Synthesis and Crystal Structure of （E）-ethyl 6-benzyl-2-[（cyclopropylmethylamino）（4-fluorophenylamino）-methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate

The crystal structure of the new title compound (E)-ethyl 6-benzyl-2-[(cyclopropylmethylamino)(4-fluorophenylamino)methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate (C28H31FN 4O2S·C2H6O, Mr=552.70) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a=13.806(10), b=10.850(7), c=19.938(14), β=98.842(9)° , V=2951(4)3 , Z=4, Dc=1.244g/cm 3 , F(000)=1176, μ=0.153 mm-1 , MoKα radiation (λ=0.71073), R=0.0758 and wR=0.2234 for 4262 observed reflections with I > 2σ(I). Intramolecular N-H…S and C-H…N interactions as well as intermolecular N-H…O and O-H…N hydrogen bonds help to stabilize the crystal structure. X-ray diffraction analysis reveals that the asymmetric unit contains one title molecule and one ethanol molecule.     

A New 3D Supramolecular Network Formed by [Zn_3（2,6-Pyridinedicarboxylate）_3Cl_4]~（4-）and 4-Carboxypyridinium

A new compound [Zn3(C7NO4H3)3Cl4]·[C6NO2H6]4·4H2O (I) has been synthesized and structurally characterized by X-ray crystallography.It crystallizes in monoclinic,space group C2/c with a=16.9018(14),b=12.6902(10),c=25.1170(2),β=90.54°,V=5387.0(8)3,Z=4,Zn3C45H41Cl4N7O24,Mr=1401.76,Dc=1.728 g/cm3,F(000)=2840,μ(MoKa)=1.615 mm-1,the R= 0.0758 and wR=0.2060 for 3468 observed reflections (I 2σ(I)).Analysis of single-crystal X-ray diffraction data shows that compound I displays an interesting example of 3D supramolecular networks with perfect neutral and ionic hydrogen bonding array.     

Hydrothermal Synthesis,Crystal Structure and Properties of a Novel Polyoxometalate {[Cu~Ⅱ(1,10-phen)]_2[PMo~Ⅵ_(11)Mo~ⅤO_(40)]} [Cu~Ⅰ(C_8N_4H_6)(C_9H_6NO)(H_2O)]

A new pseudo three-dimensional framework structure of the title compound {[CuⅡ(1,10-phen)]2[PMoⅥ11MoⅤO40]}[CuⅠ(C8N4H6)(C9H6NO)(H2O)](1) has been prepared by the hydrothermal method for the first time and characterized by elemental analyses,X-ray single-crystal diffraction and IR spectra.1 consists of two building blocks,one {[CuⅡ(1,10-phen)]2[PMoⅥ11MoⅤO40]} and one [CuⅠ(C8N4H6)(C9H6NO)(H2O)] coordinated group.Singlecrystal X-ray diffraction revealed that 1 crystallizes in the monoclinic system,space group P2/c with a=13.498(4),b=12.890(3),c=21.465(8),β=97.314o,V=3704(2)3,Mr=2693.61,Z=2,Dc=2.415 Mg/m3,μ=2.915 mm-1,F(000)=2562,S=1.009,the final R=0.0583 and wR=0.1406 for 5129 observed reflections with I2σ(I).Furthermore,compound 1 shows strong fluorescent properties in the solid state at room temperature.The electrochemical behavior of 1 has also been studied by cyclic voltammograms.     

Synthesis and Crystal Structure of [{Mn(IBG)(2,2'-bipy)(H_2O)}·4H_2O]_n

A novel MnⅡ complex [{Mn(IBG)(2,2'-bipy)(H2O)}·4H2O]n 1(H2IBG=isophtha-loylbisglycine and 2,2'-bipy = 2,2'-bipyridine) has been synthesized and characterized by singlecrystal X-ray diffraction,elemental analysis,IR spectra and thermogravimetric analysis.It crystallizes in monoclinic,space group P21/n,with a=13.667(2),b=14.045(2),c=14.195(2),β=101.483(3)°,V=2670.1(7)3,Z=4,C22H26N4O11Mn,Mr=577.41,Dc=1.436 g/cm3,F(000)=1196.0,μ(MoKα)=0.558 mm-1,the final R=0.0578 and wR=0.1460 for 2974 observed reflections with I2σ(I).In the structure,the MnⅡ atom is coordinated in a distorted octahedral environment arranged by one water molecule,one 2,2'-bipy ligand and two IBG ligands.     

Synthesis and Crystal Structure of a New [Mn_2Ni_2] Cubane Complex

A new Mn2Ni2 cubane complex has been synthesized and characterized by single-crystal X-ray diffraction,FT IR spectra and elemental analysis.The title compound [MnIII2NiII2(hmp)4(N3)4(O2CR)2](hmp-is the anion of 2-pyridinemethanol and O2CR-is α-na-phthaleneacetate)crystallizes in the monoclinic system,space group P21/c with a = 10.519(5),b = 22.109(10),c = 23.235(9),β = 106.096(17)o,C48H42Mn2N16Ni2O8,Mr = 1198.28,V = 5192(4)3,Dc = 1.533 g/cm3,F(000)= 2448,μ = 1.258 cm1,Z = 4,the final R = 0.0875 and wR = 0.2020 for 3398 reflections with I > 2σ(I).X-ray diffraction analysis reveals that each Mn(III)center is octahedrally coordinated by two nitrogen atoms of azide anions and three oxygen atoms from three 2-pyridinemethanol anion ligands together with one oxygen atom from naphthaleneacetate.Each Ni(II)is octahedrally coordinated by two nitrogen atoms of 2-pyridinemethanol anion ligands as well as three oxygen atoms from three 2-pyridinemethanol anion ligands and one oxygen atom from naphthaleneacetate.     

X-ray Diffraction Investigation of Ethyl 2-（2-Amino-3-ethoxycarbonyl-4H-benzo[f]chromene-4-yl） Cyanoacetate

The title compound,ethyl 2-(2-amino-3-ethoxycarbonyl-4H-benzo[f]chromene-4-yl) cyanoacetate 4,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=12.9408(18),b=11.1870(13),c=13.8975(19),β=109.261(2)°,Z=4,C21H20N2O5,Mr=380.39,V=1899.3(4)3,Dc=1.330 g/cm3,μ=0.096 mm-1,F(000)=800,S=1.027,R=0.0535 and wR=0.1012 for 1365 observed reflections(I 2σ(I)).X-ray analysis reveals N-H…π interactions,π…π interactions and hydrogen bonds in the title molecule.     

Structure and Luminescence Property of a Hexanuclear Thiosemicarbazone Silver（I） Cluster

A new hexanuclear silver(I) compound containing thiosemicarbazones with groups of 1-naphthalene was synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analysis and fluorescence spectrum.The title compound crystallizes in monoclinic,space group P2 1 /c with a=16.101(4),b=24.855(7),c=14.492(4),β=109.730(5)°,V=5459(3)3,C 90 H 102 Ag 6 N 24 O 6 S 6,M r=2455.54,D c=1.494 g/cm 3,μ(MoKα)=1.228 mm-1,F(000)=2472,Z=2,the final R=0.0761 and wR=0.1507 for 5258 observed reflections (I > 2σ(I)).In the structure,the S atom of ligand L serves as a triply bridged chelator to connect the six silver atoms into a Ag 6 L 6 cluster.Luminescence investigation reveals that the compound exhibits two ligand-independent cluster-centered electron transfer bands and one ligand-dependent charge transfer band.     

Synthesis,Crystal Structure and Luminescent Property of a New Copper(Ⅰ) Iodide Complex Based on 3,5-Dimethyl-4-amino-triazole

The title compound,[Cu4I4(C4H8N4)4],has been synthesized and characterized by single-crystal X-ray diffraction analysis.It crystallizes in monoclinic,space group Pbca,with a=18.1851(10),b=9.3697(5),c=19.8034(10),V=3374.3(3)3,C16H32Cu4I4N16,Mr=1210.34,Z=4,Dc=2.383 g/cm3,μ=6.183 mm-1,F(000)=2272,S=1.032,the final R=0.0309 and wR=0.1180 for 3854 observer reflections(I2σ(I)).The structure of the title compound consists of tetranuclear copper cluster units bridged by the halogen atoms with the 3,5-dimethyl-4-aminotriazole ligands coordinated to the metal ions through the triazole nitrogen atoms.The luminescent property of 1 was also studied.     

Hydrothermal Synthesis and Crystal Structure of a Manganese(Ⅱ) Polymer with a Two-dimensional Network Structure:[Mn(pzdc)(phen)]_n·nH_2O

A metal-organic coordination compound formulated as [Mn(pzdc)(phen)]n·nH2O 1 (H2pzdc=pyrazine-2,3-dicarboxylic acid,phen=1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR,TG and single-crystal X-ray diffraction.The title compound crystallizes in the monoclinic system,space group P21/n with a= 11.7689(18),b=11.7458(18),c=13.360(2),β=110.341(2)o,V=1731.7(5)3,C18H12MnN4O5,Mr=419.26,Dc=1.608 g/cm3,μ(MoKα)=0.803 mm-1,F(000)=852,Z=4,the final R=0.0323 and wR=0.0823 for 2831 observed reflections (I 2σ(I)).It exhibits an interesting two-dimen-sional network structure.     

Synthesis and Crystal Structure of 2,3,4,6-Tetra-O-acetyl-1-{2-[(4-nitrophenoxy)methyl]-1,3,4-thiadiazole-5-thione-4-yl}-1-deoxy-β-D-glucopyranose

The title compound has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of orthorhombic system (C23H25N3O12S2,Mr=599.58),space group P212121 with a=6.2102(12),b=17.803(4),c=24.223(5),V=2678.0(9)3,Z=4,Dc=1.487 g/cm3,F(000)=1248,μ=0.268 mm-1,the final R=0.0483 and wR=0.1108 for 4174 observed reflections (I 2σ(I)).The C=S bond,which parallels to the anomeric C-H,adopts α orientation relative to the anomeric position of glucopyranoside.     

Synthesis and Crystal Structure of a New Supramolecular Compound Constructed from Flexible 1,1＇-（1,4-Butanediyl）bis（imidazole） and 1,2,4,5-Benzenetetracarboxylic Acid

A new bis(imidazolium) compound,[H2L(H2btec)2]·H4btec(1,L=1,1'-(butane-1,4-diyl)bis(imidazole),H4btec=1,2,4,5-benzenetetracarboxylatic acid),has been synthesized and structurally characterized by single-crystal X-ray diffraction.The title compound crystallizes in the monoclinic system,space group Pnma,with a=13.3908(11),b=13.9249(12),c=16.2166(14),V=2957.6(4)3,Z=4,Mr=698.55,Dc=1.569 mg/m3,F(000)=1448,μ(MoKα)=0.130 mm-1,the final R=0.0584 and wR=0.1538 for 4295 observed reflections with I2σ(I).The compound consists of one 1,1'-(butane-1,4-diyl)bis(imidazolium) cation,one neutral H4btec and one H2btec2-(Only two para carboxyl groups are deprotonated,and two protonated ones remain free) anion.A one-dimensional hydrogen bonding chain and a 2D hydrogen bonding network are formed via intermolecular N-H…O and O-H…O hydrogen bonds.These adjacent chains are further stacked through intermolecular π-π and hydrogen bonding interactions to form a 3D supramolecular network.     

Synthesis, Crystal Structure Analysis and DFT Calculation of 1-Benzoyl-3,6-diphenyl-1,4-dihydro-1,2,4,5-tetrazine

The new title compound, 1-benzoyl-3,6-diphenyl-1,4-dihydro-1,2,4,5-tetrazine (C21H16N4O, Mr = 340.38), has been prepared and its crystal structure can not be confirmed by the results of MS, elemental analysis, IR spectrum and 1H NMR spectrum, but determined by X-ray diffraction. The title compound crystallizes in an orthorhombic space group P212121 with a = 7.1100(19), b = 12.115(3), c = 19.884(6), V = 1712.7(8)3, Z = 4, Dc = 1.320 g/cm3, F(000) = 712, μ = 0.085 mm-1, MoKa radiation (λ = 0.71073), R = 0.0334 and wR = 0.0845 for 2254 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the central tetrazine adopts an unsymmetrical boat conformation. According to the bond lengths of tetrazine ring, the molecule should be 1,4-dihydro-1,2,4,5-tetrazine, rather than 1,2-dihydro-1,2,4,5-tetrazine. The crystal structure is stabilized mainly by intermolecular N–H···O hydrogen bonds.     

Synthesis,Crystal Structure and Properties of a Novel Nickel Citrate Ni（H_2cit）（phen）（H_2O）·3H_2O（H_4cit = Citrate Acid,phen=1,10-Phenanthroline）

A new nickel citrate compound Ni(H2cit)(phen)(H2O).3H2O(H4cit = citrate acid,phen = 1,10-phenanthroline) has been synthesized and characterized by single-crystal X-ray diffraction.It crystallizes in the trigonal system,space group P31 with a = 13.8319(13),c = 10.425(2),V = 1727.3(4)3,Dc = 1.445 g/cm3,Mr = 501.09,F(000) = 780,μ = 0.901 mm-1,Z = 3,R = 0.0760 and wR = 0.1730 for 3859 observed reflections(I > 2σ(I)).In this compound,Ni2+ cation is chelated by a phen molecule,one H2cit2-anion and one H2O molecule.The citric acid coordinates to the Ni2+ center through three functional groups:α-hydroxyl,α-carboxylate and β-carboxylate while another α-carboxylate forms hydrogen bond with surrounding H2O molecule.And the citric acid is doubly protonated.The temperature-dependent magnetic susceptibility data revealed that the compound is a paramagnetic material.     

Synthesis and Crystal Structure of 2,3,4,6-tetra-O-Acetyl-1-{4-chloro-3-[1-（4-ethoxyphenyl）-1-methylethyl]phenyl}-1-deoxy-β-D-glucopyranose

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic system(C31H37ClO10,Mr = 605.06),space group P21 with a = 11.882(5),b = 10.106(5),c = 13.816(6),V = 1545.9(12)3,Z = 2,Dc = 1.300 g/cm3,F(000) = 640,μ = 0.179 mm-1,the final R = 0.0430 and wR = 0.0595 for 4960 observed reflections(I > 2σ(I)).The title compound was confirmed to be a β-anomer by single-crystal X-ray diffraction and 1H NMR.The proximal benzene ring is nearly orthogonal to the glucopyranoside ring,and the two benzene rings are also almost orthogonal to each other.Four non-classical intermolecular hydrogen bonds observed in the crystal lattice help to stabilize the crystal.     

Synthesis,Crystal Structure and Antitumor Activity of N-（4-tert-butyl-5-（4-chlorobenzyl）thiazol-2-yl）-2,6-difluorobenzamide

The title compound was synthesized by the reaction of 4-tert-butyl-5-(4-chlorobenzyl)-2-aminothiazole with 2,6-difluorobenzoic acid. The crystal structure of the title compound, C21H19ClF2N2OS, was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pbca with a = 12.6479(13), b = 13.1204(13), c = 14.1341(15), Z = 4, V = 2011.5(4)3, Mr = 420.89, Dc = 1.390 g/cm3, S = 1.023, μ = 0.326 mm-1, F(000) = 872, the final R = 0.0365 and wR = 0.0880 for 6101 observed reflections(I 2σ(I)), and R = 0.0507, wR = 0.0978 for 7779 independent reflections. X-ray crystal structure displays that the hydrogen bonding interactions observed link the molecules to form a dimeric unit. The preliminary biological test of the title compound shows good antitumor activity, with IC50 of 0.046 μmol/mL against the Hela cell line.     

Facile Synthesis and Crystal Structure of a Novel Cyanopyridine

The title compound 2-amino-4-(4-hydroxy-3,5-dimethoxyphenyl)-5-methyl-6-phenyl nicotinonitrile,C 21 H 19 N 3 O 3,was synthesized via four-component reactions between propio-phenone,malononitrile,syringaldehyde and ammonium acetate in ethanol under reflux without catalyst and characterized by IR,1 H NMR,13 C NMR,MS,EA and single-crystal X-ray diffraction.Single-crystal X-ray diffraction analysis shows that the compound is of monoclinic system,space group P2 1 /n with a=8.4600(17),b=17.139(3),c=13.408(3),β=107.06(3)°,V=1858.6(6)3,Z=4,M r=361.39,F(000)=760,μ(MoKα)=0.088 mm-1,D c=1.292 g/cm 3,λ=0.71073,the final R=0.0751 and wR=0.0938 for 3333 observed reflections with I > 2σ(I).The crystal packing of the title compound is stabilized by intermolecular hydrogen bonds.     

Synthesis,Crystal Structure and Biological Activity of 8-（（4-（（2,3-diaminopyridin-4-yl）oxy）-3-fluorophenyl）-amino）-2-（4-fluorophenyl）-3-methyl-2,7-naphthyridin-1（2H）-one

The new title compound 8-((4-((2,3-diaminopyridin-4-yl)-oxy)-3-fluorophenyl)-amino)-2-(4-fluorophenyl)-3-methyl-2,7-naphthyridin-1(2H)-one(C26H20F2N6O2, Mr = 486.48) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 15.365(3), b = 13.144(2), c = 11.863(2), β= 108.882(3)°, Z = 4, V = 2267.0(7)3, Dc = 1.425 g/cm3, F(000) = 1008, μ = 0.105 mm-1, MoKa radiation(λ = 0.71073), R = 0.0480 and wR = 0.1294 for 3197 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the region C(substituents of 8-amino group and 3-methyl group on the 2,7-naphthyridin-1(2H)-one ring) of compound 6 are effectively planar. Intramolecular and intermolecular hydrogen bonds together with π···π interations are found in the structure. In addition, compound 6 shows potent c-Met and c-Kit kinase inhibition activities.     

A New One-dimensional Chain-like Ag（I） Complex with Schiff Base Ligand Containing 4-Amino-1,2,4-triazole

The title compound,poly[N-[1-(3-pydidyl)ethylidene]-4H-1,2,4-triazol-4-amine sil-ver(I) tetrafluoroborate],[Ag(C9H9N5)(BF4)]n,is the result of complexing Ag cation with N-[1-(3-pydidyl)ethylidene]-4H-1,2,4-triazol-4-amine (L),and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group C2/c with a= 18.899(6),b=9.882(2),c=15.472(4),β=120.158(3)°,V=2498.5(11)3,C9H9AgBF4N5,Mr= 381.89,Dc=2.031 g/cm3,μ(MoKα)=1.659 mm-1,F(000)=1488,Z=8,the final R=0.0441 and wR=0.0619 for 1094 observed reflections (I 2σ(I)).In the structure,ligand L bridges the two metal Ag(I) centers in a bidentate fashion and each metal ion coordinates with two nitrogen atoms,forming a one-dimensional rectangular chain.The neighboring chains are connected by two additional Ag-N weak interactions into a 3D framework structure.The title compound shows blue fluorescence property at room temperature.     

Hydrothermal Synthesis and Crystal Structure of a 2D Zinc（Ⅱ） Coordination Polymer with 5-Hydroxynicotinic Acid

The title compound,[Zn(5-hydroxynicotinate) 2 2H 2 O] n,has been synthesized by reacting zinc sulfate vitriol with 5-hydroxynicotinic acid under hydrothermal conditions,and its structure was determined by X-ray crystallography with the following data:monoclinic,space group C2/c,C 12 H 12 N 2 O 8 Zn,M r=377.61,a=10.223(3),b=10.319(3),c=13.613(4),β=105.922(6)°,Z=4,V=1380.9(8)3,F(000)=768,D c=1.816 g/cm 3,μ(MoKα)=1.826 mm-1,the final R=0.0401 and wR=0.1380 for 1157 observed reflections (I > 2σ(I)).In the structure of the title compound,the Zn II ion located in an inversion center lies in a distorted tetrahedral environment at a N 2 O 2 coordination mode,and the 5-hydroxynicotinic acid ligand links symmetry-related Zn II ions at a μ 2-N,O bridging way forming a two-dimensional covalent structure.In the crystal,solvent water molecules form intermolecular O-H O hydrogen bonds and pyridine rings of adjacent layers form π-π stacking (3.346),which connect adjacent two-dimensional sheets into a three-dimensional supramolecular network.     

Synthesis and Crystal Structur of (4,4′-H_2bipy)[CdBr_4]·H_2O

The title compound (4,4′-H2bipy)[CdBr4]·H2O 1 has been synthesized via hydrothermal reaction and characterized by X-ray diffraction. The crystal belongs to monoclinic,space group P21/c with a=8.260(3),b=23.926(7),c=9.774(2),β=106.777(9)o,C10H12Br4CdN2O,Mr=608.26,V=1849.4(9)3,Z=4,Dc=2.185 g/cm3,S=1.005,μ(MoKα) =9.814 mm–1,F(000)=1128,R=0.0646 and wR=0.0989. The crystal structure analysis of 1 reveals that the title compound features an isolated structure,based on discrete 4,4′-H2bipy moieties and lattice water molecules which are linked by hydrogen bonds together with tetra-hedral cadmium atoms terminally coordinated by four bromine atoms.