Synthesis,Characterization, and Crystal Structure of One Novel Indolo[3,2-b]carbazole Derivative

Indolocarbazole derivatives have been reported to be promising organic semicon- ductor candidates and electroluminescent （EL） materials. One novel indolocarbazole derivative, 2,8-acetyl-5,11-dihexyl-6,12-（di-p-tolyl）-5,11-indolo[3,2-b]carbazole （YK4）, has been synthesized, and its crystal structure has also been carefully studied. YK4 is triclinic, space groups Pi with a = 9.409（5）, b = 13.974（5）, c = 15.488（5） A, α = 90.281（5）, β = 105.456（5）, Z= 93.728（5）°, M,. = 688.94, V= 1958.1（14） A3, Z = 2, Dc.= 1.168 g/cm-3,μ = 0.070 mm-1, F（000） = 740, Rint = 0.0475, R （I〉 20（/）） = 0.1146, wR （I〉 20（/）） = 0.2186, R（all data） = 0.2192 and wR （all data） = 0.2701. Like other indolo[3, 2-b]carbazole derivatives which were introduced in the 5- and 11-positions, the intermolecular short contacts are localized between the pendant groups and acetyl groups of the neighboring indolocarbazole molecules. The molecule of YK4 possesses poor face-to-face π-π stacking between two adjacent molecules in the crystal. The calculated bond lengths and bond angles of YK4 also proved the result of crystallography.     

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

A new 4,5-diaryl-lH-imidazole was synthesized and characterized by 1H NMR, ESI-MS, elemental analysis and FT-IR. The crystal structure of the title compound （C19H16C12N202, Mr = 375.24） has been determined by single-crystal X-ray diffraction. Crystal parameters： mono- clinic system, space group P2/n, a = 14.349（3）, b = 8.7918（18）, c = 15.352（3） A, β = 108.56（3）°, V = 1836.1（6） A3, Z = 4, F（000） = 776, Dc = 1.357 g/cm3, p = 0.368 mm-1, the final R = 0.0502 and wR = 0.1066 for 2324 observed reflections with 1 〉 2 σ（/）. 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.     

Indexing Non-merohedrally Twinned Crystals by Bruker＇sAPEX2 and Agilent＇s CrysAlis~（PRO）, an Example of a Crystal Structure That Can Be Refined through Either the PLATONRoute or the ＇HKLF 5＇ Route,and, Simultaneous Data Collection of Two Crystals in a Two-in-one Run

The first part of this report describes the data reduction of non-merohedrally twinned crystals measured on Bruker and Agilent area-detector diffractometers. The image frames of methyl-2-aminopyrazine-3-carboxylate were processed with APEX2 to furnish a set of overlapping diffraction indices that were used for solution and refinement. CrysAlisPRO was used for processing the frames of bis（diethyldicarbamato）nickel, which exists in monoclinic and tetragonal polymorphs, and in untwinned and twinned forms. In the second part, the crystal structure of [（3-formyl-4- hydroxyphenyl）methyl]triphenylphosphanium chloride was refined through the ‘HKLF 5＇（based on a combined set of diffraction indices） and PLATON（based on one set of diffraction indices） routes to give identical outcomes because the amount of overlap of the twin domains is small. For the third part, in a proof-of-concept investigation, the diffraction pattern of untwinned and twinned 4-{（E）-（4-aminophenyl）diazenyl]phenylamine was recorded simultaneously in one run; the three domains could be indexed and the crystal structure satisfactorily refined. The refinement was identical to those derived from independent measurements; the crystal structure features two independent centrosymmetric molecules, one of which is ordered and the other whole-molecule-disordered. This two-in-one run opens up the possibility that two or more crystals having different atomic compositions can be measured simultaneously if their reciprocal lattices do not overlap significantly.     

Synthesis,Crystal Structure and Photoluminescent Property of a New Ca(Ⅱ) Compound Constructed from 5-Oxyacetateisophthalic Acid

A new coordination polymer, namely [Ca(HOABDC)]n(1, H3 OABDC = 5-oxyacetateisophthalic acid), has been synthesized through hydrothermal reactions of Ca(NO3)2 and H3 OABDC. The title compound crystallizes in monoclinic, space group P21/c with a = 4.3043(2), b = 21.4959(11), c = 10.7450(6) A, β = 91.411(5)o, V = 993.88(9)A3, C10H6O7 Ca, Mr = 278.23, Z = 4, Dc = 1.859 g/cm3, F(000) = 560, μ = 0.659 mm-1, the final R = 0.0328 and wR = 0.0670 for 1469 observed reflections(I 2A(I)). Single-crystal X-ray structural analysis reveals that compound 1 features 1D Ca(Ⅱ)-carboxylate chain-shaped subunits, which are further connected together via HOABDC2- ligands into a 3D(6,6)-connected nia-type hybrid framework. Moreover, the luminescent property and thermal stability of 1 were also investigated.     

A New Cadmium（II） Coordination Polymer Constructed by 2-（2-Chloro-6-fluorophenyl）-lH-imidazo[4,5-f] [1, 10]phenanthroline and 1,2,3-Benzenecarboxylate： Synthesis,Structure and Luminescence

A new Cd（II） coordination polymer, namely, [Cd3（1,2,3-BTC）2（L）2]·2.25H2O （1, L = 2-（2-chloro-6-fluorophenyl）-1H-imidazo[4,5-A][1,10]phenanthroline and 1,2,3-BTC = 1,2,3-ben- zenetricarboxylate）, has been synthesized under hydrothermal conditions. The compound was characterized by single-crystal X-ray diffraction. It crystallizes in triclinic, space group Pī with α = 11.650（2）, b = 12.240（2）, c = 19.760（4） A, α = 72.01（3）, β = 77.11（3）, γ = 83.48（3）°, V = 2609.4（9） A3, Z = 2, C56H31Cd3Cl2F2N8O14.25, Mr = 1489.99, Dc = 1.896 g/cm3, F（000） = 1466, μ（MoKa） = 1.401 mm^-1, R = 0.0401 and wR = 0.1104. Compound 1 shows a 1D chain structure, and the neigh- boring 1D chains of 1 are joined together by π···π interactions to result in a 2D supramolecular layer. In addition, the luminescent property of 1 has been studied in the solid state at room temperature.     

A New Two-dimensional Coordination Polymer Based on Trinuclear Manganese Clusters

A novel two-dimensional Mn（II） coordination polymer, [Mn3（L）R（cis-chdc）fftrans- chdc）]n （L = 2-amino-4-（1H-imidazo[4,5-J][1,10]phenanthrolin-2-yl）phenol and chdc = 1,4-cyclo- hexanedicarboxylate）, has been hydrothermally synthesized and characterized by elemental analysis, IR, TG PL and single-crystal X-ray diffraction. Crystallographic data for this compound： monoclinic space group P2/n with a = 11.0058（13）, b = 9.0179（11）, c = 28.431（3） A, β = 92.850（2）°, V = 2818.3（6） A3, Z = 2, C62Hs6Mn3N10O14, Mr = 1329.99, Dc = 1.567 g/cm3, F（000） = 1370, p（MoKa） = 0.742 mm-1, R = 0.0553 and wR = 0.1421. The chdc carboxylates bridge the Mn（II） atoms to form a trinuclear Mn（lI） cluster. The cis-chdc ligands are held together by the trinuclear Mn（II） clusters to result in a chain structure. Further, the trans-chdc ligands link adjacent chains to furnish a two-dimensional network. The π-π interactions between neighboring layers link the adjacent layers into a three-dimensional supramolecular architecture. Moreover, the N-H...O and O-H...O hydrogen bonds further stabilize the 3D supramolecular architecture.     

Synthesis,Crystal Structure and Antiproliferative Activity of Ethyl 1-（Phenylcarbamoyl）-2-3,4,5-trimethoxyphenyl）cyclopropanecarboxylae

Many small-molecule compounds have been evaluated with potential antiproliferative activities. Ethyl 1-(phenylcarbamoyl)-2-(3,4,5-trimethoxyphenyl)cyclopropanecarboxylate, one novel cyclopropylamide analogue of combretastatin-A4(CA-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 = 15.0263(3), b = 7.6574(2), c = 19.4117(4), β = 111.9010(10)o, V = 2072.36(8)3, Z = 4, C22H24NO6, Mr = 398.42, Dc = 1.277 Mg/cm3, F(000) = 844, λ(MoKα) = 1.54178 , μ = 0.770 mm–1, R = 0.0546 and wR = 0.1889 for 3319 observed reflections(I 2σ(I)). Meanwhile, the compound revealed potential antiproliferative activities in several cancer cells in vitro.     

Synthesis and Characterization of a Two-dimensional Cadmium(Ⅱ) Metal Organic Framework with Fes Topology

A new Cd(Ⅱ) coordination polymer, {[Cd(Hnbta)(L)]·H2O}n(L = 1,4-bis(5,6-dimethylbenzimidazol-1-yl)butane), H3nbta= 5-nitrobenzene-1,2,3-tricarboxylic acid), has been hydro-thermally synthesized and characterized by elemental analyses, IR, XRPD, and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a = 17.3056(13), b = 11.0114(9), c = 17.7484(14) A, β = 117.3640(10)o, V = 3003.7(4) A3, Z = 4, C31H31CdN5O9, Mr = 730.01, Dc = 1.614 g/cm3, μ = 0.792 mm-1 and F(000) = 1488. The cadmium(Ⅱ) ions are bridged by Hnbta2- to generate a two-dimensional metal organic framework with fes topology. In addition, the thermal stability and fluorescence properties of the complex were also studied.     

Synthesis,Crystal Structure and Properties of a Novel Coordination Polymer Based on a Trinuclear Mn（II） Cluster： [Mna（bpta）2（bip）2]n

The coordination polymer, [Mn3（bpta）2（bip）2], （H3bpta = biphenyl-3,3＇,5-tricar- boxylic acid, bip = 2,6-bis（imidazole-1-yl）pyridine）, has been synthesized under hydrothermal con- ditions and characterized by elemental analysis, FT-IR, XRD, TGA and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a = 14.919（3）, b = 9.780（2）, c = 20.352（7） A, V = 2344.4（10） A3, Z= 2, C52H32Mn3N10012, Mr = 1153.70, Dc = 1.634 g/cm3, p（MoKa） = 0.876 mm-1, F（000） = 1170, the finalR = 0.0605 and wR = 0.1177. The complex forms a 2D layer with trinuclear Mn（II） units and further assembles into a 3D supramolecular network structure through C-H..＇O hydrogen bonding and C-H...π interactions. Moreover, the negative J value indicates the presence of antiferromagnetic coupling between the Mn（II） ions within a trinuclear unit.     

Syntheses,Structures, and Properties of Three Coordiantion Polymers： [Cd2（bpp）1.5（Hbpp）（phen）2]n, [Mn3（Htptc）2（phen）2（H2O）2]n,and {[Cu（btc）0.5（1,4-bib）]？2H2O}nSyntheses,Structures, and Properties of Three Coordiantion Polymers： [Cd2（bpp）1.5（Hbpp）（phen）2]n, [Mn3（Htptc）2（phen）2（H2O）2]n,and {[Cu（btc）0.5（1,4-bib）]？2H2O}n

Hydrothermal reactions of three aromatic polycarboxylic acids and the transitional metal cations in the presence of phen and 1,4-bib afford three new coordination polymers： [Cd2（bpp）1.5（Hbpp）（phen）2]n （1）, [Mn3（Htptc）2（phen）2（H2O）2]n （2）, and {[Cu（btc）0.5（1,4- bib）]·2H2O}n（3） （H2bpp = 2,6-bis（4＇-carboxyphenyl）-4-phenylpyridine, H4tptc = terphenyl-2,5,2＇,5＇-tetracar- boxylic acid, H4btc =biphenyl-2,2＇,4,4＇-tetracarboxylic acid, phen =1,10-phenanthroline, and 1,4-bib = 1,4-bis（1H-imidazol-1-yl）benzene）. Their structures have been determined by single- crystal X-ray diffraction analyses, elemental analyses, IR spectra, and powder X-ray diffraction （PXRD） analyses. In compound 1, the CdII cations are linked by bpp2- to form one ladder structure, based on which a 3D network is constructed with the help of non-covalent interactions. The topology of 2 is a 3D （3,4,5）-connected framework with the Point Schl？fli symbol of （42.6）2（43.62.8）（45.64.8）2. Compound 3 shows an unprecedented 3D （4,4）-connected framework with the Point Schl？fli symbol of （64.82）2（65.8）. Moreover, the luminescent property of 1 has been investigated.     

Synthesis,Crystal Structure and Fungicidal Activity of N-（4-tert-buty）-5-（1,2,4-triazol- 1-yl）thiazol-2-yl）propionamide

The title compound has been synthesized by the reaction of 4-tert-butyl-5-(1,2,4-triazol-1-yl)-2-aminothiazole with propionic anhydride, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system, space group Pbca with a = 18.441(2), b = 8.3284(9), c = 19.257(2) , Z = 8, V = 2957.5(5) 3, Mr = 279.37, Dc = 1.255 mg/m3, S = 1.033, μ = 0.219 mm-1, F(000) = 1184, the final R = 0.0349 and wR = 0.0876 for 2629 observed reflections(I 2σ(I)). X-ray crystal structure presents the intermolecular N–H···N hydrogen bond, which plays an important role in stabilizing the crystal structure. The preliminary bioassay indicates that the title compound exhibits potent fungicidal activity against R. Solani(25 mg/L) with inhibition rate of 80.0%.     

Solvothermal Synthesis of a 3D Luminescent Cadmium-organic Framework with msw Topological Net

A new cadmium-organic framework, [Cd2（TBDC）2（DMF）2（H2O）]n （1）, was synthesized by solvothermal reaction of rigid carboxylate ligand 2,3,5,6-tetramethyl-l,4-ben- zenedicarboxylate （H2TBDC） and cadmium nitrate and characterized by elemental analysis, infrared spectrum, thermal analysis, PXRD, single-crystal X-ray diffraction and photoluminescence in the solid state. Compound 1 crystallizes in orthorhombic, space group Pca21 with a = 21.487（6）, b = 7.790（2）, c = 20.666（6） A, C30H40Cd2N2O11, Mr = 829.44, V= 3459.3（16） A3, Z = 4, Dc = 1.593 g.cm-3,μ = 1.29 mm-1, F（000） = 1672, 2.7〈θ〈27.2°, λ（MoKa） = 0.71073 A, T= 293（2） K, the final R = 0.026, wR = 0.0548 and S = 1.027. X-ray diffraction analysis reveals that complex 1 possesses a 3D framework and exhibits rnsw net. Thus, the solid-state luminescent spectrum of 1 displays that the emission of cadmium（lI） complex shows a peak at 317 nm upon 250 nm excitation at room temperature.     

Synthesis,Crystal Structure and Cytotoxic Activity of a New N-Vinyl-1H-dibenzo[a,c]carbazole Derivative of the Dehydroabietic Acid

The title compound （C29H33NO2, 3） was synthesized and structurally characterized by elemental analysis, IR, MS, 1H- and 13C-NMR and single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21 with a = 14.428（3）, b = 7.3440（15）, c = 22.768（5） A, β = 95.17（3）°, V = 2402.7（8） A3, Z = 4, Mr = 427.56, Dc = 1.182 g/cm3, F （000） = 920, 2（MoKa） = 0.71073 A,μ = 0.073 mm-1, the final R= 0.0670 and wR= 0.1002 for 2437 reflections with I〉 2σ（I） Two crystallographically independent molecules with different conformations co-exist in the structure. The crystal structure is stabilized by intermolecular C-H…π interactions which make the molecules stack along the b axis. In addition, the preliminary cytotoxic assay showed that the title compound exhibited moderate inhibitory activity against KB and SW1116 cells.     

Syntheses and Crystal Structures of Two Nickel（Ⅱ） Complexes [Ni（dmpzm）2（L）]Cl·nH2O（L = HCO2, OAc; n = 2, 3; dmpzm = 1,1＇-Methylenebis（3,5-dimethyl-1H-pyrazole））

Reactions of NiCl2-6H2O with dmpzm and formic or acetic acid at PH = 7 produced the two title compounds, [Ni（dmpzm）2（HCO2）]Cl·2H2O 1 and [Ni（dmpzm）2（OAc）]C2·H2O 2 （dmpzm = 1,1 ＇-methylenebis（3,5-dimethyl-lH-pyrazole））. 1 and 2 were characterized by elemental analysis, IR spectra, and thermogravimetric analysis. 1 crystallizes in the orthorhombic system, space group Pcca with a = 18.700（2）, b = 8.6843（9）, c = 18.098（2）A, V= 2939.1（5）A^3, Z = 4, Dc = 1.319 g/cm^3, T = 193 K, C23H37CINsNiO4, Mr = 583.75, F（000） = 1232, p（MoKa） = 0.792 cm^-1, S = 1.079, R = 0.0772 and wR = 0.1958 for 2265 observed reflections with I〉 2σ（I）. 2 crystallizes in the orthorhombic system, space group Pcca with a = 17.011（3）, b = 18.630（4）, c = 19.300（4）A, V = 6117（2）A^3, Z = 8, Dc = 1.337 g/cm^3, T= 193（2） K, C24H41C1N8NiO5, Mr = 615.79, F（000） = 2608, μ（MoKa） = 0.768 cm^-1, S = 1.059, R = 0.0518 and wR = 0.1109 for 5124 observed reflections with I 〉 2σ（I）. The Ni atoms in 1 or 2 are chelated by two dmpzm ligands and one formate or acetate anion, forming slightly distorted octahedral geometries. In the crystals of 1 or 2, intermolecular hydrogen bonding interactions result in the formation of 2D hydrogen-bonded frameworks.     

A 3D Ba(Ⅱ) Inorganic-organic Hybrid Framework Based on 1,3,5-Benzenetricarboxylic Acid Ligand: Synthesis and Characterization

A three-dimensional(3D) barium complex with 1,3,5-benzenetricarboxylic acid(H3BTC), {[Ba1.5(BTC)(H2O)]·(H2O)}n(1), was synthesized in DMF/EtOH/H2 O mixed solution under solvothermal conditions, and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectra, thermogravimetric analyses, and photoluminescence measurement. In complex 1, the 2D I2O0 type inorganic layer is constructed by {Ba1O10} and {Ba2O9} polyhedra. Moreover, the solid-state fluorescence measurement reveals a fluorescence emission band at 465 nm under 344 nm excitation, assigned to a charge-transfer transition.     

Synthesis and Crystal Structure Analysis of 5＇-O-Tosyl-2,3＇-anhydrothymidine

In this paper, 5＇-O-tosyl-2,3＇-anhydrothymidine has been synthesized and its crystal structure was analyzed. The crystal belongs to the triclinic system, space group P1, with a = 5.397（2）, b = 6.1886（18）, c = 3.507（5）A, α = 87.74（2）,β = 89.84（4）,γ = 73.79（2）°, C17H18N2O6S, Mr = 378,39, Z = 1, V = 432.8（3）A^3, Dc = 1.452 g/cm^3, F（000） = 198 and Flack = -0.11（14）. No intermolecular hydrogen bonds exist in the crystal, and the angle between benzene ring and pyrimidine planes is 32.23°.     

Two New Cu(Ⅱ) Coordination Polymers Based on 2,5-Furandicarboxylic Acid and 2,2'-bipyridine:Synthesis and Crystal Structure

Two new Cu(Ⅱ) coordination polymers,[Cu(FDA)(BPY)(H2O)]n(1) and {[Cu(FDA)(BPY)(H2O)]·2H2O}n(2)(H2FDA = 2,5-furandicarboxylic acid,BPY = 2,2-bipyridine),have been synthesized and structurally characterized by single-crystal X-ray diffraction as well as elemental analysis and IR.Compound 1 crystallizes in monoclinic,space group P21/c,with a = 7.5915(15),b = 8.4050(17),c = 24.204(6) ,β = 99.05(3)°,V = 1525.1(6) 3,Dc = 1.706 g/cm3,C16H12CuN2O6,Mr = 391.82,F(000) = 796,μ(MoKα) = 1.470 mm–1,Z = 4,R = 0.0633 and wR = 0.1059 for 2389 observed reflections(I 2σ(I)),R = 0.0738,and wR = 0.1098 for all data.Complex 2 belongs to triclinic space group P1 with a = 8.8660(18),b = 8.9112(18),c = 12.525(3) ,α = 88.41(3),β = 69.38(3),γ = 66.95(3)°,V = 845.2(3) 3,Dc = 1.681 g/cm3,C16H16CuN2O8,Mr = 427.85,F(000) = 438,μ(MoKα) = 1.342 mm–1,Z = 2,R = 0.0290 and wR = 0.0690 for 2767 observed reflections(I 2σ(I)),R = 0.0329 and wR = 0.0706 for all data.Complexes 1 and 2 are both coordination polymers with one-dimensional chain structures bridged by the protonated FDA ligands,which are assembled into three-dimensional supramolecular structures through hydrogen bonding interactions and π-π packing interactions between the chains.     

A Chain Structure Based on Homodinuclear Scandium Units： [Sc（μ-OH）（2,5-pydc）（H2O）]n

The reaction of pyridine-2,5-dicarboxylic acid with Sc2O3 under hydrothermal con- dition yields a new complex [Sc（μ-OH）（2,5-pydc）（H2O）]n 1 which has a chain structure based on homodinuclear scandium units. Crystal data for 1： space group P^-1, a = 6.7192（13）, b = 7.6131（13）, c = 8.9313（14） A, α = 95.976（6）, β = 101.663（6）, γ = 108.151（5）^o, V= 418.26（13） A^3, Z = 2, Dc = 1.946 g/cm^3, g = 0.889 mm^-1, F（000） = 248, C7H6NO6Sc, Mr = 245.09, the final R = 0.0429 and wR = 0.1086.     

Syntheses,Structures, and Luminescent Properties of Two Zn~Ⅱ-organic Polymers Based on [Zn(ox)]_n Chains and Different Imidazole Linkers

Hydrothermal reactions of two imidazole derivatives(1,3,5-tib = 1,3,5-tris(1Himidazol-1-yl)benzene, 1,4-bimb = 1,4-bis(1H-imidazol-1-ylmethyl)benzene) and the ZnⅡ cations in the presence of oxalic acid(H2ox) afford two coordination polymers, namely, {[Zn(ox)(1,3,5-tib)]·2(H2O)}n(1) and [Zn1.5(ox)1.5(1,4-bimb)1.5]n(2). Their structures have been determined by single-crystal X-ray diffraction analyses, elemental analyses, IR spectra, and powder X-ray diffraction(PXRD) analyses. Both complexes 1 and 2 are based on the 1D zigzag [Zn(ox)]n chains, and their final structures are controlled by the two different imidazole linkers, which expanded the structure along different directions, finally giving a 3D dia net for 1 and a 2D sql layer for 2. Moreover, the luminescent properties of 1 and 2 have been investigated.     

Synthesis,Crystal Structure and Antitumor Activities of Ethyl 5-methyl-4-morpholino- 2-（3-Methyl-phenylamino）-furo [2,3-d] pyrimidine-6-carboxylate

The title compound （C21H24N4O4, Mr = 396.44） has been synthesized by the func- tionalized ethyl 4-chloro-6-methyl-2-arylamino-furo[2,3-d]pyrimidine-5-carboxylates and mor- pholine. Its structure was confirmed by means of 1H NMR IR, MS and elemental analysis. The crystal structure of the title compound was determined by X-ray single-crystal diffraction. The compound crystallizes in triclinic system, space group P1, a = 7.9919（8）, b = 9.9312（1）, c = 12.9380（13） A, aα = 86.987（2）, β = 83.604（2）, γ = 89.641（2）°, V = 1019.08（18） A3, Z = 2, F（000） = 420, Dc = 1.292 g/cm3,μ = 0.091 mm-1, R = 0.0602 and wR = 0.1548 for 3943 independent （Rint = 0.0639） and 3414 observed （I 〉 2σ（I）） reflections, lntermolecular N-H…O and π-π stacking interactions contributed to the stability of the structure. The preliminary biological test indicated the title compound exhibited cytotoxicity against human lung cancer cell lines.