Synthesis and Crystal Structure of （5-Hydroxy-6-methoxybenzofuran- 3-yl）-（4-methoxyphenyl）methanone

Compound 1 (5-hydroxy-6-methoxybenzofuran-3-yl)(4-methoxyphenyl)methanone, C17H14O5 , as a potential anti-breast cancer agent has been synthesized under microwave irradiation, which was further converted to (5,6-dihydroxybenzofuran-3-yl)(4-methoxyphenyl)methanone (2). The compounds were characterized by MS and NMR spectra. Meanwhile, the crystal of 1 was obtained and determined by X-ray single-crystal diffraction. Crystal data: monoclinic system, space group P21/n, a=8.908(6), b=10.505(7), c=15.452(11), β=105.043(9)°, V=1396.4(16)3 , Z=4, F(000)=624, Dc=1.419 g/cm3 , μ=0.105 mm1, R=0.0513 and wR=0.1246 for 14459 independent reflections (Rint=0.0647) and 2488 observed ones (I>2σ(I)). Intermolecular O-H···O and π-π stacking interactions contributed to the stability of the structure.     

Synthesis and Crystal Structure of a Novel Organic Adduct Nonlinear Optical Material: 3,5-Dinitrobenzonic Acid·ethanolamine (3,5-DNBEA)

1 INTRODUCTION The development of highly efficient nonlinear opti- cal (NLO) crystals for visible and ultraviolet (UV) regions is extremely important for both laser spe- ctroscopy and laser processing. In recent years, many new non-linear optical second harmonic gene- ration (SHG) materials of organic adduct have come out with the following main advantages over the inorganic ones. The main merits of organic materials compared with inorganic ones for such second-har- monic generation d…     

Synthesis,Crystal Structure and Properties of a Novel Decavanadate Complex with One-dimensional Chain Involving Sodium and ＇Bis-tris＇ Ligand

By using a flexible multidentate ligand,bis(2-hydroxyethyl)iminotris(hydroxyhydroxylmethy)methane('bis-tris':H5L),the title complex {[Na(H6L)2]2}n·nV10O28(1) has been successfully synthesized under self-assembly condition and characterized by IR spectroscopy,elemental analysis,PXRD and single-crystal X-ray diffraction.The crystal structure belongs to an orthorhombic system,space group Cmca with a = 23.752(2),b = 13.5360(8),c = 18.5377(11) ,V = 5960.1(7),Z = 8,Dc = 2.055 g/cm3,F(000) = 3744,μ = 1.630 mm-1,the final R = 0.0283 and wR = 0.0759 for 3353 observed reflections with I > 2σ(I).This complex consists of decavanadate [V10O28]6-motifs as counter anions intercalated with one-dimensiond chains of the composition [Na(H6L)2]n3n+.And significant intermolecular O-H…O hydrogen-bonding interactions lead to a three-dimensional supramolecular framework.     

Synthesis,Crystal Structure and Theoretical Calculations of a New Two-dimensional Co(Ⅱ) Coordination Polymer Based on Oxalic Acid and Bis(imidazol) Ligands

A new Co(Ⅱ) coordination polymer has been successfully synthesized under hydrothermal conditions [Co(C2O4)(mbix)]n(1, H2C2O4 = oxalic acid, mbix = 1,3-bis(imidazol-1-ylmethyl)benzene). Its structure has been determined by elemental analyses, IR, UV spectroscopy and single-crystal X-ray diffraction analysis. Pink crystals crystallize in the triclinic system, space group P1 with a = 8.8666(7), b = 9.5859(8), c = 10.8537(9) , α = 67.6810(10), β = 66.1260(10), γ = 77.1300(10)°, V = 777.77(11), C16H14CoN4O4, Mr = 385.24, Dc = 1.645 g/cm3, F(000) = 394, Z = 2, μ(Mo Kα) = 1.134 mm-1, the final R = 0.0482 and w R = 0.1231 for 2968 observed reflections(Ⅰ 2σ(Ⅰ)). It shows a two-dimensional(2D) network structure. The intermolecular C–H···O hydrogen bonding and π-π stacking interactions extend complex 1 into a 3D supramolecular architecture andplay an important role in stabilizing 1. In addition, Natural Bond Orbital(NBO) analysis was performed by using the PBE0/LANL2 DZ method built in Gaussian 09 Program. The calculation results showed obvious covalent interaction between the coordinated atoms and Co(Ⅱ) ion.     

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.     

Synthesis and Crystal Structure of 3,3＇-（4-Dimethylaminobenzylidene）- bis-（4-hydroxycoumarin）

The title compound 3,3'-(4-dimethylaminobenzylidene)-bis-(4-hydroxycoumarin) 3 was synthesized by the reaction of 4-hydroxycoumarin with 4-dimethylaminobenzaldehyde, and its chemical structure was determined by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P21/n with a = 11.698(2), b = 10.882(2), c = 16.594(3) , β = 90.69(3)o, V = 2112.1(7) 3, Z = 4, F(000) = 952, Dc = 1.432 Mg/m3, Mr = 455.45, μ = 0.102 mm-1, λ = 0.71073 , the final R = 0.0779 and wR = 0.2143 for 3031 observed reflections with I > 2σ(I).     

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 and Crystal Structure of a New Nickel（II） Complex with 3,4-Pyridinedicarboxylic Acid and 1,4-Bis（imidazol-l-ylmethyl）-benzene Ligands

A metal-organic coordination polymer [Ni(PDB)(bix)(H2O)]n(H2PDB=3,4-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 triclinic system, space group P1 with a=9.1849(8), b=9.2065(9), c=12.9308(12) , α=103.3070(10), β=104.7160(10), γ=90.5900(10)o, V=1026.42(16)3 , C21H19N5NiO5 , Mr=480.12, Dc=1.553 g/cm3 , F(000)=496, Z=2, μ(MoKα)=0.991 mm1 , the final R=0.0325 and wR=0.0799 for 3561 observed reflections (I>2 (I)). The structure of 1 exhibits a two-dimensional network structure.     

Synthesis,Crystal Structure and Properties of a Nanotubular Metal-organic Framework（MOFs） Based on Cu（Ⅱ） Oxide Chains and Benzenedicarboxylates

A new cooper benzenedicarboxylate metal-organic coordination polymer,[Cu(μH2O)(BDC)]n·nDMF(1,H2BDC = 1,4-benzenedicarboxylate acid,DMF = N,N'-dimethylfor-mamide),has been successfully synthesized under hydrothermal conditions and characterized by IR spectroscopy,elemental analysis,thermogravimetric analysis and single-crystal X-ray diffraction.This complex crystallizes in triclinic,space group P1 with a = 6.605,b = 10.44780(10),c = 11.0881(6) ,α = 62.064(11),β = 73.410(15),γ = 78.404(16)°,C11H13CuNO6,Mr = 318.76,V = 645.79(8) 3,Z = 2,Dc = 1.639 g/cm3,F(000) = 326,μ = 1.712 mm-1,the final R = 0.0362 and wR = 0.1330 for 2055 observed reflections with I > 2σ(I).The title compound contains infinite inorganic chains constructed by Cu oxygen octahedra by sharing corners and edges.Each chain is connected by BDC linkers to four other chains to form a three-dimensional framework with irregular rhombic channels where the DMF molecules are encapsulated.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Cadmium（Ⅱ） Complex

A metal-organic coordination polymer [Cd2(cbba)4(bix)2] n·nH2O (Hcbba=2-(4′-chlorine-benzoyl)-benzoic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Colorless crystals crystallize in the triclinic system, space group Pī with a=12.9891(15), b=15.3211(19), c=21.154(3), α=108.476(3), β=90.148(2), γ=105.429(3)°, V=3831.5(8)3 , C84H60Cd2Cl4N8O13 , Mr=1756.00, Dc=1.522g/cm3 , F(000)=1776, Z=2, μ(MoKα)=0.765 mm-1 , the final R=0.0724 and wR=0.1208 for 6916 observed reflections (I > 2σ(I)). The structure of 1 exhibits a one-dimensional infinite chain-like structure.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Cobalt（Ⅱ） Complex

A metal-organic coordination polymer [Co2(cbba)4(bix)2]n(Hcbba = 2-(4'-chlorine-benzoyl)-benzoic 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.Pink crystals crystallize in the monoclinic system,space group P21/n with a = 21.148(4),b = 15.728(3),c = 23.879(4) ,β = 102.148(3)°,V = 7764(2)3,C316H232Cl15Co8N32O48,Mr = 6248.53,Dc = 1.336 g/cm3,F(000) = 3207,Z = 1,μ(MoKα) = 0.621 mm-1,the final R = 0.0567 and wR = 0.1280 for 8510 observed reflections(I > 2σ(I)).The structure of 1 exhibits a one-dimensional chain-like structure.     

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.     

Synthesis and Crystal Structure of 1,2-Dis（1,3-diphenylpropan-2-yl）disulfane

A novel compound of 1,2-dis(1,3-diphenylpropan-2-yl)disulfane(C30H30S2,Mr=454.27)was synthesized in ethanol with 1,3-diphenyl-2-propanone as raw materials,giving high yield of product(90%).Its structure was determined by IR,1H NMR,MS,elemental analysis and X-ray diffraction.The crystal belongs to monoclinic,space group C2 with a=18.727(3),b=6.5179(9),c=13.7576(18),β=131.0610(10)o,V=1266.2(3)3,Z=2,Dc=2.136 g/cm3,μ=1.078 mm-1,F(000)=843,R=0.0490 and wR=0.1247 for 3211 observed reflections with I>2(I).X-ray analysis reveals that the molecule is not symmetrical.There exist no classical hydrogen bonds andπ-πstacking interactions.Moreover,the thermal stability of compound 3 was investigated.     

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.     

Synthesis, Crystal Structure and Electrochemical Property of 5,10,15,20-Tetrakis（4-chlorophenyl）porphyrin

The title compound 5,10,15,20-tetrakis(4-chlorophenyl)porphyrin was synthesized and structurally characterized by X-ray single-crystal diffraction method. Crystal data: triclinic, space group P, Z=1, C50H32Cl4N4, Mr=830.60, a=6.4316(13), b=11.322(2), c=13.833(3) , α =91.44(3), β=91.06(2), γ=92.67(3)°, V=1005.7(3)3 , Dc=1.371 g/cm3 , μ(MoKα)=0.34 mm-1 , F(000)=428, R=0.0563 and wR=0.0867 for 2712 observed reflections with I > 2σ(I). X-ray analysis reveals the phenyl rings and the pyrrole rings are not in the same plane. The dihedral angles between adjacent phenyl rings and pyrrole rings are 66.1 and 66.8°, respectively.     

Micro-vial Synthesis,Structure,Magnetic Properties and Hirshfeld Surface Analysis of a Penta-nuclear Fe(Ⅲ) Cluster

A new penta-nuclear Fe^Ⅲ cluster,[HN(C2H5)3]·[Fe5(timb)4(ATZ)4(μ3-O)2]·(H2O)5(1),(H2timb is 4-bromo-2-[(1H-tetrazol-5-ylimino)-methyl]-phenol;HATZ is 5-amino-1,2,3,4-tetrazole),was synthesized through micro-vial synthesis methods,which was characterized by elemental analysis,FT-IR spectra,X-ray single-crystal diffraction,thermogravimetric analysis.The single crystal belongs to the tetragonal system,space group √42d with a=0.19735(1),b=0.19735(1),c=0.26118(2)nm,Mr=1904.04,V=10.1724(10)nm^3,Z=4,Dc=1.118 g/cm^3,F(000)=3356,μ=2.314 mm^–1,R=0.0500 and wR=0.1151.The magnetic properties and Hirshfeld surface analysis of 1 were investigated and discussed in detail.     

Synthesis,Structure and Luminescent Property of a 2D Cd(Ⅱ) Coordination Polymer Based on Mixed-ligands of 1,3-Bis(imidazol)propane and Pyridine-3,5-dicarboxylic Acid

A new Cd(Ⅱ) coordination polymer, namely, [Cd(1,3-bip)(3,5-pdc)]n(1,3-bip =1,3-bis(imidazol)propane and 3,5-pdc = pyridine-3,5-dicarboxylic acid) has been synthesized under hydrothermal conditions. Compound 1 was characterized by infrared spectrum, elemental analysis,powder X-ray diffraction(PXRD) and single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 1.40178(7), b = 1.72502(12), c = 1.41635(6) nm, β =92.653(4)o, V = 3.4212(3) nm3, Z = 4, C316H15 Cd N5O4, Mr = 453.73, Dc = 1.762 g/cm, F(000) =1808, μ = 1.310 mm-1, R = 0.0899 and w R = 0.1945. In compound 1, each 3,5-pdc ligand links three Cd(Ⅱ) ions and each Cd(Ⅱ) attaches to bip ligands to form a complicated 2D double-layer structure. In addition, the thermal stability and luminescent property of 1 have been studied in the solid state at room temperature.     

Synthesis and Crystal Structure of a New Copper(II) Complex with 4-Cyanobenzoic Acid

1 INTRODUCTION Exploration on the syntheses and properties of car- boxylate complexes, especially aromatic carboxylate complexes, has always been a fascinating and chal- lenging research field for decades either in coor- dination chemistry or in functional materials[1, 2]. Cy- anobenzoic acid (Hcba) possessing two functional coordination groups should display structural diver- sities on the formation of complexes[3～15]. In particu- lar, the copper(II) carboxylate complexes bearing spe- …     

Synthesis and Crystal Structure of a Cobalt（Ⅱ） Coordination Polymer with Benzene-1,3,5-triacetate and 1,4-Di（1H-imidazol-1-yl）benzene

A novel coordination polymer, [Co3 (bta)2(dib)2]·4H2O (1, H3bta=benzene-1,3,5-triacetic acid, and dib=1,4-di(1H-imidazol-1-yl)benzene), has been hydrothermally prepared and characterized by IR spectroscopy, elemental analysis and single-crystal X-ray diffraction. The crystal is of triclinic system, space group Pī, with a=9.141(2), b=9.667(2), c=13.855(2), α=100.83(3), β=90.81(3), γ=100.94(3)°, V=1179.0(4)3 , C48H46N8O16Co3 , Mr=1167.72, Dc=1.645 g/cm 3 , F(000)=599, μ=1.127 mm-1 and Z=1. The final R=0.0634 and wR=0.1703 for 4291 observed reflections (I > 2σ(I)). In the title complex, the bta ligand acts as a four-dentate bridging ligand to link up cobalt atoms into a lamellar framework, which are further interlinked by the dib ligands to generate a binodal (3,8)-connected tfz-d net.