[（C5H4CH3）2HoN4cpH]2.[（C5H4CH3）（C5H5）HoN4CPh]2的合成和晶体结构2

（Ｃ５Ｈ４ＣＨ３）３Ｈｏ和（Ｃ５Ｈ４ＣＨ３）２Ｈｏ（Ｃ５Ｈ５）与５－本基四唑在ＴＨＦ中反应，得到了复合产物「（Ｃ５Ｈ４ＣＨ３）２ＨｏＮ４ＣＰｈ」２．「（Ｃ５Ｈ４ＣＨ３）（Ｃ５Ｈ５）ＨｏＮ４ＣＰｈ」２，该晶体属三斜晶系，Ｐ１空间群，晶胞参数为ａ＝９．３８６（３），ｂ＝１３．０７１（３），ｃ＝１６．５７１（２）Ａ，α＝８６．９０（１），β＝７４．６１（２），γ＝７７．３０（２）°，Ｖ＝１９１２．８（８     

In Situ Hydrothermal Synthesis of a Mononuclear Copper（Ⅱ） Complex： Cu（H2SIP-O）（bpy）（H2O） （H4SIP-O = 4-Hydroxyl-5-sulfoisophthalic Acid）

The mononuclear complex, Cu（H2SIP-O）（bpy）（H2O） （H4SIP-O = 4-hydroxyl- 5-sulfoisophthalic acid and bpy = 2,2＇-dipyridyl）, has been synthesized by the hydrothermal reaction of Cu（OH）2 with NaH2SIP and bpy at 160 ℃, and characterized by single-crystal X-ray diffraction, elemental analysis and IR spectrum. The new ligand 4-hydroxyl-5-sulfoisophthalic acid derived from 5-sulfoisophthalic acid ligand under an in situ hydrothermal condition. The crystal of the complex crystallizes in a triclinic system, space group P1, with a = 7.757（4）, b = 10.663（6）, c = 11.727（7）A, α = 94.272（4）, β = 104.067（7）, γ = 97.400（7）°, V= 927.4（9）A^3, Z = 2, C18H14N2O9SCu, Mr= 497.93, Dc= 1.783 g/cm^3,μ = 1.350 mm^-1, F（000） = 506, the final R = 0.0518 and wR = 0.1513 for 4180 observed reflections with I 〉 2σ（I）. The central Cu（II） ion is five-coordinated by two oxygen atoms from the H2SIP-O^2- ligand and two nitrogen atoms of bpy ligand in a distorted square-planar geometry as well as a water oxygen atom in the apical position to complete a distorted square-pyramidal coordination geometry. The mononuclear copper molecules are linked by hydrogen bonds between coordinated water molecules and sulfonate groups to form a one-dimensional double-chain structure. The chains are further held together through extensive π-π stacking interactions between the aromatic rings to form a three- dimensional supramolecular structure.     

SYNTHESIS AND CRYSTAL STRUCTURE OF （C5H5）2Ti（o—NHPhC6H4CO2）2

<正> Cp2Ti(o-NHPhC6H4CO2)2, Mr = 602. 54, space group C2/c, a = 33. 77(2), b = 12. 611(6), c=14. 486(9) A ,β=103. 28(4)°,V = 6004(5) (?)3,Z = 8, Dc= 1. 33gcm-1, MoKa(λ=0. 71069(?)) radiation, μ = 3. 21cm-1, F(000) = 2512e, R = 0. 066, Rw= 0. 085 for 2511 radiations. The Ti atom in the molecule is coordinated by two C5H5 groups and two monodentate carboxyl ligands in a distorted tetrahedral geometry with the bonds in the range of Ti-C = 2. 334 - 2. 41(?) ; Ti-O = 1. 914(5) and 1. 919(5)(?);and the bond angles O-Ti-O = 91. 7(2)°; (cent-C5H5)-Ti-(cent-C5H5) = 135. 9(6)°.     

STRUCTURE OF（C6H5COCHCOC6H5）SmI2（THF）3

<正> (C6H5COCHCOC6H5)SmI2(THF)3,Mr= 843. 75,triclinic space group P1,a=13. 274(3),b=9. 886(3),c= 12. 526(4)A,a= 110. 89(3),B=93. 98(2),y=85. 16(2) ,V=1528. 9(8)A3,Z=2,Dc=1. 83g/cm3, (MoKa) = 0. 71069A,u= 40. 3cm-1,F(000) - 810. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R value of 0.082(Rw= 0. 083). The central Sm(III) ion is coordinated by two iodine ions, two oxygen atoms from C6H5COCHCOC6H5 and three oxygen atoms from three THF molecules to form a distorted pentagonal bipyramid. The Sm-I distances are 3. 103 and 3. 092 A ,The Sm-O (O atom from C6H5COCHCOC6H5) distances are 2. 273 and 2. 307 A and the average Sm -O(THF) distance is 2. 500A.     

[（C6n5NO2）Pr（H2O）4]（CrMo6O24H6）·（C6H5NO2）·2．5H2O的合成与晶体结构

用常规合成方法制备了基于Anderson结构阴离子的二维层状化合物[（C6n5NO2）Pr（H2O）4]（CrMo6O24H6）·（C6H5NO2）·2．5H2O,通过红外光谱和X射线单晶衍射对其进行了表征．结果表明,该化合物属于单斜晶系,C2/c空间群．a=2．3442（9）nm,b=1．3291（5）nm,c=2．458（1）nm,β=103．08（1）°,V=7．460（5）nm^3,R1=0．0727,wR2=0．1903．结构分析表明,[CrMo6O24H6]^3-阴离子通过端氧担载一个配位的Pr^3＋离子形成中性的（C6H5NO2）Pr（H2O）4（CrMo6O24H6）基团,相邻的中性基团在O1-Pr-O1桥联下形成一维链,链与链又通过异烟酸的桥联形成二维层状结构．     

Synthesis and Structure of [Cu（OH）2（H2O）2（4—C5H4N—COOH）2]

1 INTRODUCTION Supramolecular chemistry and crystal engineering of coordination compounds have attracted considerable interests nowadays owing to the fascinating structural diversity and potential applications as functional materials[1,2]. Generally, architectures of supramolecules are formed through hydrogen bonds, ?- ?stacking interaction or other weak interactions between the molecules. Recently, many supramolecular compounds containing silver(I) and copper(II) species have been re-…     

Synthesis,Crystal Structure and Anticancer Property of （Z）-N-（4-Bromo-5-ethoxy-3,5-dimethyl-furan-2（5H）-ylidene）-4-methylbenzenesulfonamide

The novel title compound(Z)-N-(4-bromo-5-ethoxy-3,5-dimethylfuran-2(5H)-yli-dene)-4-methylbenzenesulfonamide 1(C15H18BrNO4S) has been unexpectedly synthesized by the aminohalogenation reaction of ethyl 2-methylpenta-2,3-dienoate with TsNBr2,and characterized by mp,IR,1H NMR,EIMS,ESIHRMS and single-crystal X-ray diffraction.It crystallizes in mono-clinic,space group P21/c with a = 11.714(5),b = 14.106(5),c = 10.402(4) ,β = 97.298(8)°,V = 1704.9(12) 3,Mr = 388.27,Z = 4,Dc = 1.513 g/cm3,μ(MoKα) = 2.549 mm-1,F(000) = 792,the final R = 0.033 and wR = 0.062 for 3098 observed reflections(Ⅰ 2σ(Ⅰ)).     

On the Crystal Structure of [Cu（OH）2（HeO）2（4-C5H4NCOOH）2]

The compound described as [Cu(OH)2(H2O)2(4-C5H4NCOOH)2] in Chin. J. Struct. Chem.,2001, 20:478-480 is instead the compound [Cu(H2O)4(4-C5H4NCOO)2], whose crystal structure has already been published elsewhere.     

An Efficient Synthesis of Highly Optically Active 4-Substituted-2（5H）-furanones from Chiral 3-Bromo-2（5H）-furanone

Highly optically active 4-substituted-2(5H)-furanones 6a-6j were obtained in good yields with de≥98% by the tandem Michael addition/elimination reaction of chiral 3-bromo-2(SH)-furanone (4a), which was conveniently prepared starting from 2-furaldehyde under mild conditions. The products were identified on the basis of their satisfactory elemental analysis and spectroscopic data of IR, UV, ^1H NMR, ^13C NMR and mass spectra. The stereochemistry and absolute configuration of this type of compounds were established by the X-ray crystallographic study. The reaction provided a short and efficient synthesis of the interesting highly optically active 4-subsdtuted-2(5H)-furanones containing an active pyrimidine and a purine base group.     

STRUCTURE OF {Mo4S4（μ—OAc）2[S2P（OC2H5）2]4H}

<正> {Mo4S4(μ-OAc)2(dtp)4H}3,(dtp=S2P(OEt)2),Mr=1371.60,Or-thorhombic, space group Pcab, a = 18. 90 (2) ,b = 21. 678 (4 ) , c = 24. 491 (4 ) A , V = 10031(7)A3,Z=8,Dc=1.818g/cm-3,F(000)=5464,λ(MoKa)=0.71073A,finalR= 0. 069 for 3738 independent reflections. This is a successful example of the formation of [Mo4S4]5+ from[3+1] reaction mode. The results of the structure determination indicate that the configuration of the title compound exhibits a tetranuclear cubane-type core [Mo4S4]5+ with six Mo - Mo distances in the range 2. 685~2. 969A and is very similar to that of the previously characterized compound {Mo4S4(μ-OAc)2(dtp)4}2, [Mo4S4]6+, which was obtained directly by the reaction of MoCl3·3H2O with dtp. Some notable differences, however, can be found when six Mo - Mo bond distances and bonding parameters of the four terminal bidentate ligands (dtp) are compared between these two compounds , That can be attributed to the difference in the oxidation state of these two clusters .     

Synthesis and Anti-inflammatory Action of （η-C5H5 ）2Ti（ Sal）2 and （η-C5H5 ）2Ti（Clo）2

IntroductionSince K pf[1]discovered that dicyclopenta die-nyltitanium dichloride possesses antitumour action in1979,a large number of cyclopentadienyltitanium com-plexes with different substituents have been synthe-sized[2,3].The experimental data reveal …     

Syntheses and Structural Characterization of 1-（4-Phenyl-2-thiazolyl）-3-（4-methylphenyl）-5-（2-furyl）-4,5-dihydro-（1H）-pyrazole and 1-（4-（4-Fluoro）phenyl-2-thiazolyl）-3-（4-methyl-phenyl）-5-（2-furyl）-4,5-dihydro-（1H）-pyrazole

The title compounds were synthesized and characterized by IR,1H-NMR,Mass and elementary analysis and single-crystal X-ray diffraction.In 1a,intermolecular C-H…π interactions produce a three-dimensional network.In 1b,intermolecular C-H…O hydrogen bonds generate an R22(22) ring.The hydrogen bonding is supported by C-H…π interactions.     

[（η^5—C5H4Si2Me5）（CO）（PPh3）2MoBr]络合物的合成

三羰基环戊二烯基卤钼络合物与三苯基膦或三乙基膦的反应有过研究,但都是单pph3配合,双pph3配合的溴钼络合物至今未见详细报道,本文通过三羰基(五甲基乙硅基)环戊二烯基溴钼络合物与三苯基膦反应制取双pph3配