[Zn(DMF)6]H2SiW12O40·(CH3)2NH的合成,晶体结构及性质

The title compound [Zn(DMF)₆]H₂SiW₁₂O₄₀·(CH₃)₂NH was synthesized in mixed solvent of aqueous and acetonitrile, and its crystal structure had been determined using single crystal X-ray diffraction. The crystal belongs to monoclinic, space group C2/m, a=2.0654(4)nm, b=1.3306(3)nm, c=1.3194(3)nm, β=119.59(3)°, V=3.1531(11)nm³, D_c=3.606Mg·m^-3, Z=2, R=0.0462, R_w=0.0836. The title compound comprises of a [Zn(DMF)₆]²⁺ unit, a polyanion and a free (CH₃)₂NH molecule. The ESR spectrum of the title compound shows that charge-transfer between organic groups and polyanion takes place under irradiation of the sunlight in solid state. The TG study of the title compound shows that it had four stages of the weight loss, and the increase of the de-composition temperature for the polyanion shows that the stability of the polyanion was enhanced due to the influence of Zn²⁺ ion. CCDC:175866.     

钾的N-酰化牛磺酸配合物的合成、表征及其晶体结构

The title complex(K(C₉H₁₃NO₅S₂)(H2O)) was synthesized by the reaction of p-tolysulfonyl chloride, taurine and potassium hydrate in water-methanol-ethanol solution. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 336.44. The crystal structure of the title complex belongs to orthorhombic space group Pbca and cell parameters: a=0.853 31(12) nm, b=0.820 42(12) nm, c=3.989 4(6) nm. V=2.792 8(7) nm³, Z=8, D_c=1.600 g·cm^-3, μ=0.699 mm^-1, F(000)=1 400. The compound is an one-dimension chain complex of infinite length which are connected with hydrogen bond and bridging coordination water. The difference and same of the complexes were discussed. CCDC: 244938.     

一种Λ型吡啶碘盐的合成和晶体结构

A new Λ type pyriding iodide was synthesized by reaction of 4-picoline and methyl diiodide. The structure was characterized by elemental analysis, IR, UV and TG. The crystal structure of the title compound was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic with space group C2/c, a=18.812(4)?, b=8.7816(6)?, c=10.3165(12)?, β=93.71(1), V=1700.7(4)?³, Z=4. In the molecule, two 4-picoline molecules are bonded by -CH₂ group to form Λ type pyridine salt. CCDC: 180871.     

Cu(Ⅱ)-牛磺酸缩水杨醛席夫碱配合物的合成及晶体结构

The title complex was synthesized by reaction of taurine salicylic schiff base(TSSB), O-phenanthroline(phen) and cupric acetate in water-ethanol solution. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 498.00. And the crystal structure belongs to orthorhombic system with space group Pbcn and cell parameters: a=31.072(4)?, b=12.8909(18)?, c=10.3478(14)?; V=4144.7(10)?³,Z=8,D_c=1.596Mg·m^-3,μ=1.197mm^-1 and F(000)=2048. The compound is an one-dimensional chain complex of infinite length connecting with hydrogen bonds. The Cu(Ⅱ) was coordinated by two oxygen atoms and three nitrogen while the O atoms of Ac- groups did not coordinate. At the same time the Cu(Ⅱ)formed a distorted tragonal cone. Besides the capacities of coordination to Cu(Ⅱ) of atoms were discussed.     

混合配体配合物[Cd2(phen)4(bmal)2]·3H2O的合成与晶体结构研究

A novel binucleus mixed-ligand[Cd₂(phen)₄(bmal)₂]·3H₂O (phen=phenanthroline; bmal=benzylmalonic acid radical) has been synthesized by the reaction of phen and bmal with cadmium(Ⅱ) salt. X-ray crystal structure analysis was carried out to determine the crystal structure of the title complex. The crystal of the title complex belongs to monoclinic system with space group P2₁/c, a=1.119 1(8) nm, b=2.480 5(17) nm, c=1.063 4(8) nm, β=142.042(12)°, Z=4, V=2.887(3) nm³, D_c=1.613 g·cm^-3, R₁=0.046 2, wR₂=0.115 6, F(000)=1 424. One carboxyl of bmal is coordinated to Cd(1) with monodentate form, the others are coordinated to Cd(2) with bidentate form. The complexes form a 1-D chain structure bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in bmal, the 2-D network structure was formed by π-π interaction of neighbouring phen. CCDC: 257080.     

Cu(Ⅱ)-牛磺酸缩水杨醛席夫碱-邻菲咯林三元配合物的合成、晶体结构及性质

The title complex was synthesized by reaction of taurine salicylic schiff base(TSSB), O-phenanthroline(phen) and cupric acetate in water-ethanol solution. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 498.00. The crystal structure of the title complex belongs to orthorhombic system with space group Pbcn and cell parameters: a=3.107 2(4) nm, b=1.289 09(18) nm, c= 1.034 78(14) nm; and V=4.144 7(10) nm³, Z=8, D_c=1.596 g·cm^-3, μ=1.197 mm^-1, F(000)=2 048. The compound is an one-dimensional chain complex of infinite length which are connected with hydrogen bonds. The Cu(Ⅱ) was coordinated by two oxygen atoms and three nitrogen while the o atoms of Ac- groups did not participate in the coordination. The Cu(Ⅱ) formed a distorted tetragonal pyramid and the capacities of coordination to Cu(Ⅱ) of atoms was discussed. Besides, the TG-IR of the complex was analyzed. The kinetics of the thermal decomposition reaction of the complex was studied under a non isothermal condition by TG-IR. TG and DTG curves indicate that the complex decomposed in three stages: (?) The kinetic parameters were obtained from the analysis of TG,DTG cures by OZAWA-Flynn-Wall method, and the activation energy and the value of A of the three stages are 74.98 kJ·mol^-1, 286.65 kJ·mol^-1, 87.55 kJ·mol^-1; 9.66×10⁸ s^-1,1.82×10²⁸ s^-1, 3.09×10³s^-1, respectively.     

一维梯子状配位聚合物[Na3Er(2，6-PDA)3]·11.5H2O的合成与晶体结构

A novel 1D Ladder-like coordination polymer [Na₃Er(2，6-PDA)₃]·11.5H₂O (2,6-H₂PDA is pyridine-2,6-dicarboxylic acid) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to Monoclinic system with space group P2₁/c, a=0.969 7(3) nm, b=1.914 6(6) nm, c=1.8031(6) nm, β=91.524(5)°, V=3.346 6(18) mm³, Z=4, D_c=1.863g·cm^-3, μ=2.645 mm^-1. The coordination geometry configuration of Er³⁺ center is tricapped trigonal prism. The structures of the title compound exhibit a novel 1D Ladder-like chain.     

二苄基锡双(四氢吡咯荒酸酯)的合成、表征和晶体结构

Dibenzyltin bis(dithiotetrahydropyrrolocarbamate) was synthesized by the reaction of dibenzyltin dichloride with dithiotetrahydropyrrolocarbamate. The compound was characterized by elemental analysis, IR, ¹H NMR and MS. and the crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to or-thorhombic with space group Pccn, a=2.1665(6)nm, b=0.9932(3)nm, c=1.1979(3)nm,α=90°,β=90°,γ=90°,Z=2,V=2.5777(12)nm³,D_c=1.529g·cm^-3,μ(MoKα)=1.330mm^-1,F(000)=1208,R₁=0.0341, wR₂=0.0627. In the crystals, the structures consist of discrete molecules in which the tin atom is six-coordinate in a distorted octahedron configuration. CCDC: 179919.     

μ-氧-双[三(对氟苄基)锡]的合成、表征及晶体结构

The μ-oxygen-bis[tri(p-fluorobenzyl)tin] was synthesized. The structure were characterized by elementary analysis, IR and ¹H NMR and the crystal structure were determined by X-ray single crystal diffraction. The crystal of the title compound belongs to rhombohedral with space group R, a=1.346 4(4), b=1.346 4(4), c=1.772 9(7) nm, α=90°, β=90°, γ=120°, Z=3, V=2.783 2(15) nm³, D_c=1.625 g·cm^-3, μ(Mo Kα)=1.408 mm^-1, S=1.088, F(000)=1 350, R₁=0.027 5, wR₂=0.065 9. In compound, the tin atom has a distorted tetrahedral coordination configuration. CCDC: 257079.     

三唑酮氯化锌配合物的合成和晶体结构研究

The new compound was synthesized by the reaction of ZnCl₂ and triadimefon(ratio 1∶2) in ethanol solution refluxing for 6 hours. The crystal used for X-ray analysis was obtained by slow evaporation of the solution at room temperature. It crystallizes in the monoclinic system, space group P2/n. The lattice parameters are: a=1.58916(6)nm, b=0.60634(2)nm, c=1.83566(8)nm, β=93.979(2)°, V=1.7645(1)nm³, Z=2, D_c=1.362g·cm^-3, F(000)=744.00, μ(Mo Kα)=1.038mm^-1, R₁=0.042, wR₂=0.106. In the complex, the Zn(Ⅱ) cation is tetrahedrally coordinated to two triadimefon ligands and two chloride in cis disposition. The title complex was also characterized by elemental analysis, molar conductance, IR and TG-DTA. CCDC: 207413.     

氯化六咪唑合铁四水分子的结构表征和电化学性能研究(英)

The crystal structure of the title compound, [Fe(Im)₆]Cl₂·4H₂O, (Im=imidazole) was determined by X-ray analysis. The crystal structure consists of Fe(Im)₆²⁺ cation, two Cl^- anions and four non-coordinated water molecules. It crystallizes in the triclinic system, space group P1, with lattice parameters a=0.879 7(2) nm, b=0.906 8(2) nm, c=1.058 1(2) nm, α=75.35(3)°, β=83.20(3)°, γ=61.85(3)°, and Z=1; The Fe(Ⅱ) ion assumes centrosymmetric octahedron geometry with the FeN₆ core. Six imidazole molecules are coordinated to each iron(Ⅱ) ion through its tertiary nitrogen atom. The bond distances of Fe-N are in range of 0.212 8(1) nm to 0.220 4(1) nm. In the solid state, [Fe(Im)₆]²⁺, H₂O molecules and chlorine anions form three dimensional hydrogen bonds network which stabilized the crystal structure. Elemental analysis and electronic spectrum are in agreement with the structural data. The thermal gravity (TG) data indicate that thermal decomposition of the title compound takes place in five steps. In these cases, the residue may be Fe. From the cyclic voltammogram measurement in EtOH/H₂O, we know that electrode reaction was a quasi-reversible process. CCDC: 215335.     

钾的配合物C9H10KNO4S的合成、晶体结构及生物活性

The title complex was synthesized by the reaction of taurine 、salicylic and potassium hydrate in water-ethanol solution. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 267.34. and the crystal belongs to monoclinic system with space group P2₁/c and cell parameters： a=2.0292(8)nm， b=0.7283(4)nm， c=0.7540(4)nm; β=94.15(1)°， V=1.1115(9)nm3， Z=4， D_c=1.598 g·cm^-3， μ=0.0663mm^-1， F(000)=552. The complex is a lamellar compound of infinite expansion. In addi-tion， the complex has been tested for its antibacterial active. The average diameter of complex antibacterial activing cycle： colibacillus is 9mm， pseudomonas aeruginosa is 8mm. CCDC： 194630.     

二苄基锡二(2-哇啉甲酸)酯的合成、结构及量子化学研究

The novel dibenzyltin bis(2-quininate) has been synthesized. The crystal structure of the complex was determined by X-ray diffraction. The crystal belongs to monoclinic space group P2₁/c with a=1.840 05(14) nm, b=2.353 66(18) nm, c=2.044 31(16) nm, β=99.3130(10)°, V=8.736 9(12) nm³, Z=4, D_c=1.507 g·cm^-3, μ(Mo Kα)=9.21 cm^-1, F(000)=4 016, R₁=0.041 4, wR=0.082 1. In this compound, the tin atom rendered six-coordinated in a distorted octahedron geometry. The study on title complex has been performed, with quantum chemistry calculation by means of G98W package and taking Lanl2dz basis set. The stabilities of the complex, the orbital energies and composition characteristics of some frontier molecular orbitals have been investigated. CCDC: 609510.     

二苄基锡双(吗啉荒酸酯)的合成、表征及晶体结构

Dibenzyltin bis(dithiomorpholinocarbamate) was synthesized by the reaction of dibenzyltin dichloride with dithiomorpholinocarbamate. The compound was characterized by elemental analysis, IR, ¹H NMR and MS. and the crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to orthorhombic with space group Pca2₁, a=1.8327(3)nm, b= 0.65678(12)nm, c=2.2583(4)nm, Z=4, V=2.718 (9)nm³, D_x=1.528g·cm^-3,μ=1.271mm^-1, F(000)=1272, R₁=0.0434, wR₂=0.1152. In the crystals, the structures consist of discrete molecules containing six-coordinate tin atoms in a distorted octahedron configuration.     

有机锡化合物四对氰苄基锡(p-NCC6H4CH2)4Sn的合成、表征和晶体结构

The organotin(Ⅳ) compound (p-NCC₆H₄CH₂)₄Sn was synthesized by the reaction of p-cyanobenzyl chloride with tin. The compound was characterized by elemental analysis, IR, ¹H NMR, and the crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic, space group P1 with a=0.894 1(4) nm, b=0.977 9(4) nm, c=1.796 8(8) nm, V=1.386 9(11) nm³, Z=2, D_c=1.397 Mg·m^-3, μ(Mo Kα)=0.948 mm^-1, F(000)=588, R₁=0.046 9, wR₂=0.101 4. The tin atom adopts a distorted tetrahedral coordination geometry. CCDC: 272939.     

[Pb2(TNR)(NO3)2(H2O)]的制备和晶体结构研究

[Pb₂(TNR)(NO₃)₂(H₂O)] was prepared by reaction of the aqueous solution of lead nitrate and magnesium styphnate. The crystal structure of Pb₂(TNR)(NO₃)₂(H₂O)was determined by single crystal diffraction analysis. The crystal is triclinic, space group P1 with crystal parameters a=0.7279(2)nm,b=1.0698(2)nm,c=1.0738(2)nm;α=86.82(1)°,β=89.52(2)°,γ=83.50(2)°;V=0.8295(3)nm³,Z=2,D_c=3.201g·cm^-3, F(000)=716. The final R value is 0.0358.In the crystal structure, one lead ion was represented by nine coor-dination geometry; the other was showed as ten coordination geometry.     

高氯酸稀土Sm(Ⅲ)开环冠醚(EO4)配合物的晶体结构

The crystal of title compounds belongs to orthorhombic system with space group P2₁2₁2₁ (No.19). The cell parmeters are a=1.432 16(3) nm, b=1.457 20(3) nm， c=3.005 85(6) nm, and V=6 273.0(2) nm³, Z=8, μ(Mo Kα)=22.21 cm^-1， D_c=1.802 g·cm^-3, F(000)=3 416.00, Finally R₁=0.033 and wR₂=0.073 (I>2.00σ(I)), S=1.023. Every center atom Sm(Ⅲ) is surrounded by the two aether chains, the title compound has ten-coordinate structure and the coordination polyhedron shows a Bicapped Square Antiprism. In the crystal, the title compound has the flack of double moleculars and non-symmetry. The anion ClO₄^- does not take part in the coordination. CCDC: 238709.     

梯形结构有机锡配合物{[(p-MeC6H4CH2)2Sn]2(O)(Cl)OC2H5}2的合成和晶体结构

The title compound {[(p-MeC₆H₄CH₂)₂Sn]₂(O)(Cl)OC₂H₅}₂ was synthesized by the reaction of bis(p-met-hylbenzyl)tin dichloride with KOH in ethanol. The crystal structure of the complex has been determined by X- ray diffraction. The crystal belongs to monoclinic, space group P2₁/c with a=1.114 0(19) nm, b=2.423 1(3) nm, c=2.521 1(3) nm, β=99.398(3)°, V=6.714(16) nm³, Z=4, D_c=1.493 g·cm^-3, μ(Mo Kα)=15.94 cm^-1, F(000)=3 024, R₁=0.049 9, wR=0.101 7. The crystal structure shows that the coordination geometry of tin is a distorted trigonal bipyramid, and the ladder-like structure is shaped by three Sn₂O₂ planar four-membered rings. CCDC: 639682.     

Cu(Ⅱ)-2′-(2-噻吩亚甲基)水杨酰腙Schiff碱配合物的合成、表征、晶体结构及抑菌活性研究

In ethanol, the copper(Ⅱ) complex with the 2′-(2-thienylidene)-h ydroxybenzoylhydrazide, Cu(C₁₂H₁₀N₂O₂S)₂, was synthesized, and it′s structure was characterized by IR, UV and elemental analysis. The single crystal structure has been determined by X-ray diffraction analysis. The crystal belongs to monoclinic system, space group C2/c with cell constants, a=2.273 6(4) nm, b=0.592 12(9) nm, c=1.828 1(3) nm, β=109.735(5)°, V=2.316 4(7) nm³, Z=4, μ=1.164 mm^-1, D_c=1.595 g·cm^-3, F(000)=1 140, R=0.048 6, wR=0.101 6. In the compound copper(Ⅱ) atom is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. Their biological activities have been measused. The results show that the anti-bacterial activity of the coordination compound is much better that of the ligand. CCDC: 272938.     

甲酸桥联四核锰配合物[Mn4(O2CH)4(phen)8](ClO4)4·6H2O的水热合成和晶体结构

The title compound, [Mn₄(O₂CH)₄(phen)₈](ClO₄)₄·6H₂O(1), where phen=1,10-phenanthroline, was synthes-ized and its crystal structure was determined by X-ray diffraction structure analysis. The crystal is of monoclinic, space group P2/c with a=1.928 0(16) nm, b=1.297 0(11) nm, c=2.126 4(18) nm, V=5.242 2(8) nm³, Z=2, M_r=2 347.36, D_c=1.487 g·cm^-3, μ=0.659 mm^-1, F(000)=2 400, R_int=0.043 7, R=0.052 3, wR=0.118 6. The Mn atoms are octahed-rally coordinated by two O atoms of two ligands and four N atoms of two 1,10-phenanthroline molecules. The carboxyl group coordinates to Mn(Ⅱ) in the bridging bidentate mode. CCDC: 675520.