Synthesis and Crystal Structure of a Luminescent Compound 5-（1H-benzoimidazol-2-yl）- 3H-[ 1,2,3 ] triazole-4-carboxylic Acid

The title compound, 5-(1H-benzoimidazol-2-yl)-3H-[1,2,3]triazole-4-carboxylic acid (C10H7N5O2·C3H7NO, Mr=302.30), has been synthesized and characterized by FT-IR and ESI-MS, 1 H-NMR spectroscopy and X-ray single-crystal diffraction. Crystal structure of the title compound was grown from DMF by slow diffusion at room temperature. Crystal data: orthorhombic structure, space group Pna21 with a=6.9635(3), b=19.4398(7), c=30.6165(12), V=4144.5(3)3, Z=12, Dc=1.454 g/cm 3, μ(MoKα)=0.108 mm-1, and F(000)=1896. The structure was refined to R=0.0450 and wR=0.0975 for 3578 observed reflections with I>2σ(I). The intermolecular hydrogen bonds and π-π stacking further stabilize the structure.     

Synthesis, Crystal Structure and Properties of a Novel Tetranuclear Nickel（II） Complex with Azo-enolic-2-hydroxybenzamide

A novel tetranuclear nickel(Ⅱ) complex [Ni4L2(DMF)2(H2O)2·2DMF] (1,H4L=azo-enolic-2-hydroxybenzamide, DMF=N,N-dimethyl-formamide) has been synthesized and characterized by elemental analysis, UV, IR and X-ray single-crystal diffraction characterization. Complex 1 crystallizes in the monoclinic system, space group P21/n with a=8.8944(11), b=14.4583(18), c=18.097(2) , β=90.00(2)o, Z=2 , V=2327.2(5)3 , C40H48N12Ni4O14 , Mr=1155.66, Dc=1.649g/cm 3 , μ=1.672 mm-1 , F(000)=1192, R=0.0392 and wR=0.0958. The local coordination environment around the nickel ions exist a distorted octahedral and quadrangle geometry in the molecular structure. Complex 1 exhibits strong photoluminescent emission in the ultraviolet region at room temperature. The electrochemical studies reveal that redox of Ni 3+ /Ni 2+ in the complex is a quasi-reversible process.     

Synthesis, Crystal Structure and Fluorescene of a One-dimensional Compound {CdI_2(2,2′-bipy)}_n

The title compound, {CdI2(2,2′-bipy)}n, was prepared by the hydrothermal reac- tion of CdI2 and 2,2′-bipy in an aqueous solution, and its crystal structure was determined by X-ray single-crystal analysis. Crystallographic data for 1: C10H8N2CdI2, monoclinic system, space group C2/c, a = 16.927(1), b = 10.0925(7), c = 7.7422(3) , β = 106.0629(4)°, V = 1271.00(14) 3, Z = 4, F(000) = 944, μ = 6.546 mm-1, Dc = 2.730 g/cm3, Mr = 522.38, the final R = 0.0309 and wR = 0.0805 for 1310 observed reflections (I > 2σ(I)). X-ray crystal structure analysis shows that the Cd atom is coordinated by four iodines and two N atoms from one 2,2′-bipy to form an 1-D chain-like structure through bridging iodines. The fluorescene of the title compound was also discussed.     

Synthesis and Crystal Structure of 3-（4-Bromobenzyloxy）-6-morpholinopyridazine

The title compound 3-(4-bromobenzyloxy)-6-morpholinopyridazine(C15H16BrN3O2) was synthesized,and its crystal structure was studied.It crystallizes in the triclinic system,space group P with a = 8.3408(17),b = 8.8620(18),c = 10.832(2) ,α = 108.09(3),β = 91.28(3),γ = 100.90(3)°,Dc = 1.562 g/cm3,Z = 2,λ = 0.71073 ,μ(MoKα) = 2.769 mm-1,Mr = 350.22,V = 744.5(3) 3,F(000) = 356,the final R = 0.0522 and wR = 0.1366 for 2016 observed reflections with I > 2σ(I).In the crystal structure,the morpholine ring adopts a chair conformation with O(2) and N(3) atoms at the flap positions-0.656(7) and 0.622(6)  out of the mean plane formed by the other four C atoms,respectively.These molecules generate centro-symmetric dimers through intermolecular π-π interaction.     

Hydrothermal Synthesis, Crystal Structure and Magnetic Properties of a Novel Zero-dimensional Manganese（Ⅱ） Complex with 2,2′-Diphenic Acid and 1,10-Phenanthroline Ligands

A novel metal-organic coordination polymer [Mn3(2,2′-dipha)3(phen)6]n·3nH2O (2,2′-dipha = 2,2′-diphenic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthe- sized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and magnetic susceptibility measurements. The crystal crystallizes in triclinic, space group P1 with a = 16.921(5), b = 18.307(5), c = 18.450(5) , α = 113.369(5), β = 108.529(5), γ = 102.984(5)o, V = 4553(2) 3, C114H72Mn3N12O14.25, Mr = 2002.66, Dc = 1.461 g/cm3, μ(MoKα) = 0.488 mm1, the final F(000) = 2058, Z = 2, R = 0.0491 and wR = 0.0980 for 9087 observed reflections (I > 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with two carboxylate oxygen atoms from different carboxylate groups of the same dipha and four nitrogen atoms from two different phen ligands, showing a slightly distorted octahedral geometry. Fur- thermore, it exhibits a zero-dimensional structure with dipha-Mn-phen- as building units. Variable- temperature magnetic measure shows an overall anti-ferromagnetic behavior for compound 1.     

A Manganese(Ⅱ) Coordination Polymer Constructed from Phosphonate Ligand:Synthesis,Crystal Structure and Magnetic Properties

A coordination polymer formulated as[Mn(5-pncH₂)₂H₂O](1,5-pncH₃=5-phosphono-1-naphthalenecarboxylic acid),was hydrothermally synthesized and magnetically characterized.Compound 1 features a three-dimensional structure in which the inorganic chains of[Mn(O-P-O)]_n are cross-linked by the organic groups of phosphonate ligands.Magnetic measurements of 1 indicate that dominant antiferromagnetic interactions are mediated between the Mn^Ⅱ centers.     

Synthesis and Crystal Structure of N,N~′-Bis(p-nitrophenyl)-2,2~′-(p-phenylene-dioxy)diacetamide DMF Monohydrate

1 INTRODUCTION Many crown ethers have been synthesized[1, 2] and widely used[3～5]. The amide-type acyclic poly- ethers with versatile molecular structures offer many advantages over the traditional crown ethers, such as their potential activity for ion-selective electrodes[6] and the extraction of metal ions[7], so they have attracted much scientific attention[8～10]. In an effort to investigate the effect of skeleton of acyclic polyether on the extractability of metal ions, and to find …     

Synthesis and Crystal Structure of 2-(4-Nitrophenyl)-1,2-benzisoselenazol-3(2H)-one DMF (1:1) Solvate

The title compound (C13H8N2O3Se-C3H7NO) has been synthesized by a simple synthetic route and by recrystallization from DMF. The molecular structure of this compound was obtained by single-crystal X-ray diffraction. The compound crystallized in the triclinic space group P with a = 7.450(6), b = 8.150(7), c = 13.859(12) , α = 75.014(14), β = 83.072(18), γ = 84.409(14)°, V = 805.0(12)3, Z = 2 and R = 0.0271 for 2575 observed reflections with I > 2σ(I). X-ray analysis reveals that not only intermolecular Se…O and C-H…O interactions, but also π…π stacking interactions exist in the adjacent molecules. The above three kinds of intermolecular interactions extend the complex into an infinite three-dimensional layered network.     

Hydrothermal Synthesis, Structure and Thermal Properties of a Novel Three-dimensional La(Ⅲ)-Sebacate Framework

A novel lanthanide-organic framework compound [La(seb)(Hseb)(H2O)]n (H2seb = sebacic acid) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectra, TG and single-crystal X-ray diffraction. Complex 1 crystallizes in the triclinic system, space group P with a = 8.5849(7), b = 9.0641(8), c = 15.4049(13), α = 98.1830(10), β = 100.6870(10), γ= 97.5650(10)°, Z = 2, V = 1150.44(17) 3, Dc = 1.612 g/cm3, Mr = 558.39, λ(MoKα) = 0.71073 , μ = 1.903 mm-1, F(000) = 568, R = 0.0219 and wR = 0.0507 for 3797 observed reflections with I > 2σ(I). The structure contains edge-shared chains of [LaO8(H2O)] tricapped trigonal prisms that propagate along the b axis. In aliphatic ligand participation, complex 1 exhibits a three-dimensional supramolecular framework. Moreover, the thermal stability of complex 1 has been investigated.     

Synthesis, Crystal Structure and Properties of a Dinuclear Cobalt（II） Complex [Co2（a-furacrylato）4（Phen）2（H2O）]·C2H5OH

A dinuclear cobalt(Ⅱ) complex [Co2(α-furacrylato)4(Phen)2(H2O)]·C2H5OH has been synthesized with α-furacrylic acid and 1,10-phenanthroline as the ligands, and its crystal structure was determined. The crystal is of monoclinic system, space group C2/c with a=1.07388(8), b=2.4300(2), c=1.86708(14)nm, β=104.3830(10)o, V=4.719.4(7) nm3 , Dc=1.503 g/cm3 , Z=2, F(000)=2196, GOOF=1.053, the final R=0.0343 and wR=0.0883. The crystal structure shows that two neighboring cobalt(Ⅱ) ions are linked by the bridging coordination of two α-furacrylic acid anions and one water molecule, and their end positions are respectively coordinated with two 1,10-phenanthroline molecules and two α-furacrylic acid anions, forming a dinuclear structure. Both cobalt(Ⅱ) ions adopt hexa-coordinated distorted octahedral geometry. The electrochemical and fluorescence properties of the title complex are also discussed.     

Synthesis and Structure of Paramagnetic β-OctamolybdateComplex, [Fe(2,2''''bipy)_3]_2[Mo_8O_26]·6H_2O

1 INTRODUCTION The polyoxoanion-based inorganic and organo- metallic complexes, especially isopolymolybdates, have attracted considerable interest for their appli- cations in catalysis, sorption, clathration, magnetism and photochemistry[1]. Octamoly…     

Synthesis, Characterization and Crystal Structure of (2,2′-Bipyridine)(μ-maleato)copper(II) Dihydrate

ＩｎｔｒｏｄｕｃｔｉｏｎＩｎｔｈｅｐａｓｔｄｅｃａｄｅ ,ａｌｏｔｏｆｉｎｔｅｒｅｓｔｈａｓｂｅｅｎｃｏｎ ｃｅｎｔｒａｔｅｄｏｎｐｒｅｐａｒｉｎｇａｎｄｃｈａｒａｃｔｅｒｉｚｉｎｇｂｒｉｄｇｉｎｇｍｅｔａｌｃｏｍｐｌｅｘｅｓｆｏｒｉｎｖｅｓｔｉｇａｔｉｎｇｔｈｅｉｒｐｏｔｅｎｔｉａｌｌｙｕｓｅｆｕｌｅｌｅｃ ｔｒｏｎｉｃｏｒｍａｇｎｅｔｉｃｐｒｏｐｅｒｔｉｅｓ .1,2 Ｒｅｃｅｎｔｌｙ ,ｓｅｖｅｒａｌｍｅｔａｌｃｏｍｐｌｅｘｅｓｂｒｉｄｇｅｄｂｙｄｉｃａｒｂｏｘｙｌａｔｅｈａｖｅｂｅｅｎｓｙｎｔｈｅｓ…     

Crystal Structure and Binding Properties of a New Molecular Clip Based on Diethoxycarbonyl Glycoluril： C42H36N6O6

A new molecular clip based on diethoxycarbonyl glycoluril 5: C42H36N6O6 , has been synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group Pbca with a=12.7639(5), b=16.9727(7),c=34.2069(14) , V=7410.5(5)3 , Z=8, Dc=1.292 g/cm3 , μ(MoKα)=0.088 mm-1 , F(000)=3024, the final R=0.0655 and wR=0.1566 for 5123 observed reflections with I>2σ(I). The crystal structural analysis shows that intermolecular c-H…O and C-H…N hydrogen bonds stabilized the whole crystal structure. The binding study by fluorescence spectroscope titration showed that the title molecule can selectively recognize Fe3+ with fluorescence quenching.     

Synthesis and Crystal Structure of 8-Methyl-7-（3-nitrophenyl）-10-phenyl-10,11-dihydrochro-meno[4,3-b]pyrazolo[4,3-e]pyridin-6-（7H）-one

The title compound(C26H18N4O4) has been synthesized via a three-component reaction and it was characterized by means of IR and 1H NMR.Its crystal and molecular structures were determined by X-ray diffractometry.It belongs to the triclinic system,space group P1 with a = 7.7288(15),b = 11.168(2),c = 12.645(3) ,α = 107.02(3),β = 90.85(3),γ = 101.93(3)°,V = 1017.9(3) 3,Mr = 450.44,Z = 2,Dc = 1.470 g/cm3,λ = 1.54178 ,μ = 0.836 mm-1,F(000) = 468,the final R = 0.0488 and wR = 0.1180.A total of 11903 reflections were collected,of which 3642 were independent(Rint = 0.0377) and 3025 were observed with I > 2σ(I).     

Synthesis and Crystal Structure of N,N′-Bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]-propane-1,3-diamine

The title compound,N,N′-bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]-propane-1,3-diamine(C31H48Cl2N2O6,Mr = 615.61),has been synthesized and characterized by IR,1H NMR,MS,elemental analysis and single-crystal X-ray diffraction.The crystal crystallizes in the monoclinic system,space group C2 with a = 16.1091(4),b = 11.1880(3),c = 19.2854(5) ,β = 106.297(2)°,V = 3336.12(15) 3,Z = 4,Dc = 1.226 mg/m3,μ = 0.237 mm-1,F(000) = 1320,the final R = 0.0531 and wR = 0.0700 for 2760 observed reflections(I > 2σ(I)).X-ray analysis reveals that the title compound possesses four rings:two chiral five-membered furanone rings and two six-membered cyclohexane rings with chair conformation,containing eight chiral centers:C2(S),C3(R),C5(R),C10(S),C18(S),C21(R),C22(S) and C25(R).The structure is stabilized by N-H…O hydrogen bonding interaction.     

Synthesis and Crystal Structure of 2-（1-Naphthalenylamino）-4-thiazolidinone

The compound 2-(1-naphthalenylamino)-4-thiazolidinone was synthesized by the reaction of 1-(naphthalene-1-yl)thiourea with ethyl chloroacetate in an ionic liquid, and its structure was characterized by IR, 1H NMR and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group P21 /c with a=10.0081(3), b=14.5312(4), c=7.8739(2) , β=99.425(3)°, Z=4, V=1129.64(5)3 , Dc=1.425 g/cm3 , μ=0.269 mm-1 , F(000)=504, the final R=0.0519 and wR=0.1507. X-ray analysis indicated that the five-membered ring is essentially planar in this molecule, and intermolecular hydrogen bonds N(1)-H(1)…N(2), C(3)-H(3)…O(1), C(4)-H(4)…O(1) and C(12)-H(12a)…O(1) were observed. π-π Stacking interactions contribute to the stability of the structure. DSC-TG analysis showed that the title compound experienced a phase change at 190 ℃ and began to decompose above 240 ℃.     

Synthesis,Crystal Structure and Bioactivity of a Pd(Ⅱ) Complex with Demethylcantharate and 2,2′-Bipyridine

A novel crystal with the molecular formula [Pd(DCA)(bipy)]2 [Pd(bipy)Cl2 ]·6.75H2O was formed by PdCl2 with disodium demethylcantharate (Na2 (DCA),DCA2= 7-oxa-bicyclo[2.2.1]heptane-2,3-bicarboxylate) and 2,2-bipyidine (bipy) through the hydrothermal method.The complex was characterized by elemental analysis and infrared spectroscopy.The structure of the complex was determined by single-crystal X-ray diffraction,which is of triclinic system,space group P1 with a=13.6818(7),b=14.8426(8),c=15.0043(8),α=97.319(3),β=92.521(3),γ=105.776(2)°,V=2898.4(3) 3,Dc=1.545 g·cm-3,Z=1,F(000)=1420,S=0.852,the final R=0.0525 and wR=0.1777 for 13634 observer reflections (I>2σ(I)).The binding reaction of the complex with ct-DNA and bovine serum albumin (BSA) was studied by fluorescence spectroscopy.The results indicated that the complex binds to ct-DNA via the partial intercalation.The binding constant K A of the complex interaction with BSA was 3.98×10 5 L·mol-1 and one binding site would be formed.The antiproliferative activity of the complex against human hepatoma cells (SMMC7721) in vitro is much higher than that of Na 2 (DCA).     

Synthesis, Crystal Structure and Electrochemistry Properties of a (N,N'-Ethylene-bis(salicylaldiminato)) Nickel(Ⅱ) Complex, [Ni2(salen)2]·NCS-NH4

A new Ni(Ⅱ) complex [Ni2(salen)2]·(NCS)·NH4 (salen = N,N'-bis(salicylidenea-mino)ethanato) has been prepared and structurally characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pbca with a = 16.8725(13), b = 19.0046(15), c = 20.0583(16) (A), Z = 8, V = 6431.8(9) (A)3, C33H32N6Ni2O4S1, Mr= 726.13, Dc = 1.500 g/cm3, F(000) = 3008, μ = 1.284 mm-1, the final R = 0.0394 and wR = 0.0767 for 4449 observed reflections with Ⅰ＞2σ(Ⅰ). The complex involves a N,N'-ethylene-bis(salicylaldiminato) Schiff base, an isothiocyanato anion and an ammonium cation. The nickle(Ⅱ) ion adopts a distorted square coordination geometry with N2O2 set of Schiff base ligand. The complexes are linked into a dimmer via intermolecular hydrogen bonds and the [Ni(salen)] moieties are connected together to form a 2-D layer structure by intermolecular N-H…O hydrogen bonds and π-π stacking. Cyclic-voltammetry method was used to characterize electrochemically the complex.     

A Cadmium(II) Coordination Polymer: Crystal Structure and Fluorescent Property of [CdCl_2(4,4''''-bipyridine)]_ ∞

1 INTRODUCTION The metal-organic coordination polymers have proved to be promising in developing new mate- rials[1]. It is crucial to select or synthesize the suita- ble bridging organic ligand. Some simple rigid li- gands are skillfully employed[2～4].…