Synthesis, Crystal Structure and DNA Binding Studies of α,α'-Bis(3,5-bismethyl-1-pyrozolyl)- carbene-acetyl-isopropenyl Hydrazine

The title compound α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopro-penyl hydrazine (C16H22N6O, Mr = 314.40) has been prepared. It was characterized by elemental analysis as well as IR, MS, 1H-NMR and 13C-NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction, getting the following data: triclinic, space group P1 with a = 6.9734(16), b = 10.773(3), c = 12.001(3) A, α = 75.311(4), β = 82.695(4), γ = 77.143(4)°, Z = 2, V = 847.9(3) A3, Dc : 1.231 g/cm3, F(000) = 336 and μ(MoKα) = 0.082 mm-1 (λ = 0.71073 A). The results of crystal structure determination show that there exist intermolecular and intramolecular hydrogen bonds, resulting in a two-dimensional supramolecular framework of the title compound. The binding of the title compound to DNA was investigated by absorption, emission, and viscosity measurements. The title compound shows absorption hyperchromicity accompanied by a blue shift at about 254 nm. The binding constant Kb for the title compound has been determined to be 1.89 × 104 M-1 from absorption measurements. The addition of the title compound to DNA pretreated with EB causes appreciable reduction in the emission intensity, indicating that the DNA-bound EB fluorophore is partially replaced by the title compound. The value of K is 3.093 × 104 M-1. The relative viscosity of DNA decreased with the addition of the title compound. Results suggest that the title compound binds to DNA with a non-classical intercalative or groove interaction mode. The observed efficient nuclease activity of the title compound is interesting and may have further influences on the chemistry of DNA minor groove binders.     

Crystal Structure and Antitumor Activity of Tri[2-[N-（4′-methyl-benzylsulfonyl）amino]ethyl]-amine

The crystal structure of the title compound (C27H38N4O7S3, Mr = 626.79) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pīwith a = 9.411(1), b = 11.645(2), c = 14.672(2) (A。), α = 91.80(1), β = 95.36(1), γ =104.56(1)o, V = 1547.0 (A。)3, Z = 2, Dc = 1.346 g/cm3, λ = 0.71073 (A。), μ(MoKα) = 0.289 mm－1 and F(000) = 664. The structure was refined to R = 0.0406 and wR = 0.1177 for 4103 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the title compound is a practically distorted tetrahedron and each molecule contains one lattice H2O by hydrogen bond. The antitumor activity of the title compound against HL-60 human leukemia cells has also been studied by MTT method.     

Synthesis,Crystal Structure and DNA Binding Studies of α,α'-Bis(3,5-bismethyl-1-pyrozolyl)-carbene-acetyl-isopropenyl Hydrazine

The title compound α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopro- penyl hydrazine (C16H22N6O, Mr = 314.40) has been prepared. It was characterized by elemental analysis as well as IR, MS, 1H-NMR and 13C-NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction, getting the following data: triclinic, space group P1 with a = 6.9734(16), b = 10.773(3), c = 12.001(3) , α = 75.311(4), β = 82.695(4), γ = 77.143(4)o, Z = 2, V = 847.9(3) 3, Dc = 1.231 g/cm3, F(000) = 336 and μ(MoKα) = 0.082 mm-1 (λ = 0.71073 ). The results of crystal structure determination show that there exist intermolecular and intramolecular hydrogen bonds, resulting in a two-dimensional supramolecular framework of the title compound. The binding of the title compound to DNA was investigated by absorption, emission, and viscosity measurements. The title compound shows absorption hyperchromicity accompanied by a blue shift at about 254 nm. The binding constant Kb for the title compound has been determined to be 1.89 × 104 M-1 from absorption measurements. The addition of the title compound to DNA pretreated with EB causes appreciable reduction in the emission intensity, indicating that the DNA-bound EB fluorophore is partially replaced by the title compound. The value of K is 3.093 × 104 M-1. The relative viscosity of DNA decreased with the addition of the title compound. Results suggest that the title compound binds to DNA with a non-classical intercalative or groove interaction mode. The observed efficient nuclease activity of the title compound is interesting and may have further influences on the chemistry of DNA minor groove binders. Keywords: α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopropenyl, preparation, crystal structure, DNA binding     

SYNTHESIS AND CRYSTAL STRUCTURE OF MgCl_2(CH_3COOC_2H_5)_2

The crystal of the title compound was prepared and its structure determined by X-ray diffraction method.1672 independent reflections were collected. The crystal is orthogonal with space group P2_12_12, and a=7.353(3),b=25.111(10), c=8.631(2), Z=8. The structure was solved by using Patterson method and modified with LSM program.The final R= 0.0795. The structural features of the title compound are:Mg(Ⅱ) is octahedral and ethyl acetate is located on trans-position.Mg atoms are connected by double chloro-bridge and form polychains.     

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 silver(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 singlecrystal 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) (A), β = 120.158(3)°, V = 2498.5(11) (A)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.     

Crystal and Molecular Structure of 4-Hydroxy-3-Methoxy-4-N-Methylstilbazonium Iodide C15H16NO2+·I-

The crystal structure of the title compound C15H16NO2+ · I-(Mr=369. 19) has been determined by single crystal X-ray diffraction analysis. The crystal belongs to tbe monoclinic system with space group P21/c, a=8. 957(1), b=21. 8117(2), c=7. 8760(10)A , β=103.94(1)°, V=1493.8(3)A3, Z=4, Dc=1. 642g cm3,μ=2. 141mm-1, F(000)=728, final R=0. 0264, and Rw=0. 0644(I＞2σ(I)) for 2938 independent reflections. The results show that in the crystal structure of the title compound the planar cations have two configurations, and these cations are anti-parallelly packed through the strong π…π interaction.     

Synthesis and Crystal Structure of [(PPh3)(CH3COS)2NiB10H10]·0.4(C5H12)

The title compound [(PPh3)(CH3COS)2NiB10H10]·0.4(C5H12) has been synthesized by the reaction of [NiCl2(PPh3)2], closo-[B10H10]2- and CH3COSH in CH2Cl2 solution. It was recrystallized from n-pentane/CH2Cl2 solution and its structure was determined by X-ray diffraction analysis. The crystal is triclinic, space group P1, Mr=618.23, with a=10.049(1), b=12.638(2), c=14.077(2) , α=110.13(1), β=87.65(1), γ=96.01(1)°, V=1669.3(4)(A)3, Dc=1.230 g/cm3, Z=2, λ(MoKα)=0.71073(A), μ=7.76 cm-1, F(000)=642. The final refinement is converged with R=0.042 (5986 observed reflections with I≥2σ(I)), wR2 =0.151. The cluster is a nido eleven-vertex {NiB10} cage with the Ni atom in the open NiB4 face. Cyclizations resulting in two five-membered rings, Ni(7)-S(1)-C(1)-O(1)-B(2) and Ni(7)-S(2)-C(2)-O(2)-B(3), have occurred.     

Synthesis, Structure and Geometrical Calculation of a Novel Co-crystal of {[4-Bromo-2-(benzimidazol-2-yl)phenolato][2- (1-butylbenzimidazol-2-yl)phenolato]zinc(Ⅱ)] and Bis[μ-2- (1- butylbenzimidazol-2-yl)phenolato]- 1κN3: 2κO; 1κO:2κN3-bis{[2-(1-butylbenzimidazol-2-yl)phenolato-κ2N3,O]zinc(Ⅱ)}

The title compound has been synthesized and characterized crystallographically. It is a co-crystal consisting of two different neutral zinc(Ⅱ) complexes with Hbpbm (Hbpbm = 4-bromo-2-(benzimidazol-2-yl)phenol) and Hnpbm (Hnpbm = 2-(1-butylbenzimidazol-2-yl)phenol).One is a monomeric mixed-ligand complex of [Zn(bpbm)(npbm)] 1 and the other a dimer of[Zn2(npbm)4] 2 with their ratio of 2:1. Thus the overall formula for the title compound is 21·2.Adjacent 1 and 2 are connected to each other by intermolecular hydrogen bonding interactions in the lattice. The crystal data: monoclinic, space group P21/c, a= 15.0141(12), b = 20.9941(17), c =18.4686(15) (A), β = 97.445(2)°, V= 5772.4(8) (A)3, Mr= 2429.68, Z = 2, Dc = 1.398 g/cm3,μ = 1.579mm-1, F(000) = 2504, R = 0.0637 and wR = 0.1771 for 6464 observed reflections (I＞ 2σ(Ⅰ)). The geometrical structure for 1 has also been theoretically optimized and compared with the experimental one.     

Synthesis and Structure Characterization of a Manganese(Ⅱ) Complex With Eight Coordination Geometry: [Mn(O_2CMe)_2(phen)_2]

The title compound [Mn(O2CMe)2(phen)2] (phen = 1,10-phenanthroline) 1 has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal is of orthor- hombic, space group Pbcn, with a = 12.554(4), b = 10.168(3), c = 17.704(5) , V = 2259.7(12) 3, Z = 4, C28H22MnN4O4, Mr = 533.44, Dc = 1.568 g/cm3, F(000) = 1100, Rint = 0.0242, T = 293(2) K and μ = 0.631 mm–1. The final R = 0.0687 and wR = 0.1960 for 2046 observed reflections with I > 2σ(I). The structure of the complex consists of one Mn(II) core coordinated by two bidentate-bound CH3COO- groups and two η2-phen groups forming an eight-coordinate geometrical configuration.     

CRYSTAL AND MOLECULAR STRUCTURE OF BENZO-15-CROWN-5 POTASSIUM TETRACHLOROAURATE K(C_(14)H_(20)O_5)_2-AuCl_4

<正> The crystal and molecular structure of the title compound K(C14 H20O5)2AuCl4 has been determined by X-ray diffraction method.The crystallographic data are as follows;Mr=914.51,triclinic,space group P1,a=10.988(2),b=13.472(4),c=13.696(2)A,α=77.72(1),β=79.02(2),γ=64.92(2)°,V=1782.6(4)A3,Z=2,Dc=1.704 g.cm-3,μ=45.858 cm-1,F(000)=454,R=0.019,Rw=0.018 for 5697 observed reflections with I≥3σ(I).X-ray structure determination shows that benzo-15-crown-5(B15C5)forms a 2:1 complex with KAu-C14 in which K+is sandwiched between two crown rings.The dihedral angle between these two ether oxygen planes is 11.9°.The anion AuCl4-has a planar square configuration which is bound with the complex cation K(B15C5)2+by electrostatic force to form an ion-pair.     

A novel one-dimensional organic-inorganic polymer: synthesis and crystal structure of[{Ca(DMF)_5}_2SiMo_(12)O_(40)]_n

A novel polyoxometalate-based organic-inorganic polymer [{Ca(DMF)5}2SiMo12O40]n has been synthesized and characterized by elemental analysis, IR, UV and X-ray single-crystal structural analysis. The title compound crystallizes in a monocline lattice, P21/n, with a =1.3379(3), b = 1.9796(4), c = 1.4574(3) nm, β = 92.24(3)°, V = 3.8568(13) nm3, Z = 2, R1 = 0.083 and Rw = 0.2065. The result of crystal structure analysis indicates that Ca2+ is surrounded by seven coordination oxygen atoms with pentagonal bipyramidal geometry and bridged with terminal oxygen atom of polyanion in the structure. The compound contains an unprecedented one-dimensional linear chain built by alternate polyanions and cationic units through Mo-Od-Ca-O-Ca links in crystal. The IR spectra and X-ray crystallography analysis exhibit that there is a strong interaction between the polyanion and organic group in solid state. The electronic spectra (λ = 200-500 nm) for the title compound dissolved in the mixed solvent of acetonitrile and     

CRYSTAL STRUCTURE OF CYCLOOCTADIENYL POTASSIUM TE- TRAHYDROFURANATE ,C_8H_(11)K(OC_4H_8)_2

<正> The title compound, cyclooctadienyl potassium tetrahydrofuranate was prepared by the reaction of cycloocta-1,5-diene with metallic potassium in tetrahydrof u-ran(THF) in the presence of triethylamine. Its crystal structure was determined by a low temperature X-ray diffraction analysis method. The crystal is monoclinic with space group Pc,a=6. 192(3),b=9. 444(8),c=14. 543(1) A ,β=94. 92(5)°,V = 847. 24 A3,Z = 2,DC= 1. 14 g/cm3 and μ(MoKa) = 5. 58cm-1. The structure was solved by heavy-atom methods and refined by least-squares to a final R value of 0. 049. The potassium cations, each with two complex THF molecules attached,are linked by bridging cyclooctadienyl an-ions,while the anions are connected to the bridging cations to form a puckered chain.     

Synthesis, Crystal Structure and Luminescent Property of a Novel 1-D Cadmium(II) Complex: [Cd_2(C_8H_3NO_6)_2(H_2O)_4]_n·2nH_2O

A novel one-dimensional chain-like coordination polymer constructed from 3-nitro- benzene-1,2-dicarboxylic acid, [Cd2(C8H3NO6)2(H2O)4]n·2nH2O, has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to monoclinic, space group P21/c with a = 6.1252(8), b = 20.706(3), c = 8.8067(11) , β = 95.608(2)°, V = 1111.6(2) 3, Mr = 751.12, Dc = 2.244 g/cm3, F(000) = 736, μ = 2.011 mm-1, Z = 2, the final R = 0.0262 and wR = 0.0692 for 2338 observed reflections with I > 2σ(I). The structure of the title compound presents a 1-D chain-like structure constructed by dimer units, [Cd2(C8H3NO6)2(H2O)4]n, through two carboxylate oxygen atoms. The fluorescence of the title compound has been also discussed in this paper.     

Synthesis, Structure and Properties of (n-Bu_4N)_3[Mo_6O_18NNAr(NO_2)_2]

The title compound was synthesized and characterized by means of elemental analysis, IR, DTA-TG and UV. Its single crystal structure was solved by using direct methods. The compound crystallizes in the orthorhombic space group Pmc(?) with lattice parameters: a = 1. 7261(2), b=l. 7537(3), c=2. 4258(3) nm. V=7. 34220 nm3, F(000) = 3648, Z = 4. The structure was refined to conventional discrepancy factors of R=0. 060 for 3176 observed reflections [Ⅰ>3σ/(Ⅰ)]. The anion represents a modification of the well-known [Mo6O19]2- anion, in which a single terminal oxo group is replaced by a 2,4-dinitrophenyl hydrazine ligand while the structure integrity of the hexanuclear framework is maintained.     

Synthesis,Crystal Structure and Antitumor Activity of a New Indolequinone Derivative of Ursolic Acid

The title compound(C_(37)H_(48)BrNO_5, 6) was synthesized from ursolic acid and its crystal structure was determined by single-crystal X-ray diffraction analysis. The compound is of orthorhombic system, space group P2_12_12_1 with a = 16.846(3), b = 18.844(4), c = 11.262(2) ?, Z =4, V = 3575.1(13) ?~3, M_r = 666.67, D_c = 1.239 Mg/m~3, S = 1.002, μ = 1.190 mm~(-1), F(000) = 1408,the final R = 0.0831 and wR = 0.1459 for 2286 observed reflections(I 2σ(I)). The crystal structure is stabilized by two intermolecular hydrogen bonds(N–H(0A)···O(2) and O(1)–H(1A)···O(3)). In the preliminary antitumor assay, the title compound 6 exhibits potent cytotoxic activity against Hep G2 and SMMC-7721 cells with IC50 values of 1.64 ± 0.21 and 1.22 ± 0.13 μM, respectively.     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF A NOVEL MOLYBDENUM-COPPER-SULFUR CLUSTER COMPOUND [(CH_3CH_2 )_4N]_2 [(μs-S)CusS_6(S_2)_6Mo_6O_6].DMF

The synthesis and crystal structure of a novel molybdenum-copper cluster compound with [(μs-S)Cus] core is reported. It was prepared from Cu2Br2 upon reaction with molybdenum sulfur compound [CH3CH2)4N]2[Mo2O2S2-(S2)(S4)]. The title compound crystallizes in the monoclinic system space group Cc with cell dimensions: a=21.320(5), b=21.869(3), c=13.029(5)A,β=118.28(1)°,Z=4, V=5349A3 and Dc=2.48 g.m-3. The structure has been determined by Patterson and Fourier methods and then refined by the least squares method to a final R of 0.053. There are some distortions from octahedron in configuration of the [(μs-S)Cu6]6 core with three weak Cu-Cu bonds.     

Synthesis and Crystal Structure of Monochloridehepta (dimethyl sulfoxide)gadolinium (Ⅲ) di(tetraphenyl boron) Salt [Gd(dmso) 7Cl][BPh4]2

The crystal of the title compound (C62H82B2ClGdO7S7 Mr= 1378.02)is triclinic with space group P-1. a=12. 532(2), b=12. 774(2), c=24. 580(5)A; α=93.389(9), β=104. 640(8), γ=112. 923(9)°, V=3451.4(8)A3, Z=2, Dc=1.326g/cm3. μ(MoKα)=1. 258mm-1, F(000)=1426. R=0.036 , Rw= 0. 091for 12101 reflections with I＞2σ(I). The crystal is composed of a discrete cation [Gd(dm-so )7Cl]+ and two anions [BPh4]-. The Gd( Ⅲ ) ion is coordinated by a chlorine and seven oxygen atoms from seven monodenate dimethylsulfoxides formimg a distorted square antiprism coordination polyhedron.     

Synthesis and Structure Characterization of a Tetranuclear Manganese(Ⅲ) Complex:[Mn_4O_2(O_2CMe)_6(MeOH)_2(dbm)_2]·2MeCOOH·2CH_2Cl_2

The title compound, [Mn4O2(O2CMe)6(MeOH)2(dbm)2]·2MeCOOH·2CH2Cl2 (Hdbm = dibenzoylmethane), has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1, with a = 10.729(3), b = 12.269(3), c = 13.085(4) , α = 106.367(3), β = 107.643(2), γ = 94.771(2)o, V = 1547.9(7) 3, Z = 1, C50H64Cl4Mn4O24, Mr = 1410.57, Dc = 1.513 g/cm3, F(000) = 724, Rint = 0.0147, T = 293(2) K and μ = 1.046 mm–1. The final R = 0.0359 and wR = 0.0938 for 5791 observed reflections with I > 2σ(I). The structure of the complex consists of one [Mn4(μ3-O)2]8+ core with four coplanar Mn atoms disposed in an extended “butterfly-like” arrangement and two O atoms triply bridging each “wing”, and the peripheral ligation is provided by six μ2-MeCO2– , two terminal μ2-dbm– groups at the two ends of the molecule, and two MeOH molecules on the central Mn atoms. Intermolecular O…H–O hydrogen bonding interactions are found within the structure of the compound.     

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.     

CRYSTAL AND MOLECULAR STRUCTURE OF MOLYBDENUM COM-PLEX MoO_2Cl_2(C_4H_3OCOOH)_2

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction method. The complex crystallizes in the mono-clinic space group P21/n with a = 10. 306 ( 3) , b = 10. 161 (2), c = 14. 798 ( 4) A . β= 108. 52(2)°, V= 1469. 4(6)A3,Z= 4. The structure was solved by direct methods. Least-squares refinement converged to a final value of R = 0. 043 and Rw= 0. 040 for 1237 reflections. The molybdenum (Ⅵ) ion is bonded to two chlorine atoms, two oxo atoms and two oxygen atoms from two monodentately and weakly coordinated carboxyl groups of molecules C4H3OCOOH, forming a octahedron. The Mo-O distances are in the range 1. 66 - 2. 39A ,the Mo-Cl distances fall in the range 2. 33-2. 34A.