CRYSTAL STRUCTURE OF（Bu4N）2[Pt（C3S5）2]

<正> The title compound C38H72N2PtS10(Mr=1072.74)crystallizes in triclinic system,space group P1 with cell constants a=11.994(4),b=18.117(7),c=11.855(6)A,α=95.55(4),β=99.14(3),γ=75.71(3)°,V=2460.0A3,Z=2 and Dc=1.45 gcm-3.The structure is solved by direct methods and refined by full-matrix least-squares technique to final R=0.046 and Rw=0.045 based on 5919 independent reflections with I≥3.0(I).The anion [Pt(C3S5)2]2-is approximately planar,of which the platinum-sulfur coordination polyhedron takes a square form with mean Pt-S bond length of 2.310(4)A.     

Synthesis,Crystal Structure and Neuroprotection of Methyl 2-（（4-（2-（2-Methylphenoxy）acetyl）- piperazin-1-yl）-methyl）benzoate①

A new phenoxyacetamide derivative, methyl 2-((4-(2-(2-methylphenoxy)acetyl)piperazin-1-yl)methyl)benzoate(C22H26N2O4, Mr = 382.45), has been synthesized and characterized by 1H NMR, 13 C NMR, H RMS and single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a = 11.145(2), b = 13.667(3), c = 13.998(3)A, β = 112.01(3)o, V = 1976.8(7)A3, Z = 4, Dc = 1.285 g/cm3, F(000) = 816, μ = 0.089 mm-1, MoKα radiation(λ = 0.71073 A), the final R = 0.0602 and wR = 0.1533 for 2343 observed reflections with I 2σ(I). Intramolecular C–H···O interactions as well as intermolecular C–H···O hydrogen bonds help to stabilize the crystal structure. The preliminary bioassay results show that the title compound exhibits potent neuroprotective activity.     

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.     

Solvothermal Synthesis and Crystal Structure of a Layered Thioantimonate（Ⅲ） [C4HgNH3]2Sb4S7

An inorganic-organic hybrid thioantimonate(Ⅲ) [CH3(CH2)3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method.1 crystallizes in the triclinic system, space group P with a = 7.0124(11), b = 11.919(2), c = 14.879(3) (A), α = 108.791(3), β = 102.441(3), γ = 92.846(2)o, V = 1140.1(3) (A)3, Mr = 859.71, Z = 2, Dc = 2.504 g/cm3, μ= 5.324 mm-1, F(000) = 804, S = 1.013, the final R = 0.0297 and wR = 0.0618 for 3534 observed reflections with I＞2σ(I). 1 consists of [C4H9NH3] cations and two-dimensional [Sb4S7]n2n-anion which is composed of three SbS3 trigonal pyramids and one SbS4 unit joined by sharing common corners. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3] cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.     

A New Heteropolyoxotungstate with a Three-dimensional All-inorganic Framework [（C2H4N2）4（P4Co3W4O（28）H6）（H2C2O4）]n

A new heteropolyoxotungstate [(C2H4N2)4(P4Co3W4O28H6)(H2C2O4)]n with a three-dimensional framework was hydrothermally synthesized.The compound crystallizes in a tetragonal system,space group I41/a with a = 17.1006(17),b = 17.1006(7),c = 10.7525(5),V = 3144.2(2)3,Z = 4,Dc = 3.795 g·cm-3,F(000) = 3300,MoKα(λ = 0.71073 ),μ = 16.460 mm-1,the final R = 0.0335 and wR = 0.0776.In the heteropolyoxotungstate,tungsten-oxygen octahedra are linked by sharing two cis-vertexes into an infinite helical chain extending along the c axis.Cobalt atoms in the octahedral geometry act as the linkers of these chains,forming a three-dimensional framework.The cobalt and phosphorus atoms in the tetrahedral geometry play a role in stabilizing the three-dimensional framework.Ethylenediamine molecules are polymerized into organic chains which locate in the interspaces of the framework in the way of interwinding with the W-O chains.     

Synthesis and Crystal Structure of [Cd（NBA）（μ3-OH）（4,4＇-bipy）1/2]n

A new cadmium polymer [Cd(NBA)(μ3-OH)(4,4'-bipy)1/2]n 1 (NBA=m-nitrobenzoic acid and 4,4'-bipy=4,4-bipyridine) has been synthesized by hydrothermal reaction. Its structure was determined by single-crystal X-ray diffraction method, and characterized by elemental analysis and IR spectrum. The crystal is of monoclinic, space group C2/c, with a=15.6912(9), b=25.9394(15), c=6.7332(4)(A), β=114.7700(10)°, V=2488.4(3)(A)3, C12H9CdN2O5, Mr=373.61, Z=8, Dc=1.995 g/cm3,μ=1.776 mm-1, F(000)=1464, R=0.0411 and wR=0.1128 for 2130 observed reflections (I ＞ 2σ(I)).X-ray diffraction studies reveal that the compound features a layered structure, in which 4,4'-bipy ligands bridge Z type of double chains [Cd(μ3-OH)]n and NBA ligands locate at the two sides of the layer. The π-π interactions between the benzene rings of NBA ligands of two adjacent layers lead to the 3D framework.     

Syntheses, Crystal Structures and Antibacterial Activities of Copper（Ⅱ） and Zinc（Ⅱ） Complexes Based on （E）-4-fluoro-2-（（3-morpholinopropylimino）methyl）phenol

Two Schiff base complexes [Cu(L)2] (1) and [Zn(L)2]·3H2O(2) of (E)-4-fluoro-2-((3-morpholino propylimino)methyl)phenol (HL) have been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. Crystal data for 1: triclinic, space group Pī with a=4.8000(10), b=11.109(2), c=13.921(3),α=66.55(3),β=80.35(3),γ=81.09(3)°, V=668.2(2)3 , Z=1, Dc=1.477g/cm 3 , F(000)=311, and the final R=0.0744 and wR=0.1601 for 2301 observed reflections with I > 2σ(I). And those for 2: monoclinic, space group P21 /c with a=14.789(3), b=11.713(2), c=18.846(4),β=107.85(3)°, V=3107.4(11)3 , Z=4, D c=1.389 g/cm 3 , F(000)=1368, and the final R=0.0749 and wR=0.1348 for 5423 observed reflections with I > 2σ(I). Both 1 and 2 are four-coordinated complexes, with a square-planar geometry of copper(Ⅱ) in 1 and a slightly distorted tetrahedral geometry of zinc(Ⅱ) in 2. An asymmetric unit consists of only one half of a Cu ion and one L ligand in 1, while an asymmetric unit is composed of one Zn ion, two L ligands and three water molecules in 2. Non-classical C-H···O and C-H F hydrogen bonds play important roles in the formation of a 1D chain of 1, but O-H O and O-H N hydrogen bonds play dominant roles in the self-assembly of a 3D network of 2. The antibacterial activities of 1 and 2 against B. subtilis, S. aureus, S. faecalis, P. aeruginosa, E. coli and E. cloacae have been evaluated by MTT method.     

Synthesis, Structure and Photo- luminescence of Cu[（PPh3）2]（acac） （PPh3 = Triphenylphosphine, acac = Acetylacetone）

A novel complex Cu(PPh3)2(acac) 1 (PPh3 = triphenylphosphine, acac = acetylacetone) was obtained by a solution reaction and structurally characterized by X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 13.7361(8), b = 12.8204(7), c = 19.7638(13) , β = 95.946(2)°, C41H37CuO2P2, Mr = 687.19, V = 3461.7(4) 3, Z = 4, Dc = 1.319 g/cm3, S = 1.067, μ(MoKα) = 0.758 mm–1, F(000) = 1432, R = 0.0403 and wR = 0.0990. Complex 1 is characterized by an isolated structure. X-ray structure analysis of 1 shows that acac behaves as a chelating ligand and PPh3 coordinates as a monodentate ligand to the Cu(I) atoms. Photoluminescent investigation reveals that the title complex displays a strong green-light emission.     

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.     

A New Luminescent Complex Cd（Ⅱ）-xanthene-9-carboxylate: [Cd（L）2（H2O）]n

A new luminescent Cd(Ⅱ) coordination polymer, [Cd(L)2(H2O)]n 1 (HL = xan-thene-9-carboxylic acid), was synthesized hydrothermally and characterized by satisfactory elemental analysis, FT-IR spectra and single-crystal X-ray diffraction. The crystal is of orthorhombic system, space group P212121 with a = 6.4548(4), b = 13.0876(12), c = 27.466(2), V = 2320.3(3)3, C28H20CdO7, Mr = 580.84, Z = 4, Dc = 1.663 g/cm3, F(000) = 1168, μ = 0.990 mm-1, Flack parameter = 0.00(2), the final R = 0.0296 and wR = 0.0691 for 5301 observed reflections (I > 2σ(I)). 1 features a one-dimensional (1D) carboxylate oxygen-bridged inorganic chain, which is further connected by intermolecular hydrogen bonds into a three-dimensional (3D) framework. Moreover, compound 1 exhibits strong photoluminescence in the solid state at room temperature.     

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.     

2-[4-(2,6-二氟苯基)噻唑-2-基]-3-羟基丙烯腈衍生物的合成及生物活性

为了寻找生物活性良好的噻唑基丙烯腈类化合物, 利用2-[4-(2,6-二氟苯基)噻唑-2-基]乙腈(3)分别与取代氯甲酸酯4和取代苯基异氰酸酯6在碱存在下反应, 合成了8个2-[4-(2,6-二氟苯基)噻唑-2-基]-3-羟基-3-烃氧基丙烯腈化合物5和7个2-[4-(2,6-二氟苯基)噻唑-2-基]-3-羟基-3-取代苯胺基丙烯腈化合物7, 均为首次报道的丙烯腈类化合物. 化合物结构经1H NMR, IR, MS和元素分析表征. 初步生物活性测定结果表明, 在试验浓度下, 目标化合物均具有一定的杀虫和抑菌活性, 其中化合物5f和5h在100 mg/L浓度下对炭疽病菌的抑制率达95%; 化合物5g和7d在250 mg/L浓度下对棉红蜘蛛的致死率达85%.     

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%.     

4-(7-甲氧基-2,2-二甲基-2,3-二氢苯并呋喃-5-基)-2-芳氨基噻唑的合成、晶体结构与杀虫活性

以2-(2-甲基烯丙氧基)苯酚为原料, 经Claisen重排、呋喃环化、醚化、Friedel-Crafts乙酰化、α-溴代和噻唑环化等反应合成了22种4-(7-甲氧基-2,2-二甲基-2,3-二氢苯并呋喃-5-基)-2-芳氨基噻唑化合物. 化合物的结构经质谱、1H NMR和元素分析等确证. 采用单晶X射线衍射仪测定了化合物7j的晶体结构, 该晶体属于单斜晶系, 空间群为C2/c, 晶胞参数a=2.21140(12) nm, b=0.87602(5) nm, c=2.13911(12) nm, β=115.5380(10)°; V=3.7391(4) nm3, Z=8, Dc=1.375 g/cm3, F(000)=1616, S=1.046, μ=0.333 mm-1, 最终偏差因子R1=0.0390, wR2=0.1079. 杀虫活性实验结果表明, 化合物7a, 7b, 7h和7t在浓度为500 mg/L时对蚕豆蚜死亡率分别为95.12%, 62.60%, 57.53%和59.06%.     

2-(Benzo[d]thiazol-2-yl) phenyl-4-nitrophenyl alkyl/aryl substituted phosphoramidates: Synthesis,characterization and antimicrobial activity evaluation

A series of new 2-(benzo[d]thiazol-2-yl) phenyl-4-nitrophenyl alkyl/aryl substituted phosphoramidate derivatives (7a-j) of biological interest are synthesized in two steps via an in situ process without the isolation of the intermediate. 2-(Benzo[d]thiazol-2-yl) phenol (3) was treated with 4-nitrophenyl phosphorodichloridate(4) to obtain the monochloro intermediate, 2-(benzo[d]thiazol-2-yl)phenyl (4-nitrophenyl) phosphorochloridate(5). It was subsequently reacted with various amines, 6(a-j) to afford the desired title products. IR, NMR (¹H, ¹³C and ³¹P), mass spectral and elemental analysis are used to characterize the structures of the newly synthesized compounds. The antibacterial and antifungal activities are determined by the growth of inhibition of bacteria and fungi of the title compounds at two concentrations, 50 and 100 µg/mL, and minimum inhibitory concentrations to the active compounds. The compounds 7e, 7f and 7j exhibited promising inhibition activity against bacterial strains and 7c, 7e and 7i against A. niger and C. albicans and MIC values are in the range of 10.0–15.0 µg/mL.     

SYNTHESIS AND CRYSTAL STRUCTURE OF AZACROWN (2, 2) DINITRATE [C_(12)H_(28)O_4N_2] (NO_3)_2

<正> [C12H28O4N2](NO3)2, Mr = 388. 45, monoclinic space group P21/ n,a = 7. 811(2), b = 10.626(4), c= 11. 823(6) A , β=106.51(3)°, Z = 2, Dc = 1.37 gem-3, V = 940. 8(7) (?)3 F(000) = 416, μ(MoKα) =1. 3 cm-1, R =0. 044 for 1373 reflections. The structure contains prdtonated azacrown [H2(2,2)]2+ and two (NO3-) which are bridged by four hydrogen bonds O(nitrate) ...H-N(crown). The ion [H2(2,2)]2+ in the title crystal lies on the crystallographic center of symmetry. There is half a [H2(2,2)]2+ and one NO3- in an asymmetric unit.     

Cobalt(II)-selective membrane electrode based on N,N′-di(thiazol-2-yl)formimidamide

A new PVC-membrane electrode for Co²⁺ ions based on N,N′-di(thiazol-2-yl)formimidamide (TF) as membrane carrier has been developed. The electrode resulted in Nernstian response (29.5?±?0.4?mV decade^?1) for Co²⁺ ion over a wide concentration range (2.5?×?10^?7 ?1.0?×?10^?1?M) with a detection limit of 6.1?×?10^?8?M. The sensor has a response time of about 10?s, and can be used for at least 2 months without observing any deviation from the Nernstain response. The electrode revealed good selectivity towards cobalt(II) ion over a wide variety of alkali, alkaline earth, transition, and heavy metal ions and could be used in the pH range 2.0–7.0. The electrode was used for determination of Co²⁺ in real samples.     

Synthesis, Crystal Structure and Fungicidal Activity of (E)-2-[(4-tert-Butyl-5- (4-methoxybenzyl)thiazol-2-ylimino)methyl]phenol

The title compound(E)-2-(4-tert-butyl-5-(4-methoxybenzyl)thiazol-2-ylimino)me-thylphenol was synthesized by the reaction of 5-(4-methoxybenzyl)-4-tert-butylthiazol-2-amine with salicylaldehyde=and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system=space group P21/c with a=5.9362(8)=b=11.5070(15)=c=29.460(4)=β=97.326(3)°=V=1995.9(5)3=Z=4=F(000)=808=C22H24N2O2S=Mr=380.49=Dc=1.266 g/cm3=S=1.031=μ=0.181 mm--1=the final R=0.0474 and wR=0.1441 for 4327 observed reflections(I > 2σ(I)).Intramolecular O-H…N hydrogen bond is observed in the crystal.The preliminary bioassay showed that the title compound exhibits 95% inhibition rate against Rhizoctonia solani at the test concentration of 500 mg/L.     

Synthesis and Structure of [Er4（μ3—OH）4（Hpro）4（Pro）2（H2O）7]（ClO4）6.7H2O

1 INTRODUCTION The design and synthesis of polynuclear com- plexes have attracted chemists?attention in the contemporary chemistry, since their clusters maybe lead to novel materials with magnetic, optical, electronic and catalytic properties of the constituent metals[1～3]. It is also prevalently interesting to synthesize high-nuclearity metal complexes for their nanoscopic dimensions[3, 4]. Spectroscopic properties of the lanthanides are widely used in the study of biological systems. …