonamido）-3-（1H-indol-3- yl）propanoate （R = H （1）, Cl （2）） have been synthesized and their crystal structures also have been determined by X-ray single-crystal diffraction. Compound 1 （C18H18N2O4S） belongs to orthorhombic, space group P212121 with a = 9.6348（14）, b = 11.1517（17）, c = 16.412（3） A, V = 1763.4（5） A^3, Mr = 358.40, Z = 4, De = 1.350 g/cm^3,/t = 0.209 mm^-1, F（000） = 752, R = 0.0348 and wR = 0.0714. Compound 2 （CI8H17ClN2O4S） crystallizes in orthorhombic, space group P212121 with a = 9.3128（14）, b = 10.9655（16）, c = 17.783（3） A, V = 1815.9（5） A^3, Mr = 392.85, Z = 4, De = 1.437 g/cm^3, p = 0.352 mm^-1, F（000） = 816, R = 0.0389 and wR = 0.0845. The absolute structure Flack parameters X of compounds 1 and 2 are -0.03（8） and -0.06（7）, respectively. X-ray analysis reveals that the crystal structures of these two compounds both involve two intermolecular N-H…O hydrogen bond＇s.     

［Cu（C_（14）H_（11）O_3）（C_（10）H_8N_2）_2］NO_

合成了［Ｃｕ（Ｃ_（１１）Ｈ_（１１）Ｏ_３）（Ｃ（１０）Ｈ_８Ｎ_２）_２］ＮＯ_３·Ｃ_２Ｈ_５ＯＨ化合物并测定其晶体结构。晶体属Ｐ１空间群，ａ＝１．１９１１（２）ｎｍ，ｂ＝１．５３２２（２）ｎｍ，ｃ＝１．０４９２（２）ｎｍ，ａ＝１０８．９８（１）°，β＝１０７．０４（１）°，γ＝７０．２５（１）°，Ｚ＝２．在［Ｃｕ（Ｃ_（１１）Ｈ_（１１）Ｏ_３）（Ｃ_（１０）Ｈ_８Ｎ_２）_２］￣＋配合阳离子中，２个２，２’－联吡啶的４个氮原子和二苯羟乙酸的１个羧基氧原子位于铜原子周围，从而使铜原子子具有畸变的三角双锥配位构型。对红外光谱进行了归属。     

Synthesis and Crystal Structure of a Novel Hexanuclear Copper-indium Thiolate Complex [（InCl）2（OMe）（μ-OMe）2（μ3-OMe）（μ-SPrn）2（CuPPh3）]2

A novel hexanuclear copper-indium thiolate complex, [（InCl）2（OMe）（μ-OMe）2（μ- OMe）（μ-SPrn）2（CuPPh3）]2 1, was synthesized from the reaction of NaSPrn, InCl3 and [Cu（Me- CN）a][PF6] in the presence of Ph3P and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P211n with a = 11.3533（8）, b = 15.4939（11）, c = 20.5189（14） A, β = 98.577（2）°, V = 3569.0（4） A3, Z = 2, C56H82Cl4Cu2In4O8P2S4, Mr = 1801.56, Dc = 1.676 g/cm3,μ（MoKa） = 2.213 mm^-1, F（000） = 1796, S = 0.985, the final R = 0.0559 and wR = 0.1099 for 8878 observed reflections with I 〉 2σ（I） and 367 variables. Complex 1 consists of two CuPPh3 fragments which symmetrically side-attach to the tetranuclear core of [InaCl4（OMe）2（μ-OMe）a（μ- OMe）2（μ-SPrn）4] by coordinating with sulfur atoms of propane-thio moieties. The average In-Ot （terminal）, In-μ-O and In-μ3-O bond distances are 2.305（4）, 2.144（4） and 2.294（4） A, respectively.     

（Pb_（0．88）Nd（0．10））（Ti_（0．92）In_（0．06）Mn_（0．2））O_3超细陶瓷粉末的制备与研究

（Ｐｂ_（０．８８）Ｎｄ（０．１０））（Ｔｉ_（０．９２）Ｉｎ_（０．０６）Ｍｎ_（０．２））Ｏ_３超细陶瓷粉末的制备与研究杨昆山，陈种菊，陈坚业，张惊涛（四川联合大学化学系，成都，６１００６４）关键词超细粉，共沉淀，制备掺Ｉｎ２Ｏ３、Ｎｄ２Ｏ３和ＭｎＯ?..     

Rapid Thermolysis Studies of [Pb2（TNR）2（CHZ）2（H2O）2]·4H2O and Cd（CHZ）2（TNR）（H2O）

T-jump/FT-IR spectroscopy was used to study the rapid thermal decomposition activity of [Pb2（TNR）2（CHZ）2（H2O）2]·4H2O and Cd（CHZ）2（TNR）（H2O） under 0.1 MPa Ar atmosphere. The results show that the main gaseous products of [Pb2（TNR）2（CHZ）2（H2O）2]·4H2O are NH3, H2O and HONO, while CO and NO are the major gaseous products of flash pyrolysis of Cd（CHZ）2（TNR）（H2O）. Thus Cd（CHZ）2（TNR）（H2O） is not an eco-friendly and chemically compatible primary explosive. Both compounds liberate volatile metal carbonate, oxide and isocyanate compounds. The combustion temperature and products of the two compounds were calculated by Real code. The results of theoretical calculation show that the combustion temperature of [Pb2（TNR）2（CHZ）2（H2O）2].4H2O is higher than that of Cd（CHZ）2（TNR）（H2O）, there is no HNCO in the combus- tion products and the amount of NO is less than the experiment result from T-jump/FTIR.     

Ni（bpy）（H2O）（V2O6）和[Ni（bpy）2]2（V6O17）的水热合成与晶体结构

用NiCl2·6H2O,2,2＇-联吡啶（bpy）,NH4VO3,WO3在443K下通过水热反应法得到了两种多钒酸镍配合物Ni（bpy）（H2O）（V2O6）（1）和[Ni（bpy）2]2（V6O17）（2）．单晶X射线衍射结果表明化合物（1）属于正交晶系,空间群为Pcα2（1）,晶胞参数为0=0．91704（18）nm,b=1．0519（2）nm,c=1．4336（3）nm,V=1．3830（5）nm^3,Z=4;化合物（2）属于单斜晶系,空间群为P2（1）／c,晶胞参数为α=1．5467（3）nm,b=1．4740（3）nm,c=1．0457（2）nm,β=91．99（3）°,V=2．3826（8）nm^3,Z=4．化合物（1）由2,2’-联吡啶修饰的二维[Ni（V2O6）（H2O）]∞电中性层构成,而化合物（2）则由2,2＇-联吡啶修饰的、呈正弦波浪状的[Ni：（V6O17）]∞二维电中性层构成．     

A New Chain-like Copper（Ⅱ） Polymer： [Cu（MOPIP）（BDC）]n·0.5n（H2O）

A metal-organic coordination compound formulated as [Cu（MOPIP）（BDC）]n·0.5n（H2O） 1 （MOPIP - 2-（4-methoxyphenyl）-1H-imidazo[4,5-f][1,10] phenanthroline, BDC = 1,4-benze Nedicarboxylate） has been hydrothermally synthesized and structurally characterized by elemental analysis, thermogravimetric analysis, IR spectrum, and single-crystal X-ray diffraction. The title compound crystallizes in the triclinic system, space group P1^-, with a = 8.872（5）, b = 11.163（6）, c = 12.589（6）A, α = 94.687（7）, β = 99.930（6）, γ = 103.074（7）°, V = 1186.7（12）A^3, C28H19CuN4O5.5, Mr= 563.01, Dc = 1.576 g/cm^3,μ（MoKa） = 0.973 mm^-1, F（000） = 576, Z = 2, the final R = 0.0607 and wR = 0.1618 for 3419 observed reflections （I 〉 2σ（I））.     

A Facile Approach to Synthesis of the Di-O-methyl Ethers of （-）-Agatharesinol, （-）-Sugiresinol, （＋）-Nyasol and （＋）-Tetrahydronyasol

The facile enantioselective synthesis of the di-O-methyl ethers of （-）-agatharesinol （1b）, （-）-sugiresionl （2b）, （＋）-nyasol （3b） and （＋）-tetrahydronyasol （4） were achieved in high yield. The absolute configuration of （＋）-3a was confirmed via first total synthesis of （＋）-3b and （＋）-4.     

Synthesis,Structure and Photoluminescence of a Tetranuclear Zinc（II） Complex： [Zn4（SO4）2（DPPZ）4（HSal）2（OH）2]

A new tetranuclear zinc（II） complex [Zn4（SO4）2（DPPZ）4（HSal）2（OH）2] 1 （DPPZ = dipyrido[3,2-a：2＇,3＇-c]phenazine, H2Sal = salicylic acid） was prepared by using hydrothermal synthesis and characterized by elemental analysis, IR spectrum, thermal gravimetry （TG）, fluorescent emission and single-crystal X-ray diffraction. Its crystal structure is of monoclinic, space group P2 1/c with a = 9.8897（8）, b = 14.2506（12）, c = 26.384（2） ,A, β = 94.8940（10）°, V = 3704.8（5） A3 Z = 2, C86H52N16O16S2Zn4, Mr = 1891.04, Dc = 1.695 g/cm^3, μ= 1.423 mm^-1, F（000） = 1920, GOOF = 1.039, the final R = 0.0358 and wR = 0.0872 for 6038 observed reflections with I 〉 2σ（I）. In 1, ＂cage-like＂ tetranuclear clusters of [Zn4（SO4）2（DPPZ）4（HSal）2（OH）2] are further stacked through π-π interactions to generate a 3D supramolecular network.     

用聚乙二醇—硫酸铵—铝试剂体系萃取分离铁（Ⅲ）铝（Ⅲ）,铜（Ⅱ）钴（Ⅱ）…

研究了在聚乙二醇－硫酸铵－铝试剂体系中Ｆｅ（Ⅲ），Ａｌ（Ⅲ）、Ｃｕ（Ⅱ）、ＣｏⅡ）Ｃｄ（Ⅱ）Ｍｎ（Ⅱ）、Ｎｉ（Ⅱ）的萃取分离行为。结果表明，在ＰＨ５．０－６．５ＨＡｃ－ＮａＡｃ缓冲溶液中，Ｆｅ（Ⅲ）、Ａｌ（Ⅲ）可被ＰＥＧ相几乎完全萃取，而Ｃｕ（Ⅱ）、Ｃｏ（Ⅱ）Ｃｄ（Ⅱ）Ｍｎ（Ⅱ）基本上不被萃取，从而实现了Ｆｅ（Ⅱ）与Ｃｕ（Ⅱ）Ｃｏ（Ⅱ）Ｃｄ（Ⅱ）Ｍｎ（Ⅱ)及Ａｌ（Ⅲ）与Ｆｅ（Ⅲ）Ｃｏ（Ⅱ）、Ｃｕ（     

双膦配合物Ru（OAc）2（Ph3P）（dppe）和Ru（OAc）2（dppe）2的设计合成,表…

Ｒｕ（ＯＡｃ）２（Ｐｈ３Ｐ）２和１或２摩尔的双－（二苯基膦）乙烷（ｄｐｐｅ）在回流的甲苯中反应，分别生成双膦配位的Ｒｕ（ＯＡｃ）２（Ｐｈ３Ｐ）（ｄｐｐｅ）和Ｒｕ（ＯＡｃ）２（ｄｐｐｅ）２。并进行了元素分析、ＩＲ、ＮＭＲ等谱学表征。在温度－５０至４０℃的范围内，测定了Ｒｕ（ＯＡｃ）２（Ｐｈ３Ｐ）（ｄｐｐｅ）的＾３１Ｐ｛＾１Ｈ｝ＮＭＲ谱，讨论了配合物中膦配体的配位状态。在反应温度３０至９０℃、氢压１．     

Synthesis and Crystal Structure of （Z）-5-fluoro-3- （phenyl（（5-（pyridin-3-ylmethyl）thiophen-2- yl）amino）methylene） Indolin-2-one

The crystal structure of the title compound （Z）-5-fluoro-3-（phenyl（（5-（pyridin-3- ylmethyl）thiophen-2-yl）amino）methylene） indolin-2-one （C25H18FN3OS, Mr = 427.50） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 5.931（1）, b = 12.413（1）, c = 28.102（2） A, V= 2090.4（3） A3, Z = 4, Dc = 1.358 g/cm3, F（000） = 888, μ= 0.186 mm-1, MoKa radiation （2 = 0.71073）, R = 0.041 and wR = 0.105 for 4567 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the indole and thiophene rings are not coplanar with a dihedral angle of 46.26（5）°. Intramolecular and intermolecular N-H＇..O hydrogen bonds together with C-H...π interations can be observed in the lattice.     

Crystal Structure and Molecular Absolute Configuration of （＋）－Isocedranol （C_（15）H_（26）O）

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅａｎｄＭｏｌｅｃｕｌａｒＡｂｓｏｌｕｔｅＣｏｎｆｉｇｕｒａｔｉｏｎｏｆ（＋）－Ｉｓｏｃｅｄｒａｎｏｌ（Ｃ_（１５）Ｈ_（２６）Ｏ）￥ＬｉｕＪｉｅ；ＣｈｅｎＭｉｎ－Ｑｉｎ（ＣｅｎｔｅｒｏｆＡｎａｌｙｓｉｓ＆Ｍｅａｓｕｒｅｍ...     

Co3（CO）7（μ3—S）[μ,η^2—SCNC（O）C（R1）（R2）N（COR3）]的…

Ｃｏ２（ＣＯ８）分别与４种硫代乙内酰脲Ｓ＝ＣＮＨＣ（Ｏ）Ｃ（Ｒ１）（Ｒ２）Ｎ（ＣＯＲ３）反就，得到４个新的含硫代乙内酰脲桥基双齿配位的三核钴羰基硫族合物。用元素分析、ＩＲ、＾１Ｈ ＮＭＲ和ＭＳ等手段表征了它们的结构，用Ｘ射线衍射测定了其中一个族合物Ｃｏ３（ＣＯ７）７（μ３－Ｓ）［μ，η＾２－ＳＣＮＣ（Ｏ）Ｃ（ＣＨ３）（ＣＨ３）Ｎ（ＣＯＣＨ３）］（Ⅳ）的晶体结构，晶体属三斜晶系，Ｐ１↑－空间群，晶胞     

Synthesis and Characterization of a Reduced Molybdenum（V） Phosphate,（H3dien）2（H2dien）2[NaMo12O24（OH）6-（H2PO4）（HPO4）5（PO4）2]·nH2O （n = 10.92）

A new reduced molybdenum（V） phosphate （H3dien）2（H2dien）2[NaMo12O24 （OH）6 （HEPO4）（HPO4）5（PO4）2]·nH2O （n= 10.92, dien = diethylenetriamine） has been synthesized under hydrothermal conditions and characterized by elemental analyses, IR and X-ray diffraction. C16H96.84MO12N12NaO72.92P8 （Mr = 3046.73） crystallizes in the monoclinic system, space group P21/c with a = 13.3575（18）, b = 21.907（3）, c = 15.654（2）A, β= 110.22（2）°, V= 4298.4（10） A^3 Dc = 2.354 g/cm^3, Z = 2,μ（MoKcr） = 1.966 mm^-1, F（000） = 2990.4, the final R = 0.0357 and wR = 0.1086 for 8739 observed reflections with I 〉 2σ（I）. It consists of sandwich-shaped cluster anions [Na{Mo6P4}2]^10- held together into a three-dimensional supramolecular framework through intermolecular hydrogen-bonding contacts. A probe reaction of the oxidation of acetaldehyde with H2O2 showed that this compound has high catalytic activity in the reaction.