Synthesis and Crystal Structure of α,α,β,β-5,10,15,20-Tetrakis（2-aminophenyl）porphyrin

The title compound,α,α,β,β-5,10,15,20-tetrakis（2-aminophenyl）porphyrin, has been obtained and characterized by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 31.804（6）, b = 19.314（4）, c = 12.872（3） A, β= 90.592（3）°, Z = 4, V = 7907（3） A^3, Dc= 1.193 g/cm^3, Mr= 1419.67, λ（MoKα） = 0.71073A, μ= 0.073 mm^-1, F（000） = 2984, R = 0.0773 and wR = 0.2045. The crystallographic analysis indicates the existence of N-H...π intermolecular interactions and hydrogen bonds which link the complex molecules into a 3D network structure.     

Synthesis,Crystal Structure and DNA-binding Properties of a New Copper（Ⅱ） Schiff Base Complex

A new asymmetric bidentate copper(Ⅱ) complex,CuL 2(HL=2-((E)-(4-bromophenylimino)methyl)-6-bromo-4-chlorophenol),has been synthesized and characterized by elemental analyses and single-crystal X-ray diffraction.The complex crystallizes in the monoclinic space group P2 1 /c with a=11.218(3),b=9.355(3),c=13.449(4),β=108.722(4)°,V=1336.8(6)3,Z=2,Dc=2.008 g/cm 3,μ(MoKα)=7.024 mm-1,F(000)=806,S=0.999,the final R=0.0342 and wR=0.0641for2611observed reflections (I>2σ(I)).The central copper(Ⅱ) is four-coordinate and bonds to two nitrogen and two oxygen atoms from two Schiff base ligands.The complex is linked into a two-dimensional supramolecular structure by weak intermolecular interactions.In addition,DNA-binding properties of the metal complex were investigated using spectrometric titrations and viscosity measurements.The results show that the complex binds with calf-thymus DNA(CT-DNA),presumably via a partial intercalative mode.The intrinsic binding constant of the Cu(Ⅱ) complex with DNA is 7.335×10 3 M-1.     

Crystal Structure of 6β,7β,14β-Trihydroxy-1α-acetoxy-7α,20-epoxy-ent-kaur-16-en-15-one

6β,7β,14β-Trihydroxy-1α-acetoxy-7α,20-epoxy-ent-kaur-16-en-15-one was isolated from the natural plant of Isodon japonica (Burm.f), Haravar. galaucocalyx (maxim) Hara. The structure was elucidated by means of spectral and chemical studies. In addition, its crystal was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1, Z = 2, a = 6.3506(4), b = 13.5766(8), c = 15.2777(9) , α = 80.506(1), β = 83.856(1), γ = 88.307(1)o, C25H36O9, Mr = 480.54, V = 1291.64(13) 3, Z = 2, Dc = 1.236 g/cm3, F(000) = 516, μ = 0.093 mm-1, S = 0.988, the final R = 0.0761 and wR = 0.1955. Flack factor is 0.02(19), and the largest peak and deepest hole on the final difference Fourier map are 0.556 and –0.265 e/3, respectively. The X-ray diffraction shows the existence of intermolecular C–H…O (DA) hydrogen bonds between adjacent molecules.     

Preparation and Crystal Structure of 12β,15α-dihydroxyprogesterone

Progesterone(1) was biotransformed into the title compound 12β,15α-dihydroxy-progesterone(2) with Colletotrichum lini AS3.4486.The biotransformation process was monitored with HPLC.The structure of 2 was determined by 1H NMR,13C NMR,ESI-MS and single-crystal X-ray diffraction.The crystal of the compound belongs to orthorhombic,space group P212121 with a = 8.0671(9),b = 12.3970(15),c = 18.532(3) ,Z = 4,V = 1853.3(4)3,Dc = 1.242 mg/m3,μ = 0.084 mm-1,F(000) = 752,R = 0.0373 and wR = 0.0850.Single-crystal X-ray diffraction analysis reveals that a 1D supramolecular structure of 2 has been constructed by multiply intermolecular O(2)-H(2)…O(4) and O(3)-H(3)…O(2) H-bonding interactions.     

Synthesis of Some Novel Phenyl Substituted Oxothiazolidin- 1’’,3’’,4’’-thiadiazolo-[3’,4’-b]thiazoline of 3β-Substituted Cholestane

Three title compounds 4a—4c have been synthesized by the cyclodehydration of 1’-benzylidine-4’-(3β-substituted-5α-cholestane-6-yl)thiosemicarbazones 2a—2c with thioglycolic acid followed by the treatment with cold conc. H2SO4 in dioxane. The compounds 2a—2c were prepared by condensation of 3β-substituted-5α-cholestan- 6-one-thiosemicarbazones 1a—1c with benzaldehyde. These thiosemicarbazones 1a—1c were obtained by the reaction of corresponding 3β-substituted-5α-cholestan-6-ones with thiosemicarbazide in the presence of few drops of conc. HCl in methanol. The structures of the products have been established on the basis of their elemental, analytical and spectral data.     

Syntheses,Crystal Structures,and Antimicrobial Activities of N′-(5-Hydroxy-2-nitrobenzylidene)-4-dimethylaminobenzohydrazide Methanol Solvate and 2-Fluoro-N′-(5-hydroxy-2-nitrobenzylidene)benzohydrazide

Two new hydrazone compounds,N'-(5-hydroxy-2-nitrobenzylidene)-4-dimethyl-aminobenzohydrazide methanol solvate (1) and 2-fluoro-N'-(5-hydroxy-2-nitrobenzylidene)benzo-hydrazide (2),have been synthesized and characterized by elemental analysis,IR spectra,1H NMR,and single-crystal X-ray diffraction.Compound 1 crystallizes in the monoclinic space group P21/c with a=11.571(3),b=12.420(3),c=12.360(2) ?,β=97.495(2)°,V=1761.1(7) 3,Z=4,R=0.0735 and wR=0.1344.Compound 2 crystallizes in the triclinic space group P with a=7.551(3),b=8.254(3),c=11.365(2) ?,α=79.352(2),β=76.154(2),γ=71.624(2)°,V=648.2(4) 3,Z=2,R=0.0393 and wR=0.1008.The hydrazone molecules of the compounds display E configurations with respect to the C=N double bonds.In the crystal structure of 1,the hydrazone molecules are linked by methanol molecules through N-H…O,O-H…N and O-H…O hydrogen bonds,forming chains running along the c axis.In the crystal structure of 2,molecules are linked through N-H…O and O-H…O hydrogen bonds,forming ribbons running along the b axis.The preliminary antimicrobial activities were studied.     

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Novel Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]_2·[BiCl_6]·Cl}

A novel supramolecular compound,{[2-(2-pyridyl)benzimidazoleH2]2·[BiCl6]·Cl},was synthesized by the hydrothermal reaction of o-phenylenediamine and α-pyridinecarboxylic acid with BiCl3 in 6.0 mol·L-1 HCl solution,and characterized by elemental analysis,IR,X-ray single-crystal diffraction and photoluminescence spectroscopy.The crystal (C24H22N6Cl7Bi,Mr= 851.61) belongs to the triclinic system,space group P1 with a =7.2887(18),b =9.548(2),c= 12.469(3),α=85.306(4),β=82.814(4),γ=71.349(4)°,Z=1,V=814.9(3)3,Dc=1.735 g/cm3,μ(MoKα)=6.007 mm-1,F(000)=410,R=0.0307 and wR=0.0787.The bismuth ion and six chlorine ions construct a distorted octahedral configuration.The three-dimensional supramolecular network is built from electrostatic attractions,hydrogen bonds and π-π interaction between the BiCl6 anion,Cl anion and [2-(2-pyridyl)benzimidazoleH2] cation.The photoluminescence spectroscopy study shows that the title compound has a blue fluorescent emission at 450 nm in the solid state.     

Hydrothermal Synthesis,Crystal Structure and Antimicrobial Activity of a New Ni(Ⅱ) Complex

The title complex [NiL]·H2O(C20H24N2NiO5,L = paeonol-ehylenediamine) was synthesized by the hydrothermal method and characterized by IR,cyclic voltammetry and X-ray single-crystal diffraction.The complex belongs to the monoclinic system,space group P21/c with a=13.4361(13),b=7.3290(10),c=20.981(2),β=109.244°,V=1950.6(4)3,Z=4,F(000)=904,Dc=1.468 g/cm3,μ(MoKα)=1.029 mm-1,the final R=0.0588 and wR=0.1577.The complex exhibits antimicrobial activities(antimicrobial activities against Staphylococcus aureus and Escherichia codi) by agar diffusion measurement.     

Synthesis and Crystal Structure of 9-（2-Hydroxy-5-nitrophenyl）-9H-dibenzo[c,h]-2,7,10-trioxanthene-1,8-dione DMF Solvate

The title compound 9-(2-hydroxy-5-nitrophenyl)-9H-dibenzo[c,h]-2,7,10-trioxan-thene-1,8-dione DMF solvate (C28H20N2O9,Mr=528.46) was synthesized and crystallized.The crystal belongs to the triclinic system,space group P1 with a=10.210(3),b=10.698(4),c=12.522(4),α=92.214(6),β=113.751(5),γ=105.040(5)°,Z=2,V=1193.0(7)3,Dc=1.471 g·cm-3,μ(MoKα)=0.112 mm-1,F(000)=548,R=0.0444 and wR=0.1141 for 2667 observed reflections (I 2σ(I)).X-ray analysis reveals that atoms C(1),C(2),C(3),C(4),C(5) and O(1) on the new 4H-pyran ring are slightly distorted,forming a half-chair conformation.     

MOLECULAR STRUCTURES AND SINGLE CRYSTAL ESR SPECTRA OF IMIDAZO-LATE-BRIDGED Co(Ⅲ)-Cu(Ⅱ)-Co(Ⅲ)AND Co(Ⅲ)-Zn(Ⅲ)-Co(Ⅲ) COMPLEXES

The structures of the heterotrinuclear complexes, [(NH_3)_5ColmCu(dien)ImCo(NH_3)_5]-(C10_4)_6·4H_20 and [(NH_3)_5CoImZn(dien)ImCo(NH_3)_5]-(ClO_4)_6·4H_2O, are reported. Co--Cu--Cocrystallizes in the monoclinic space group C2/c with a =32.414(4), b= 9.421(1), c=15.167(5)?,β= 90.91(2)°, Z=4 and Co--Zn--Co in the same space group with a = 32.578(2), b = 9.419(1), c = 15.125(3)?, β=91.10(1)°Z=4. The Cu(Ⅱ) and Zn(Ⅱ) geometriesare intermediate between a trigonal bipyramid and a square pyramid,the Co(Ⅲ) is a-hexagonal coordination and the dien ligand shows a disordered contribution in the respectivestructure.The magnetic properties of Co--Cu--Co are investigated. From the single crystalESR spectra studies, the anisotropic g and A tensors and electronic spin-density of Co--Cu--Co are obtained and the nature of the bonding for Cu~(2+) is discussed.     

CRYSTAL STRUCTURE OF GdCl_3(DIMETHOXYETHANK)_2

<正> C8H2oCl3GdO4,Mr=443.80,monoclinic, space group P21/c, a=11.442 (3),b= 8.849(2), c= 15.575(5)A,β=104.8l(2)° ,V=1521.9(7)A3,Z= 4, DC = 1.94 g/cm3,λ(MoKα) =0.71069A,F(000)=860. The structure was solved by Patterson and Fourier techniques and refined by least-squares nethod to a final conventional lvalue of 0.051 (Rw=0.054). The central ion Gd(III) is bonded to three chlorine atoms and four oxygen atoms froa two dimethoxye-thane molecules to form a distorted pentagonal bipyramid. The Qd-Cl distances are in the range of 2.460-2.628A (average 2.571A). The Gd-O distances are in the range of 2.408-2.493A (average 2.458A).     

Syntheses, Structures and Fluorescent Property of Two Cd（II） 3D Coordination Polymers with Mixed Ligands of Azide and Piperazine Derivatives

Two new coordination polymers, [Cd(N3)2(Baep)1/2]n(1) and [Cd2(N3)4(CH3OH)(Bapp)1/2]n(2) (Baep=1,4-bis(2-aminoethyl)piperazine, Bapp=1,4-bis(3-aminopropyl)piperazine) were synthesized. The crystal of 1 is of monoclinic system, space group P21/c with a=9.341(7), b=11.677(9), c=8.195(6), β=93.925(13)°, V=891.8(11)3 , Z=4, μ(MoKα)=2.42 mm-1 , Mr=280.58, Dc=2.090 g/cm3 , the final R=0.0297 and wR=0.0720. The crystal of 2 is of triclinic system, space group PI with a=9.121(5), b=9.666(5), c=10.250(6), α=72.91(2), β=77.10(2), γ=73.95(2)°, V=820.0(8)3 , Z=2, μ(MoKα)=2.62 mm-1 , Mr=522.10, Dc=2.114 g/cm3, the final R=0.0251 and wR=0.0632. Single-crystal X-ray diffraction studies reveal that 1 is a 3D structure based on a dinuclear unit {Cd2(N3)4(Baep)}, in which the Baep ligands formed in situ display two different bridging modes. Compound 2 also has a 3D structure based on a tetranuclear cluster {Cd4(N3)8(CH3OH)2(Bapp)}, in which the azido anions exhibit four different bridging modes (μ-1,1, μ-1,3, μ-1,1,1 and μ-1,1,3). The thermal stability and fluorescent property of 1 and 2 have also been investigated.     

Synthesis and Crystal Structure of a Vanadium(Ⅴ) Complex with 2-Hydroxy-1-naphthaldehyde Isonicotinoyl Hydrazone

The mononuclear vanadium(Ⅴ) complex with 2-hydroxyl-1-naphthaldehyde isoncotinoyl hydrazone was synthesized and characterized by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P2 1/n with a = 10.3153(15),b = 7.4024(11 ),c = 24.413(4) (A),β= 101.911(2)°,V= 1824.0(5) (A)3,Z = 4,Mr = 427.28,Dc = 1.556 g/cm3,F(000) = 880,μ(MoKα) =0.591,the final R = 0.0372 and wR = 0.0926.The vanadium(Ⅴ) atom adopts a distorted square-pyramidal geometry coordinated by the tridentate ligand and two oxygen atoms.The hydrogen bonds and strong π…π stacking interactions link the complex molecules into a 3-D network structure.     

Synthesis and Crystal Structure of a Vanadium（V） Complex with 2-Hydroxy-1-naphthaldehyde Isonicotinoyl Hydrazone

The mononuclear vanadium(Ⅴ) complex with 2-hydroxyl-1-naphthaldehyde isoncotinoyl hydrazone was synthesized and characterized by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P2 1/n with a = 10.3153(15),b = 7.4024(11 ),c = 24.413(4) (A),β= 101.911(2)°,V= 1824.0(5) (A)3,Z = 4,Mr = 427.28,Dc = 1.556 g/cm3,F(000) = 880,μ(MoKα) =0.591,the final R = 0.0372 and wR = 0.0926.The vanadium(Ⅴ) atom adopts a distorted square-pyramidal geometry coordinated by the tridentate ligand and two oxygen atoms.The hydrogen bonds and strong π…π stacking interactions link the complex molecules into a 3-D network structure.     

Synthesis,Crystal Structure and Herbicidal Activity of Methyl(E)-α-(Methoxyimino)-2-((4-(3-chloro-5-(trifluoromethyl)-pyridine-2-yl)phenoxy)methyl)benzeneacetate

The title compound methyl(E)-α-(methoxyimino)-2-((4-(3-chloro-5-(trifluoromethyl) pyridine-2-yl)phenoxy)methyl)benzeneacetate(C23 H18 ClF3 N2 O4) has been synthesized and structurally characterized by 1 H and 13 C NMR, and HRMS. Its absolute molecular configuration was investigated by X-ray crystallography. The crystal crystallizes in monoclinic system, space group P21/c with a = 15.0928(7), b = 19.6070(10), c = 7.5535(5) ?, β = 98.176(5)°, V = 2212.6(2) ?3, Z =4, Dc = 1.438 g/cm3, F(000) = 984, μ(Mo Kα) = 0.231 mm-1, the final R = 0.0619 and wR = 0.1681 with 4034 observed reflections with I 2σ(I). The title compound has significant inhibitory rate against broadleaf weeds. They are all 100% under the dose of 37.5 g.a.i/ha, which was better than mesotrione.     

SYNTHESIS AND STRUCTURE OF EUROPIUM (Ⅲ) WITH N,N'''' BISSALICYLIDENE ETHYLENEDIAMINE (H_2salen)

<正> A europium (Ⅲ) complex with N, N' - bissalicylidene-ethylenediamine (H2salen) has the formula Eu(Hsalen)(salen)4H2O,where water molecules are in the outer sphere and do not coordinate with Eu (Ⅲ), was synthesized and structurally studied. The central atom Eu is coordinated by four nitrogen atoms and four oxygen atoms in a deltadodecahedron arrangement. The crystal is monoclinic,space group P21/a with cell constants a=16. 441(2),b=20. 599(3),c=10. 719(2) A ,β=84. 16(1)°,Z=4 and V = 3611. 5(8) A3,Dc=1. 392g/cm3.The final standard deviation R is 0. 093.     

Synthesis,Crystal Structure and Biological Evaluation of 4-Chloro-2-(morpholine-4-carbonyl)phenyl-4′-methoxybenzoate as Molluscicidal Agent

The title compound 4-chloro-2-(morpholine-4-carbonyl)phenyl-4'-methoxybenzoate(C19H18ClNO5, Mr = 375.79), a 5-chlorosalicylic acid derivative incorporating morpholine moiety, was conveniently synthesized through two steps and crystallized in the monoclinic space group P21/c with a = 7.8501(10), b = 9.3149(12), c = 25.133(3), V = 1836.2(4)3, Z = 4, Dc = 1.359 Mg/m3, λ = 0.71073, μ(MoKα) = 0.237 mm-1, F(000) = 784, R = 0.0447 and wR = 0.1227 for 3982 independent reflections with I 2σ(I). The dihedral angles formed between 4-methoxybenzene and 5-chlorobenzene rings, the 5-chlorobenzene and morpholine, and 4-methoxybenzene and morpholine rings are 82.55(3), 72.56(5) and 47.68(0)° by X-ray analysis, respectively. Bioassay shows that the title compound has a good molluscidal effect.     

Synthesis and Crystal Structure of 8-(2,3-Dimethoxyphenyl)-10,11,12,13-tetrahydro-9H-benzo [f] cyclohepta [c] quinoline

The title compound 8-(2,3-dimethoxyphenyl)-10,11,12,13-tetrahydro-9H-benzo[f]-cyclohepta[c]quinoline(C26H25NO2,Mr=383.47) was synthesized and characterized by IR,1H NMR,13C NMR and elemental analysis.The crystal belongs to triclinic,space group P1 with a= 8.1490(16),b=9.2550(19),c=14.373(3) ,α=86.96(3),β=89.66(3),γ=70.32(3)°,Z=2,V=1019.2(4) 3,Dc=1.250 g·cm-3,μ(MoKα)=0.078 mm-1,F(000)=408,the final R=0.0555 and wR=0.1240 for 2228 observed reflections(Ⅰ > 2σ(Ⅰ)).X-ray analysis reveals that the seven-numbered ring is slightly similar to a six-numbered ring,forming the chair-like conformation.The four rings(Ⅰ,Ⅱ,Ⅲ and Ⅳ) in the benzo[f]cyclohepta[c]quinoline moiety form a screw structure.     

Synthesis and Crystal Structure of N-[(3aR,4R,4aR,5aS,6S,6aS)-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]isoindol-2(1H)yl]-4-(trifiuoromethyl)phenylmethanimine Monohydrate

The crystal structure of the title compound (C19H17F3N2O4,Mr=394.35) was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group C2/c with a=28.383(6),b=10.355(2),c=12.799(3)(A),β=111.74(3)°,V=3493.8(12)(A)3,Z=8,De=1.499 g/cm3,λ(MoKα)=0.71073,F(000)=1632,μ= 0.127 mm-1,R=0.0412 and wR=0.1019.In the title compound,there exist three intennolecular hydrogen interactions (O(4)...O(1),O(4)...O(3) and O(4)...N(1)) between water.The neighboring molecules are linked to each other generating a two-dimensional network structure via the three intermolecular hydrogen bonds and π-π interactions shaped by phen-phen with centroid distance of 4.049 (A).     

Vanadium(Ⅳ)dimer complexes containing [V(o-C_6H_4OS)_3]~(2-)fragment and caged sodium ions

Tris[o-mercaptophenolato]vanadium(IV)dimer complexes(A)_2[V(mp)_3NaLL']_2(A=Ph_4P~+,H_2mp=o-mercaptophenol,L=MeCN,L'=EtOH,(1);L'=MeOH,(2))were prepared bythe reaction of anhydrous VCl_3 and Na_2mp in the molar ratio 1:3.Complex(3)(A=Et,N~+,L=L'=MeOH)was prepared by the reaction of VCl_3,Na_2mp and Li_2S in the molar ratio 1:2:1.The com-plexes were characterized by X-ray diffraction crystallography,infrared spectra,magnetic suseepti-bility,and cyclic voltammetric measurements.Complex 2 crystallizes in the triclinic space groupP1 with a=12.813(6),b=14.199(4),c=12.790(5),α=112.72(2),β=104.24(4).γ=88.68(4)°,V=2073.6,and Z=1.The structure was refined to R=0.058.Complex 3 crystallizes in the mono-clinic space group P2_1/n with a=12.359(3),b=17.452(6),c=14.829(13),β=96.51(5)°,V=3177.8,and Z=2.The final R factor is 0.067.Both of the anions of 2 and 3 contain two[V(rap)3]~(2-) fragmentslinked by sodium ions through the μ_3-O bridges with a crystallographic center of symmetry.The V(IV)atom is in a coordination environment intermediate between a trigonal prism and an ideal octahedron.