Addition Reaction of Bis（diphenylphosphinyl） Butadiyne with Methylcyclopentadiene

Bis(diphenylphosphinyl)butadiyne reacted with methylcyclopentadiene at room tem- perature and four isomeric products were obtained. Crystal structures of isomers 1 and 3 have been determined. Crystal data for compound 1 C40H36O2P2·2CHCl3: monoclinic, space group C12/c1 with a = 17.983(2), b = 11.8723(12), c = 20.081(2) , β = 111.218(3)°, V = 3996.5(8) 3, Z = 4, Mr = 849.36, Dc = 1.412 g/cm3, F(000) = 1752, μ = 0.546 mm-1, the final R = 0.0351 and wR = 0.0951 for 3965 observed reflections (I > 2σ(I)); and those for compound 3 C40H36O2P2·H2O: triclinic, space group P1 with a = 10.4144(15), b = 13.0558(18), c = 13.742(2) , α = 70.453(8), β = 75.382(8), γ = 72.312(8)°, V = 1653.7(4) 3, Z = 2, Mr = 628.64, Dc = 1.262 g/cm3, F(000) = 664, μ = 0.169 mm-1, the final R = 0.0593 and wR = 0.1296 for 4891 observed reflections (I > 2σ(I)). The structures of the other two isomers are identified via IR, 1H NMR and MS spectra.     

Synthesis and Single Crystal X-ray Studies of 3-(3,5-Bis(trifluoromethyl)phenyl) Quinoline and 3-(4-Fluoro-3-methylphenyl) Quinoline

The title compounds 3-(3,5-bis(trifluoromethyl)phenyl)quinoline(1) and 3-(4-fluoro-3-methylphenyl)quinoline(2) were synthesized through Suzuki-Miyaura Cross coupling reaction of 3-bromoquinoloine with aryl boronic acids.The title compounds were characterized by single-crystal X-ray diffraction,1H NMR,13C NMR,EI-MS,elemental analysis and IR.The crystals of 3-(3,5-bis(trifluoromethyl)phenyl)quinoline(C17H9F6N,Mr = 341.25) belongs to the monoclinic system,space group P21n,a = 12.3072(13),b = 4.9378(6),c = 24.493(2) ,V = 1473.1(3) 3,Z = 4,Dc = 1.539 Mg m-3,λ = 0.71073 ,μ = 0.144 mm-1,F(000) = 688,the final R = 0.0715 and wR = 0.1873 for 1875 observed reflections with I 2σ(I) and the crystal of 3-(4-fluoro-3-methylphenyl)quinoline(C16H12FN,Mr = 237.27) belongs to the orthorhombic system,space group Pca21,a = 23.794(2),b = 3.9094(3),c = 25.669(2) ,V = 2387.7(4) 3,Z = 8,Dc = 1.320 Mg m-3,λ = 0.71073 ,μ = 0.088 mm-1,F(000) = 992,the final R = 0.0534 and wR = 0.1188 for 2270 observed reflections with I 2σ(I).     

Syntheses, Crystal Structures and Characterization of Layered and Layer-pillared Zinc Arsonates

Two zinc arsonate coordination polymers, Zn(4-apa)·H2O (1, 4-apaH2 = 4-amino- phenylarsonatic acid) and Zn(4-apa) (2), have been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal and powder X-ray diffraction. Crystal data for 1: monoclinic, space group C2/c with a = 23.056(5), b = 5.4224(11), c = 15.027(3) , β = 121.22(3)°, V = 1606.6(6) ?3, Dc = 2.468 g·cm-3, F(000) = 1168, μ = 7.122 mm-1, Z = 8, the final R = 0.0309 and wR = 0.0752 for 1763 observed reflections with I > 2σ(I). For 2: monoclinic, space group P21/c with a = 8.7852(18), b = 9.2744(19), c = 9.752(2) , β = 103.45(3)°, V = 772.7(3)3, Dc = 2.410 g·cm-3, F(000) = 544, μ = 7.387 mm-1, Z = 4, the final R = 0.0321 and wR = 0.0741 for 1696 observed reflections with I > 2σ(I). The structure of 1 shows a two-dimensional (4,4)-network composed of an inorganic ladder chain bridged by the phenyl-linkers of 4-apa ligands. Compound 2 exhibits a 3D layer-pillared framework with crb net, in which inorganic (4-82)-networks are joined by the phenyl-linkers.     

Synthesis and Crystal Structure of（3S,4R,Z）-3,6-dimethyl-2-（3-methylbut-2-enylidene）-2,3,3a,4,7,7a-hexahydrobenzofuran-3,4-diol

The title compound of(3S,4R,Z)-3,6-dimethyl-2-(3-methylbut-2-enylidene)-2,3,3a,4,7,7a-hexahydrobenzofuran-3,4-diol,C15H22O3,as a potential gastric cytoprotective agent has been synthesized by the reduction of bisabolangelone in methanol with sodium borohydride.The title compound was characterized by IR and NMR spectra.Meanwhile,the crystal was obtained and determined by X-ray single-crystal diffraction.Crystal data:monoclinic system,space group P21 with a = 6.0692(12),b = 8.9954(18),c = 13.182(3) ,β = 92.59(3)°,V = 718.9(2) 3,Z = 2,F(000) = 272,Dc = 1.156 g/cm3,μ = 0.633 mm-1,R = 0.0362 and wR = 0.1051 for 9490 independent reflections(Rint = 0.0172) and 2461 observed reflections(I > 2σ(I)).Intermolecular O-H…O interactions link the molecules into one-dimensional infinite chains running along the b axis,which contributes to the stability of the crystal structure.     

Syntheses and Crystal Structures of 3-Carboxylsalicylidenefurfurylimine And Its Trinuclear Nickle(Ⅱ) Complex

A Schiff base ligand(H2CSF,C13H11NO4,1) derived from 3-carboxylsalicylaldehyde and furfurylamine,and its trinuclear complex [Ni3(CSF)2(CH3COO)2(DMF)2(H2O)2](2) were synthesized.Compound 1 was characterized by elemental analysis,1H NMR,IR,MS and X-ray diffraction analysis.The crystal of 1 belongs to the monoclinic system,space group P21/c with a = 8.472(2),b = 19.743(5),c = 7.2300(18) ,β = 110.278(4)°,V = 1134.4(5) 3,Z = 4,Mr = 245.23,Dc = 1.436 g·cm-3,μ = 0.108 mm-1,F(000) = 512,λ = 0.71073 ,the final R = 0.0440 and wR = 0.1199 for 1426 observed reflections(I 2σ(I)).In the crystal of 1,there exist intramolecular hydrogen bonds and weak intermolecular C-H···O hydrogen bonds.Compound 2 was characterized by elemental analysis,IR,TG and X-ray diffraction analysis.The crystal of 2 is of triclinic system,space group P1 with a = 10.1237(17),b = 10.4086(18),c = 10.4884(18) ,α = 82.528(2),β = 67.339(2),γ = 83.010(2)°,V = 1008.1(3) 3,Z = 1,Mr = 962.87,Dc = 1.586 g·cm-3,μ = 1.463 mm-1,F(000) = 498,λ = 0.71073 ,the final R = 0.0517 and wR = 0.0805 for 2065 observed reflections(I 2σ(I)).The geometry of the trinuclear molecule is centrosymmetric,in which every Ni(Ⅱ) ion is coordinated in a slightly distorted octahedron.The three Ni(Ⅱ) ions are arranged in a straight line.The two CSF2-ions act as NOO tridentate ligands with the phenolate and carboxylate oxygen as bridging atoms.The coordination atoms of CSF2-anions and water molecules are coordinated on the equatorial plane,while the two bridging acetate ions and two DMF are trans-coordinated on the apical sites.     

Syntheses,Crystal Structures and Electrochemical Properties of Supramolecular Complexes [M4L12]·（HPO4）·（PO4）2（L=2,2＇-Dibenzimidazole,M=Co and Ni）

Two novel supramolecular complexes,[M4L12]·(HPO4)·(PO4)2(L = 2,2'-dibenzi-midazole,M = Co and Ni) were synthesized by the hydrothermal method and characterized by elemental analysis,IR,UV,and TG-TGA,and the crystal structures were determined by single-crystal X-ray diffraction.The results showed that both of them belong to the cubic system and space group I 4 3d.Crystal parameters of C168H121Co4N48O12P3(1):a = b = c = 2.5104(6) nm,V = 15.820(7) nm3,Mr = 3332.75,Z = 4,Dc = 1.399 Mg/m3,μ = 0.521 mm-1,F(000) = 6852,S = 1.011,the final R = 0.0248 and wR = 0.0663 for 2120 observed reflections(I > 2σ(I)) and R = 0.0315 and wR = 0.0706 for all data.Crystal parameters of C168H121Ni4N48O12P3(2):a = b = c = 2.4977(5) nm,V = 15.581(5) nm3,Mr = 3331.87,Z = 4,Dc = 1.420 Mg/m3,μ = 0.587 mm-1,F(000) = 6868,S = 1.074,the final R = 0.0443 and wR = 0.1364 for 1774 observer reflections(I > 2σ(I)) and R = 0.0647 and wR = 0.1492 for all data.Each of them consisted of four M(II) cations,twelve 2,2'-dibenzimidazole ligands,one monohydrogen phosphate anion and two phosphate anions in the single cell.The central M(II) cation,coordinated with six alkaline nitrogen atoms from three 2,2'-dibenzimidazole ligands,displayed the expected distorted-octahedral geometry.The 3D supramolecular system was formed by the hydrogen bond N-H...O and π-π stacking interaction between neighboring single cells.Complex 1 showed two irreversible single-electron reduction processes of the central metal ion at-0.06 and-0.42 V in DMF solution.     

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.     

Two Metal-organic Frameworks（MOFs） Assembled from One Asymmetric Semirigid Multicarboxylate Ligand：Syntheses and Crystal Structural Characterizations

Hydrothermal reactions between a new flexible multicarboxylate ligand of 3-(2-carboxy-phenoxy)-benzoic acid(H2L) and transitional metal cations of M2+(M = Cu2+,Ni2+) in the presence of the secondary ligands of 1,10-phenanthroline(phen),2,2'-bipyridine(2,2?-bpy),and 4,4'-bipyridine(4,4'-bpy) afford two novel coordination polymers Ni2(H2O)2L2(phen)(μ-4,4'-bpy)(1) and CuIIL(2,2'-bpy)(2).Both compounds were characterized by X-ray crystallography.Crystal data of 1:C31H24N3NiO7,Mr = 609.24,monoclinic,space group P21/c,a = 17.560(8),b = 10.528(5),c = 30.613(15) ,V = 5659(5) 3,Z = 4,Dc = 1.430 g/cm3,F(000) = 502,μ = 0.739 mm-1,R = 0.0902,wR = 0.1346(I > 2σ(I)),S = 1.002.Crystal data of 2:C24H16CuN2O5,Mr = 475.93,monoclinic,space group P21/n,a = 9.8904(13),b = 11.0782(16),c = 18.321(3) ,β = 11.0782(16)°,V = 1993.8(5) 3,Z = 4,Dc = 1.585 g/cm3,F(000) = 972,μ = 1.137 mm-1,R = 0.0433,wR = 0.0723(I > 2σ(I)) and S = 1.004.Compound 1 displays a one-dimensional(1D) zigzag chain structure constructed from phen ligands and the deprotonated ligands of L2-,which further forms a ladder-shaped supramolecular architecture via the bridge of 4,4'-bpy ligand.Complex 2 also possesses a ladder-shaped architecture based on the dinuclear CuII units.     

Syntheses, Crystal Structures and Magnetism of Two New Coordination Polymers [Ni（bix）2Cl2]n and [Co（bix）Cl2]n

The self-assembly reactions of MIICl2 (M = Ni, Co) with the flexible bix ligand [bix = 1,4-bis(imidazole-1-ylmethyl)benzene] yielded a 2D network [NiII(bix)2Cl2]n 1 and a 1D chain [CoII(bix)Cl2]n 2. Their crystal structures have been determined by X-ray single-crystal diffraction analysis. Complex 1 characters a two-dimensional grid-type structure and crystallizes in monoclinic, space group P21/c with a = 7.7231(7), b = 12.7787(9), c = 13.9374(13) , β = 105.419(4)o, C28H28Cl2N8Ni, Mr = 606.19, Ζ = 2, V = 1326.0(2) 3, Dc = 1.518 g/cm3, μ = 0.969 mm-1, F(000) = 628, R = 0.0429 and wR = 0.0783 for 2503 observed reflections (I > 2σ(I)). Compound 2 is a one-dimensional chain and crystallizes in orthorhombic, space group Pbca with a = 11.3696(6), b = 10.2128(6), c = 14.4943(9) , C14H14Cl2CoN4, Mr = 368.12, Z = 4, V = 1683.01(17) 3, Dc = 1.453 g/cm3, μ = 1.334 mm-1, F(000) = 748, R = 0.0317 and wR = 0.0800 for 1778 observed reflections (I > 2σ(I)). Magnetic properties of the title complexes were also investigated.     

Syntheses,Crystal Structures and Properties of Three New Complexes [Ni（C9N2O2H7）2（CH3OH）2],[Zn（C9N2O2H7）2（H2O）2] and [Cd（C9N2O2H7）2（CH3OH）2]

Three novel metal-organic complexes with formulas [Ni(C9N2O2H7)2(CH3OH)2](1),[Zn(C9N2O2H7)2(H2O)2](2) and [Cd(C9N2O2H7)2(CH3OH)2](3) were synthesized by the reactions of Ni,Zn and Cd salts with ethyl 2-benzimidazolylacetate under hydrothermal conditions or layering technique,and characterized by single-crystal X-ray diffraction analysis,IR spec-troscopy,solid-state luminescent properties and thermogravimetric(TG) analysis.The crystal data for these three complexes are as follows:for 1,monoclinic,space group P21/c,a = 9.384(3),b = 9.634(3),c = 11.292(3) ,β = 95.787(5)°,V = 1015.7(5) 3,Z = 2,F(000) = 492,Dc = 1.547 Kg/m3,μ = 1.002 mm-1,the final R = 0.0451 and wR = 0.0900 for 1833 observed reflections with Ⅰ 2σ(Ⅰ);for 2,orthorhombic,space group Pbca,a = 10.031(4),b = 10.379(4),c = 17.525(7),V = 1824.6(12) 3,Z = 4,F(000) = 928,Dc = 1.645 Kg/m3,μ = 1.392 mm-1,the final R = 0.0452 and wR = 0.0996 for 1661 observed reflections with Ⅰ 2σ(Ⅰ);for 3,monoclinic,space group P21/c,a = 9.9114(13),b =10.4852(15),c = 10.4120(14) ,β = 108.453(5)°,V = 1026.4(2) 3,Z = 2,F(000) = 532,Dc = 1.705 Kg/m3,μ = 1.110 mm-1,the final R = 0.0322 and wR = 0.0805 for 1822 observed reflections with Ⅰ 2σ(Ⅰ).In the three complexes,the ethyl 2-benzimidazolylacetate shows the same chelating mode,and the adjacent units are interlinked into a two-dimensional layer through hydrogen-bonds(O-H···O,N-H···O).     

Two New Three-dimensional Supramolecular Complexes with 5-Carboxyl-1-carboxymethyl-2-oxidopyridinium: Syntheses and Crystal Structures

Two new supramolecular complexes [MnL(H2O) 4](1) and [ZnL(H2O) 5]·0.25H2O(2) (H2L = 5-carboxy-1-carboxymethyl-2-oxidopyridinium) have been synthesized and structurally characterized by elemental analysis,IR and X-ray single-crystal structure determination. Complex 1 crystallizes in the monoclinic system,space group P21/n with a = 5.1537(2) ,b = 21.2008(9) ,c = 10.9727(4) ,β = 99.182(2) °,V = 1183.54(8) 3,C8H13MnNO9,Mr = 322.13,Dc = 1.808,Z = 4,F(000) = 660,μ = 1.160,R = 0.0372 and wR = 0.0750 for 2217 observed reflections(I > 2σ(I)) . Complex 2 crystallizes in the triclinic system,space group P1 with a = 7.730(2) ,b = 8.030(2) ,c = 11.400(2) ,α = 104.27(3) ,β = 92.93(3) ,γ = 102.67(3) °,V = 664.9(2) 3,C8H15.5ZnNO10.25,Mr = 355.08,Dc = 1.774,Z = 2,F(000) = 365,μ = 1.899,R = 0.0243 and wR = 0.0695 for 2759 observed reflections(I > 2σ(I)) . Their thermal properties have been studied.     

Synthesis and Crystal Structure of a New Nickel（II） Complex with 2,4-Pyridinedicarboxylic Acid and 1,4-Bis（imidazol-1-ylmethyl）-benzene） Ligands

A metal-organic coordination polymer [Ni(PDC)(bix)(H2O)]n (H2PDC = 2,4-pyri- dinedicarboxylic acid, bix = 1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. Blue crystals crystallize in the monoclinic system, space group C2/c with a = 25.1475(18), b = 13.1621(9), c = 14.2739(10), β = 118.4150(10)o, V = 4155.4(5) 3, C21H19N5NiO5, Mr = 480.12, Dc = 1.535 g/cm3, F(000) = 1984, Z = 8, μ(MoKα) = 0.979 mm-1, the final R = 0.0478 and wR = 0.1004 for 3727 observed reflections (I > 2σ(I)). The structure of 1 exhibits a one-dimensional chain-like structure.     

Syntheses and Crystal Structures of Two Silver（Ⅰ） Complexes with Organic Carboxylic Acid and Bidentate N-donor Ligands

The title complexes(NH4)[Ag(dpe)(H2bptc)](1) and Ag2(bpy)(ox)·7H2O(2) were synthesized via slow evaporation at room temperature,and characterized by elemental analysis and infrared spectra.The crystal of 1 crystallizes in triclinic,space group P1 with a = 8.3959(7),b = 11.8088(12),c = 12.8175(13) ,α = 85.507(2),β = 79.245(1),γ = 84.174(2)o,V = 1239.7(2) 3,Z = 2,C28H22AgN3O8,Mr = 636.36,Dc = 1.705 g/cm3,F(000) = 644 and μ(MoKα) = 0.874 mm-1.The final R = 0.0479 and wR = 0.1426 for 3632 observed reflections with I > 2σ(I) and R = 0.0559 and wR = 0.1503 for all data.The crystal of 2 crystallizes in orthorhombic,space group Pnna with a = 17.2291(17),b = 7.5289(6),c = 21.369(2),V = 2771.9(4) 3,Z = 4,C22H30Ag2N4O11,Mr = 742.24,Dc = 1.779 g/cm3,F(000) = 1488 and μ(MoKα) = 1.476 mm-1.The final R = 0.0648 and wR = 0.2058 for 1996 observed reflections with I > 2σ(I) and R = 0.0769 and wR = 0.2192 for all data.X-ray diffraction reveals that in complexes 1 and 2,both 1,2-di(4-pyridyl)ethylene and 4,4'-bipyridine act as typical bidentate N-donor ligands to link two Ag centers.3,3'4,4'-Biphenyltetracarboxylate and oxalate anions play the role of organic linkers and counter-ions to balance the cationic charge of AgI.The rich hydrogen-bonding interactions and ligand-unsupported Ag…Ag interactions as well as π-π stacking interactions contribute to the construction of three-dimensional sandwich-like frameworks.     

Crystal Structure and Photoluminescence of a New Cadmium Complex with 6,7-Dicyanodipyridoquinoxalin

The reaction of CdCl2 with 6,7-dicyanodipyridoquinoxaline (DICNQ) by solvothermal reaction gives rise to a coordination polymer [CdCl2(DICNQ)]n 1. Single-crystal X-ray diffraction analysis reveals that the compound in space group Pbcn creates 1-D chloro-bridging chains. Crystal data for 1: a = 6.756(1), b = 35.371(6), c = 7.027(1) , V = 1679.1(5) 3, Z = 4.00, C16H6CdCl2N6, Mr = 465.57, Dc = 1.842 g/cm3, μ = 1.630 mm-1, F(000) = 904, S = 1.005 and T = 293(2) K. The final R = 0.0376 and wR = 0.1029 for 1291 observed reflections with I > 2σ(I), and R = 0.0499 and wR = 0.1125 for all data. The 1-D chloro-bridging chains are parallel-stacked in the a and b directions, and further stabilized through π-stacking interactions, hydrogen-bonding interactions and C≡N···π interactions to generate a 3-D structure. Compound 1 displays intense bluish-green photoluminescence from the intraligand charge-transfer of the DICNQ ligand and the Cl--to-DICNQ charge-transfer mechanism which is probed by the density of states (DOS) calculations.     

Synthesis,Crystal Structure and Biological Activity of a New 4,5-Diaryl-1H-imidazole Derivative

A new 4,5-diaryl-1H-imidazole was synthesized and characterized by 1H NMR, ESI-MS, elemental analysis and FT-IR. The crystal structure of the title compound(C19H16Cl2N2O2, Mr = 375.24) has been determined by single-crystal X-ray diffraction. Crystal parameters: monoclinic system, space group P21/n, a = 14.349(3), b = 8.7918(18), c = 15.352(3) , β = 108.56(3)°, V = 1836.1(6) 3, Z = 4, F(000) = 776, Dc = 1.357 g/cm3, μ = 0.368 mm-1, the final R = 0.0502 and wR = 0.1066 for 2324 observed reflections with I 2σ(I). A total of 16117 reflections were collected, of which 3615 were independent(Rint = 0.0595). The preliminary bioassay suggested that the title compound exhibits distinct effective inhibition on the proliferation of cancer cell lines.     

Two Cobalt(II) Complexes Derived from the Hydrolysis Product of Di-Schiff Base Ligand N,N'-Bis-(1-benzimidazo-2-yl-ethylidene)-ethane-1,2-diamine:Preparation,Characterization and Crystal Structure of the 6-Coordinate Species [CoL_2]X·H_2O (X = ClO_4~-, NO_3~-)

The reactions of Co(ClO4)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](ClO4)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) , β = 135.219(4)o, C22H30Cl2CoN8O9, Mr = 680.37, V = 2780.1(4) 3, Z = 4, Dc = 1.625 g/cm3, μ(MoKα) = 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) , β = 130.099(3)o, C22H30CoN10O7, Mr = 605.49, V = 2606.5(4) 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 ligands 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.     

Formation and Crystal Structure of 1-（N-tert-butyloxycarbonyl-L-prolyl）-1,3-dicyclohexylurea

The title compound 1-(N-tert-butyloxycarbonyl-L-prolyl)-1,3-dicyclohexylurea formed in the coupling reaction of N-Boc-L-proline and n-butyl amine activated by DCC as an unexpected product was characterized through IR,1H NMR,13C NMR and HRMS spectra as well as single-crystal X-ray diffraction analysis.The crystal(C23H39N3O4,Mr = 421.57) belongs to the orthorhombic system,space group P212121,a = 10.8990(5),b = 12.2153(6),c = 18.8102(9) ,V = 2504.3(2) 3,Z = 4,Dc = 1.118 g/cm3,λ(MoKα) = 0.71073 ,μ = 0.076 mm-1,F(000) = 920,the final R = 0.0572 and wR = 0.1521 for 3564 observed reflections with I > 2σ(I).An intramolecular hydrogen bond N(3)-H…O(2) is observed.     

Characterization and Crystal Structures of Two Copper（Ⅱ） Complexes Constructed by a Flexible Double Betaine Ligand

A flexible double betaine 1,4-bis(pyridinil-4-carboxylato)-1,4-dimethylbenzene L has been used to generate two Cu(II)-containing metal complexes that exhibit different polymeric structures: [Cu(H2O)2 L]·2NO3 1 and [Cu(H2O)3 L]·2Cl·H2O 2. The crystal structures of 1 and 2 have been determined by single-crystal X-ray diffraction method. Crystal data for 1: triclinic, space group P 1, a = 5.253(2), b = 7.406(3), c = 14.792(5) , α = 84.195(5), β = 80.014(5), γ = 78.053(5)°, V = 553.2(3) 3, Z = 1, F(000) = 293, Dc = 1.717 g/cm3, the final R = 0.0385 and wR = 0.1079 for 1883 observed reflections (I > 2σ(I)); and those for 2: monoclinic, space group P21/c, a = 10.222(3), b = 25.287(7), c = 9.277(3) , β = 93.572(5)°, V = 2393.2(12) 3, Z = 4, F(000) = 1140, Dc = 1.540 g/cm3, the final R = 0.0472 and wR = 0.0956 for 3204 observed reflections (I >2σ(I)).     

Synthesis and Crystal Structure of 3,3'-Bis(5-(N-(4-hydroxylphenyl)imidomethyl)- pyrrol-2-yl)pentane·2CH_3OH

3,3'-Bis(5-(N-(4-hydroxylphenyl)imidomethyl)pyrrol-2-yl)pentane 1 has been synthesized and characterized. The crystal of its methanol complex, 1·(CH3OH)2, belongs to the orthorhombic system, space group Pccn with a = 18.094(2), b = 11.6890(16), c = 13.3629(19) , V = 2826.3(7) 3, Z = 8, C14.5H18N2O2, Mr = 252.31, Dc = 1.186 g/cm3, F(000) = 1080 and μ(MoKα) = 0.080 mm-1. The final R = 0.0662 and wR = 0.1801 for 1908 observed reflections with I 2σ(I), and R = 0.0800 and wR = 0.1948 for all reflections. In the solid state, bridged by included methanol molecules, the molecules of compound 1 form interpenetrated grid structure through N–H···O and O–H···O hydrogen bonds.     

Synthesis and Crystal Structure of 3′-Ethyl 5′-Methyl 1-Benzyl-4′-methyl-2-oxo-3′,4′-dihydrospiro-[indoline-3,2′-pyrrole]-3′,5′-dicarboxylate

The crystal structure of the title compound(C24H24N2O5, Mr = 420.45) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 8.991(1), b = 11.166(1), c = 11.169(1) , α = 91.413(2), β = 105.887(2), γ = 90.992(2)°, V = 1077.8(2) 3, Z = 2, Dc = 1.296 g/cm3, F(000) = 444, μ(MoKα) = 0.091 mm-1, the final R = 0.0466 and wR = 0.1507 for 4185 observed reflections(I 2σ(I)). The single-crystal X-ray diffraction data indicated intermolecular C(17)–H(17)O(4), C(5)–H(5)… O(4) hydrogen bonds and C–H…π interaction in the structure.