Synthesis and Crystal Structure of a 3-D Hydrogen-bonded Supramolecular Decavanadate Compound [Habo]6[V10O28]·2C3H7OH·2H2O

A new inorganic-organic hybrid supramolecular compound [Habo]6[V10O28]·solvents and its crystal structure was reported as follows: monoclinic, space group P21/n, a =11.419(9), b = 16.811(16), c = 15.521(12) (A), β= 102.98(2)°, V= 2903(4) (A)3, Z = 4, C15H46N3O19V5,Mr = 827.25, Dc = 1.893 g/cm3, λ(MoKα) = 0.71073 A,μ = 1.636 mm-1, F(000) = 1696, the final R =0.0696 and wR = 0.1361 for 4641 observed reflections with I ＞ 2σ(I). The compound is based on decavanadate clusters [V 1oO28]6-. The hydrogen bonding interactions among Habo+ cations, solvents and decavanadate clusters extend 1 into a three-dimensional supramolecular architecture.     

Synthesis,Crystal Structure and Antimicrobial Study of N,N,N''-Tris(3-aminopropyl)ethylenediamine Copper(Ⅱ) Diperchlorate

The title compound [Cu(C11H29N5)](ClO4)2 was synthesized and characterized by elemental analysis,IR and X-ray single-crystal diffraction.The compound crystallizes in the monoclinic system,space group P21/n with a = 9.405(2),b = 14.495(3),c = 14.715(3)(A),β = 90.262(3)°,V =2006.1(7)(A)3,Mr = 493.83,Z= 4,F(000) = 1028,Dc= 1.635 g/cm3,T= 298(2) K,μ = 1.403 mm-1 and λ = 0.71073(A).The structure was refined to R = 0.0508 and wR = 0.1250 for 2293 observed reflections with I ＞ 2σ(I).The Cu(Ⅱ)atom possesses a five-coordinate CuN5 environment which shows a slightly distorted square-pyramidal geometry.Antimicrobial activity study found that the complex is active against Salmonella species,Staphylococcus aureu,Bacillus pumilus and Bacillus coliforms.     

Synthesis, Crystal Structure and Photoluminescent Property of a 3D Hydrogen-bonded Supramolecular Compound with Large Channels

The title compound, [Pd（2,2′-bipy）2]（Haadip）2·4H2O, was synthesized via the hydrothermal reaction of PdCl2 with 5-aminodiacetic isophthalic acid （H4adip） in an acetic acid water solution. It was characterized by elemental analysis and infrared spectrum. Crystal data for C44H44N6O20Pd： monoclinic, space group P21/n, a = 11.0674（2）, b = 9.9716（2）, c= 20.5770（3）A, β = 92.7300（3）°, V = 2268.29（7）A^3, Z = 2, Mr = 1083.25, Dc = 1.586 g/cm^3, F（000） = 1112,μ = 0.499 mm^-1, 2（MoKa） = 0.71073 A, T = 293（2） K, 2θmax = 51.38°, GOOF = 1.067, R = 0.0268 and wR = 0.0710 for 3770 reflections with 1 〉 2σ（I）. X-ray diffraction studies reveal that the title compound has an interesting 3D microporous architecture via hydrogen bonds with the cations located inside the channel.     

Syntheses and Crystal Structures of Methyl 2-（4,5-Dibromo- 1-methylpyrrole-2-carbonylamino）-3-phenyl propanoate and 4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole

1 INTRODUCTION Pyrrole and its derivatives have attracted much attention due to their chemical properties as well as biological activities[1]. They have been widely used as the materials to produce pharmaceutical, essences, biochemicals, etc. It has been found that a great deal of pyrrole derivatives present bioactivities, such as antitumor and antiviral activities[2~5]. Thus, due to the interest in exploring the syntheses of potential bioactive materials which contain pyrrole ring andna…     

Synthesis and Crystal Structure of the Copper Complex {[Cu（CH3COO）2（bbtz）]（H2O）2}n

1 INTRODUCTION The design and synthesis of metal-organic frame- work structures have been extensively studied due to their unexpected properties for potential applications as functional materials as well as the intriguing ar- chitectures and topologies[1～4]. When rigid bifunc- tional ligands are used to connect metal centers, to- pology of the network is usually determined by the coordination geometry of the central metal prefer- ence. Contrary to rigid ligands, the bifunctional fle- xib…     

Crystal Structure of a Ternary Copper(Ⅱ) Complex of N,N'-(p-Xylylene)dialanine Acid and 1,10-Phenanthroline

The compound [Cu2(bpy)2(PDIAla)(H2O)2](ClO4)2·H2O(H2PDIAla = N,N'-(p-xylylene)dialanine,bipy = 2,2'-bipyridine) 1 has been synthesized and structurally determined by single-crystal X-ray diffraction,elemental analyses and IR spectroscopy.The crystal belongs to the monoclinic system,space group P21 with a = 10.9772(6),b = 18.5464(9),c = 11.0790(6) ,β = 116.3110o,V = 2021.87(18) 3,Z = 2,Dc = 1.594 Mg/m3,Mr = 970.70,μ = 1.260 mm-1,F(000) = 996,λ(MoKα) = 0.71073 ,the final R = 0.0400 and wR = 0.1050 for all observed reflections.In the structure,the O(5)-H(52)···O(4) hydrogen bonding between aqua ligand and carbonyl oxygen of the H2PDIAla ligand along the c axis produce hydrogen-bonded helices which are assembled along the b axis through O(61)-H(61)···O(2) and N(6)-H(6N)···O(2) interactions to form 2-D layers that are further linked by π···π interactions between bpy ligands to yield a three-dimensional supramolecular network.     

Synthesis and Crystal Structure of α-(N-Protected amino) β-lactam Derivative of 1,5-Benzothiazepine

The crystal of the title compound C, C30H30N2O3S has been prepared by reaction of 1,5-benzothiazepine with N-protected glycine and determined by X-ray single crystal diffraction. Crystal data: Mr=498.62, triclinic with P space group, a=10.880(2), b=13.955(3), c=9.537(2)(A), α=99.34(3)°, β=110.43(3)°, γ=88.56(3)°, V=1338.2(5)(A)3, F(000)=528, λ(MoKα)=0.71073(A), Z=2, Dc=1.237g/cm3, μ=0.154mm-1. Final R=0.0453, wR=0.1256 for 3491 observed reflections [I>2σ(I)]. Structure analysis reveals that the substituents at C(23) and C(7) in four-membered ring are located on the same side. The conformation of seven-membered ring is chair-like.     

Synthesis and Crystal Structure of [（ArO）2Sm（OPPh3）（μ—OH）]2（ArO=2,6—tBu—4—Me—C6H2O）

1 INTRODUCTION In recent years, the syntheses, structures and reactivities of aryloxo lanthanide complexes have attracted a great deal of attention due to their various applications as homogeneous catalysts for organic reactions and precursors for organolan- thanide syntheses[1]. However, the reactivity of divalent lanthanide aryloxides has seldom been studied[2]. We have previously reported that (ArO)2- Sm(THF)4 (ArO = OC6H2-2,6-di-tert-butyl-4-Me) can efficiently initiate the poly…     

Structure of Low Temperature Phase β—Ba3Y（BO3）3 Crystal

Crystals of the low temperature phase β-Ba3Y(BO3)3 have been synthesized by the flux method. The structure of the title compound crystallizes in the hexagonal system, space group P63cm with the following parameters: a = 9.416(3), c = 17.536(8) A, V= 1346.6(8) A3, Ba3YB3Og,Mr = 677.36, Z = 6, Dc = 5.012 g/cm3, λ(MoKα) = 0.71073 A,μ = 19.409 mm- 1, Flack parameter =0.02(3), F(000) = 1764, R = 0.0714 and wR = 0.1696 for 1076 observed reflections with Ⅰ＞ 2σ(Ⅰ).The compound contains two sets of YO6 octahedra, four sets of BaO9 polyhedra and three sets of BO3 planar triangles.     

Synthesis and Crystal Structure of 5,5-Dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexene-1-one

The title compound 5,5-dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexen-1-one has been synthesized,and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to monoclinic,space group P21/c with a=9.4193(13),b=26.915(4),c=21.188(3),β =101.906(3)°,V =5256.2(13)3,Z =4,C60H68Cl2N2O8,Mr=1016.06,Dc=1.284 g/cm3,F(000)=2160,λ(MoKα)=0.71073,μ=0.182 mm–1,R=0.0530 and wR=0.1131 for 4128 observed reflections (I>2σ(I)). X-ray analysis reveals that there are two independent molecules in the unit and the cyclohexenone rings adopt different conformations. In addition,there are four intramolecular hydrogen bonds in the title molecule.     

Syntheses and Structures of Two New Schiff Base Metal Complexes

1 INTRODUCTION Schiff base ligands have been studied for a longtime due to the instant and enduring popularity fromtheir easy synthesis and versatility complexes. Theyplay an important role in the development of coor-dination chemistry as well as inorganic biochemistry,catalysis, optical materials and so on[1, . Consider- 2]able attention has been focused on the syntheses andstructures of copper(II) and nickle(II) complexes.The nickel complexes with multidentate Schiff baseligands have …     

Crystal Structure of 3-Methyl-4-methoxy-3-(3-methyl-4- methoxy-2-benzofuranyl) -2-H-benzofuranyl

1　ＩＮＴＲＯＤＵＣＴＩＯＮ3ｍｅｔｈｙｌ4ｈｙｄｒｏｘｙｂｅｎｚｏｆｕｒａｎｉｓａｎｉｎｔｅｒｍｅｄｉａｔｅｕｓｅｄｆｏｒｔｈｅｓｙｎｔｈｅｓｉｓｏｆｎａｔｕｒｅｐｒｏｄｕｃｔｓ[1].Ｉｔｈａｓｂｅｅｎｓｙｎｔｈｅｓｉｚｅｄｆｒｏｍ1,3ｄｉｈｙｄｒｏｘｙｂｅｎｚｅｎｅ[2-3].Ｔｏｓｙｎｔｈｅｓｉｚｅａｂｉｅｔａｎｅｑｕｉｎｏｎｅｄｉｔｅｒｐｅｎｏｉｄｓｗｉｔｈｉｔ[4,5],ｗｅｉｎｔｅｎｄｅｄｔｏｐｒｏｔｅｃｔｔｈｅｈｙｄｒｏｘｙａｔｔａｃｈｅｄｔｏｉｔｗｉｔｈＭｅ2ＳＯ4.Ｆｉｎａｌｌｙ,ｔｗｏｃｏｍｐｏｕ…     

Syntheses and Crystal Structures of Two Isomeric Au Complexes

<正>Two new isomeric Au complexes,Au(PPh_3)(bmt),have been synthesized via the reaction of Au(PPh_3)Cl with 2-benzimidazolethiol(Hbmt)in dichloromethane(CH_2Cl_2)solution. Their crystal structures were determined by elemental analysis and single-crystal X-ray diffraction studies.Complex 1 crystallizes in the monoclinic system,space group C2/c with a=19.589(2),b= 21.1368(15),c=23.424(2)(?),β=108.346(4)°,V=9206.1(14)(?)~3,M_r=1216.85,D_c=1.756 g/cm~3,μ=6.566 mm~(-1),F(000)=4704,Z=8,the final R=0.0563 and wR=0.1028 for 8125 reflections with I2σ(I).Complex 2 crystallizes in the monoclinic system,space group P2_l/n with a= 9.627(3),b=21.384(8),c=22.308(8)(?),P=92.068(6)°,V=4590(3)(?)~3,M_r=1216.85,D_c=1.761 g/cm~3,μ=6.585 mm~(-1),F(000)=2352,Z=4,the final R=0.0500 and wR=0.0883 for 10477 reflections with I2σ(I).X-ray diffraction studies reveal that complexes 1 and 2 both feature a 1D chain along the a axis.     

Syntheses and Structures of Two New Coordination Polymers:[Cu(C14H9O4)(C14H10O4)(C12H12N2)2] and [Ag(C14H9O4)(C13H14N2)]·0.5 H2O

Under hydrothermal conditions, two new ribbon-like structures, [Cu(C14H9O4)-analysis revealed that these structures were constructed by mixed ligands. The coordination polymer forms the basic architecture while the weak interactions extend the framework into a secondary structure. The whole structures of them are governed by collaboration of the strong and weak interactions. Compound 1 crystallizes in monoclinic, space group C2/c with a = 17.0485(3), b =1 1.0558(3), c = 22.7623(4) A, β = 102.465(1)°, V = 4189.2(2) A3, Z = 4, Mr = 915.44, Dc = 1.451g/mL, F(000) = 1900 andμ(MoKα) = 0.587 cm-1. The final R and wR are 0.0030 and 0.1022,respectively for 3037 observed reflections with I ＞ 2σ(I). Compound 2 crystallizes in monoclinic,space group P21/c with a = 11.5963(4), b = 11.7004(5), c = 17.1254(5) A,β = 95.620(1)°, V =2312.4(1) A3, Z = 4, Mr = 556.35, Dc = 1.598 g/mL, F(000) = 1132 andμ(MoKα) = 0.912 cm-1The final R and wR are 0.0431 and 0.1050, respectively for 2629 observed reflections with I ＞ 2σ(I).     

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

The title Schiff base compound,C19H19N3O3,a derivative of antipyrine,has been synthesized and characterized by elemental analysis,IR,and single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group C2/c,with α = 27.935(5),b = 7.553(1),c =16.692(3) (A),β = 105.810(3)°,Z= 8,V= 3388.7(10) (A)3,Dc = 1.323 g/cm3,Mr = 337.37,λ(MoKα) =0.71073 (A),μ = 0.091 mm-1,F(000) = 1424,R = 0.0630 and wR = 0.1273.A total of 3513 unique reflections were collected,of which 2112 with I ＞ 2σ(I) were observed.The molecular structure adopts a trans configuration about the C=N double bond.The pyrazoline and C(1)～C(6) pheny1 ring are approximately coplanar (mean deviation from the combined plane is 0.069(3) (A)),with the dihedral angle of 9.7(2)°.The preliminary biological tests show that the compound has high antibacterial activities.     

Two Cobalt(Ⅱ) Complexes Derived from the Hydrolysis Product of Di-Schiff Base Ligand N,N'-Bis-(1-benzimidazo-2-ylethylidene)-ethane-1,2-diamine: Preparation,Characterization and Crystal Structure of the 6-Coordinate Species [CoL2]X·H2O (X = ClO4-,NO3-)

The reactions of Co(CIO4)2.6H2O and Co(NO3)2·6H2O with the di-Schiff base ligand N,N'-bis-(1-benzimidazo-2-yl-ethylidene)-ethane-1,2-diamine (LA) in ethanol have been investigated.The reactions of LA with excess amount of cobalt salts yield the six-coordinate complexes [CoL2](CIO4)2·H2O 1 and [CoL2](NO3)2·H2O 2 as isolatable products (L = N-(1-benzimidazo-2-yl-ethylidene)-ethane-1,2-diamine), where L is a tri-dentate mono-Schiff base ligand, resulting from the hydrolysis of the precursor di-Schiff base LA.Both complexes were characterized by X-ray crystallography.Crystal data for complex 1: monoclinic, space group P21/c, a = 11.9214(10), b = 23.5828(17), c = 14.0387(12)(A), β= 135.219[4]°,C22H30CI2CoN9O9,Mr = 680.37, V = 2780.1(4)(A)3, Z = 4, Dc = 1.625 g/cm3,μ(MoKa) = 0.876 mm-1, F(000) = 1404,the final R = 0.0725 and wR = 0.1530 for 5726 observed reflections (I＞2σ(I)).Crystal data for complex 2: monoclinic, space group P21/c, a = 18.2162(16), b = 10.0610(6), c = 18.593(2)(A),β=130.099(3)°, C22H30CoN10O7, Mr = 605.49, V = 2606.5(4)(A)3, Z = 4, Dc = 1.543 g/cm3,μ(MoKα)= 0.722 mm-1, F(000) = 1260, the final R = 0.0619 and wR = 0.1429 for 5194 observed reflections (I ＞ 2σ(I)).X-ray diffraction analysis reveals that each cobalt atom in the two complexes is chelated by six nitrogen atoms from two tridentate iigands L, exhibiting a slightly distorted octahedral coordination sphere.In both complexes, the strong hydrogen-bonding interactions between the lattice waters and N-H groups of the ligands result in 1D chains which are further connected by ClO4- (or NO3-) groups to form a 3D framework.In complex 2, the strong π-π interactions increase the stability of the structure.     

Synthesis and Crystal Structure of a Dicyanamide-bridged One-dimensional Gadolinium(Ⅲ) Complex [Gd(dca)3(phen)2(H2O)]n

A chainlike coordination polymer [Gd(dca)3(phen)2(H2O)]n (dca = dicyanamide,phen = 1,10-phenanthroline) has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a = 10.6581(13), b = 15.6129(16), c = 17.733(3) (A), β = 90.499(5)°, V = 2950.8(7) (A)3, Z = 4,C30H18GdN13O, Mr = 733.82, Dc= 1.652 g/cm3, F(000) = 1444, λ(MoKα) = 0.71073 (A),μ = 2.297 mm-1, R = 0.0258 and wR = 0.0616 for 4570 observed reflections (I ＞ 2σ(Ⅰ)). In this complex, the gadolinium atom is nine-coordinated by four dca anions, two chelated phen ligands and one H2O molecule in a distorted tricapped trigonal prism. Two bridging dca anions connect the Gd(Ⅲ) ions yielding chainlike polymers that are linked by hydrogen bonds and π-π interactions to form a three-dimensional network.     

Syntheses and Crystal Structures of Mono- and Binuclear Copper( Ⅱ ) Mixed-ligand Complexes Involving Schiff Base

The mononuclear copper(Ⅱ) complex [Cu(L)(2-AP)] 1 and binuclear copper(Ⅱ)complex [Cu(L)(py)]2 2 (L = C1oH1 1O5NS, taurine o-vanillin, py = prydine, 2-AP = 2-aminopyridine)with mixed ligand have been synthesized and characterized by X-ray diffraction method. Crystal data for 1: orthorhombic, space group Pbca with a = 11.921(4), b = 15.816(6), c = 17.076(6) (A), V=3219.7(19) (A)3, C15H17CuN3O5S, Z = 8, Mr = 414.92, Dc = 1.712 g/cm3,μ(MoKα) = 1.520 mm-1,F(000) = 1704, the final R = 0.0300 and wR = 0.0705 for 2840 observed reflections with I ＞ 2σ(I);and crystal data for 2: monoclinic, space group P21/c with a = 7.929(3), b = 17.038(5), c = 11.734(4)(A), β = 98.162(6)°, V = 1569.1 (9) (A)3, C15H16CuN2O5S, Z = 4, Mr = 399.90, Dc = 1.693 g/cm3, F(000)= 820,μ(MoKα) = 1.554 mm-1, the final R = 0.0351 and wR = 0.0848 for 2767 observed reflections (I ＞ 2o(I)). The molecular structure of complex 1 consists of one tetra-coordinated Cu(Ⅱ) atom generating a slightly distorted square plane, and a one-dimensional chain structure is formed by intermolecular hydrogen bonds. Complex 2 consists of a diphenolic hydroxyl O-bridged binuclear copper(Ⅱ) structure. The crystal structures of complexes 1 and 2 reveal that the coordinate copper centers are bound to both nitrogen and oxygen atom donors. The usual N,O-trans arrangement of ligands is observed in both cases.     

Synthesis, Crystal Structure and Luminescent Property of a Novel Pt(II) Complex with Weak Metal-metal Interaction

The title complex cis-bis(tetrahydrothiophene)-bis(nitrate) platinum(II), (tht)2Pt(NO3)2, was the reducing product from potassium hexachloroplatinate(IV) K2PtCl6 where the platinum is tetra-valenced. Crystal data for C8H16N2O6PtS2: monoclinic, space group P21/c, a = 9.8833(5), b = 8.6744(4), c = 18.6407(9) (A), β = 114.401(3)°, V = 1455.35(12) (A)3, Z = 4, Mr = 495.44, Dc = 2.261 g/cm3, F(000) = 944, μ = 9.950 mm-1, λ(MoKα) = 0.71073 (A), T = 293(2) K, 2θmax = 54.96o, GOOF = 1.033, R = 0.0350 and wR = 0.0785 for 2572 observed reflections with I > 2σ(I). X-ray diffraction studies reveal that the title complex has interesting weak metal-metal interactions and two molecules linked by metal-metal interaction exist as a group. Luminescent spectrum illuminates red emission of the complex at room temperature.     

Synthesis and Crystal Structure of Complex [Cdq3] [Cd（qH）3]（ClO4）CH3OH（q = 8-Quinolinolate, qH = 8-Quilinolinol）

1 INTRODUCTION 8-Quinolinolate is a very useful ligand and used to synthesize many complexes with special physical properties. For example, the complex tris(8-quinoli- nolate)aluminum(III) displays distinguished physical property in the area of electroluminescence ma- terials[1]. Based on tris(8-quinolinolate)aluminum(III), high-luminance low-voltage driven devices have been made, which opens the route to design low-cost large area displays and illuminators. The crystals thatcontain com…