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.     

二聚体有机锡配合物{[n-Bu2Sn(O2CCH2CS2NC4H8)]2O}2的合成，表征及晶体结构(英)

The title compound, {[n-Bu₂Sn(O₂CCH₂CS₂NC₄H₈)]₂O}₂, has been synthesized by the reaction of (tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in 1∶1 molar ratio. The complex has been characterized by elemental analysis, IR and NMR. The crystal structure of it has been determined by X-ray single crystal diffraction. And the results showed that the crystal belongs to triclinic system with space group P1 and some crystal parameters: a=1.220 2(9) nm, b=1.315 8(10) nm, c=1.380 4(10) nm, α=111.215(9)°， β=99.357(9)°， γ=96.075(10)°, V=2.006(2) nm³, Z=1, F(000)=908, μ=1.489 mm^-1, D_c=1.474 g·cm^-3, R₁=0.037 5, wR₂=0.0839. The complex has a centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom which has a distorted octahedron. Each of the endo-cyclic tin atoms exhibits a distorted trigonal bipyramid coordination geometry with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are bidentate and connecting to each of exo-cyclic tin atoms by using both oxygen atoms, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom only. CCDC: 220513.     

弱桥联二聚体丙酮酸异烟酰腙合锡(Ⅳ)配合物[(p-CNC6H4CH2)2Sn(C9H7N3O3)(H2O)]2的合成、表征和晶体结构

Diorganotin(Ⅳ) compound [(p-CNC₆H₄CH₂)₂Sn(C₉H₇N₃O₃)(H₂O)]₂ was synthesized by the reaction of tri-p-cyanobenzyltin chloride with Schiff base ligand pyruvic acid isonicotinyl hydrazone. The compound was characterized by elemental analysis, IR, ¹H NMR. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic space group C2/c, with a=3.143 1(3) nm, b=0.989 99(10) nm, c=1.785 68(18) nm, β=114.908 0(13)°, V=5.039 6(9) nm³, Z=4, μ=1.054 mm^-1, D_c=1.513 Mg·m^-3, F(000)=2 304, R=0.042 8, wR=0.090 3, GOF=0.997. In this compound, the Sn atom exists in a distorted octahedral coordination environment in which one water molecule, one tridentate pyruvic acid isonicotinyl hydrazone ligand, and two trans p-cyanobenzyl groups coordinate to each Sn center, the angle of the axial C10-Sn1-C18 is 166.1(2)°. Two molecules form a weak-bridged dimmer with weak interactions of Sn…O bonding and hydrogen bonds. CCDC: 270796.     

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.     

三苯基锡(Ⅳ)N-烃基哌嗪氨荒酸酯配合物的合成、表征、性质和Ph3SnS2CN(C2H4)2NCH3的晶体结构

Six triphenyltin(Ⅳ)N-alkylpiperazinyldithiocarbamates have been synthesized by the reaction of triphenyltin chloride with N-alkylpiperazinyldithiocarbamates and characterized by elemental analysis, UV, IR and ¹H NMR. The crystal structure of Ph₃SnS₂CN(C₂H₄)₂NCH₃(1) has been determined by X-ray single crystal diffraction. The crystal of the compound 1 belongs to triclinic with space group P1, a=1.033 56(18) nm, b=1.148 8(2) nm, c=1.191 6(2) nm, α=66.282(2)°, β=78.756(2)°, γ=67.476(2)°， Z=2, V=1.195 2(4) nm³, D_c=1.460 g·cm^-3, μ=1.256 mm^-1, R=0.025 1, wR=0.058 3. The structure shows a distorted tigonal bipyramidal configuration with five-coordination for the central tin atom. CCDC: 240375.     

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.     

夹层化合物四氯合镉(Ⅱ)酸4-硝基苯铵的合成与结构

The title compound was prepared by the solid state reaction of stoichiometric amounts of CdCl₂·H₂O and 4-nitroaniline . The crystal used for X-ray analysis was obtained by slow evaporation of an ethanol-aqueous solution of the solid state reaction at room temperature. The structure of compound was characterized by X-ray diffraction analysis. The crystal belongs to orthorhombic, space group Pbca, a=0.77864(7)nm,b=0.72547(6)nm,c=3.3126(2)nm,Z=4,V=1.8712(3)nm³,D_c=1.890g·cm^-3,μ=1.763mm^-1, F(000)=1048,R=0.0300,wR=0.0697. The title compound is a typical two-dimensional organic intercalated compound. The inorganic layers of the compound are formed by CdCl₆ octahedra sharing corner Cl atoms (i.e. catena-poly[dihlorocadmium-di-μ-chloro]). The organic ammonium cations are intercalated between every two metal-halogen layers and formed the organic layers of the compound through hydrogen bonding.     

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.     

有机锡配合物[(o-Cl-PhCH2)2Sn(OCOC9H6N)2]·2(C6H6)的合成和晶体结构研究

A novel organotin complex [(o-Cl-PhCH₂)₂Sn(OCOC₉H₆N)₂]·2(C₆H₆) has been synthesized. The crystal structures of the complex was determined by X-ray diffraction.The crystal belongs to monoclinic space group P2/c with a=1.322(4) nm, b=1.035(3) nm, c=1.498(4) nm, β=101.62(4)°, V=2.008(10) nm^{3Z=2, D_x=1.440 g·cm-3, μ(MoKα)=8.16 cm-1, F(000)=884, R₁=0.058 6, wR=0.099 1. The bond length Sn-C is 0.217 2(7) nm, The Sn-O is 0.208 9(6) nm, The Sn-N is 0.257 5(8) nm. This compound is monomeric, with six-coordinated tin atom in a distorted octahedron geometry. CCDC: 243549.}     

鼓形有机锡氧簇合物[nBuSn(O)(NNA)]6的合成、晶体结构及生物活性

The title complex [ⁿBuSn(O)(NNA)]₆(1), was synthesized by the reaction of ⁿBuSn(O)OH with naphthalene acetic acid in 1∶1 molar radio, where HNNA=naphthalene acetic acid. The complex was characterized by IR, ¹H NMR spectra and elemental analysis. The crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic system with space group P2₁/n. The crystal data are: a=2.647 1(5) nm, b=1.412 9(3) nm, c=2.805 7(6) nm, β=116.185(3)°, Z=4, V=9.417(3) nm³, D_c=1.595 g·cm^-3, μ=1.632 mm^-1, F(000)=4 512, R₁=0.050 3, wR₂=0.131 2. The structure shows a distorted octahedral configuration with six-coordination for the central tin atom. The bioactivity test shows that the Sn(Ⅳ) complex has selective antibacterial property. CCDC: 752497.     

半开口立方烷型簇合物[WOS3Cu3I(4-bpy)3]·0.25EtOH的合成及晶体结构(4-bpy=4-叔丁基吡啶)

Reaction of (NH₄)₂[WOS₃] with CuI and 4-tert-butylpyridine (4-bpy) in EtOH afforded a tetranuclear neutral cluster [WOS₃Cu₃I(4-bpy)₃]·0.25EtOH. This compound was characterized by elementary analysis, IR, ¹H NMR, TGA, and its crystal structure was determined by X-ray single crystal diffraction. It belongs to monoclinic, space group P2/c with a=2.220 9(2) nm, b=1.364 66(11) nm, c=2.490 6(2) nm, β=104.953(2)°, V=7.292 9(12) nm³, Z=4. The title compound may be viewed as having a half-open cubane-like structure in which three [Cu(4-bpy)]⁺ units are linked by a triply-bridging [WOS₃]^2- unit and a doubly-bridging iodine atom. CCDC: 266412.     

新配合物[Cd(H2O)2(phen)2](PA)2的制备及晶体结构

The new compound was prepared by the reaction of Cd(ClO₄)₂·6H₂O,1,10-phenanthroline (phen)and picric acid (HPA)(ratio 1∶3∶2) in methanol-aqueous solution refluxing for 4 hours. The crystals used for X-ray analysis was obtained by slow evaporation of the solution at room temperature. The crystal compound is in triclinic with space group with a=1.1363(4)nm,b=1.2593(2)nm,c=1.3972(4)nm,α=93.97(2)?,β=100.84(3)?,γ=106.29(2)?,Z=2,V=1.8690(9)nm³,D_c=1.715g·cm^-3, μ(MoKα)=0.677mm^-1,F(000)=972,R=0.0907,wR=0.2240. In the complex, the Cd(Ⅱ) cation is octahedrally coordinated to two 1,10-phenanthroline ligands and two water molecules in cis disposition. As outer sphere, picrate anions are combined with inner by hydrogen bond and static electricity interaction.     

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.     

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.     

有机锡化合物[n-Bu2Sn(OH)OS(O)2(p-ClPh)]2的合成、晶体结构和催化性能

An organotin compound, [n-Bu₂Sn(OH)OS(O)₂(p-ClPh)]₂, has been synthesized by the reaction of n-Bu₂SnO with p-ClPhSO₃H and characterized by IR, elemental analysis and X-ray diffraction single crystal structure analysis. The results show that it possesses a polymeric sheet structure with repeating 20-membered macrocycles by virtue of the bridging bidentate sulfonate groups; the crystal belongs to monoclinic, space group P2₁/c with a=1.460 72(12) nm, b=0.897 41(11) nm, c=2.896 94(14) nm, β=107.629(4)°, V=3.619 2(6) nm^-3, Z=4; all the tin atoms are six-coordinated in a distorted octahedral geometry. The compound showed the very high catalytic activity in the transesterification of dimethyl carbonate and phenol to diphenyl carbonate. CCDC: 751163.     

μ-氧-双[三(邻溴苄基)锡]的合成和结构研究

The tri(o-bromobenzyl)tin bromide was treated with aqueous solution of NaOH to formed the μ-oxygen-bis[tri(o-bromobenzyl)tin]. The crystal structures of compound was determined by X-ray diffraction. The crystal belongs to triclinic, space group with a=1.0544(4) nm, b=1.1029 (4) nm, c=1.1309 (4) nm, α =117.031(5) °, β=107.685 (6) °, γ=98.523(6) °, V=1.0506(6)nm³, Z=1, D_x=2.013g·cm^-3, μ(MoKα)=69.25cm^-1, F(000)=606, R₁=0.0524, wR₂=0.1196. In the struture the tin atom has a distorted tetrahedral geometry. CCDC: 220514.     

[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.     

配位聚合物[Mn(2，4，6-TMBA)2(H2O)3]n·2nH2O的水热合成和晶体结构

The title compound, [Mn(2,4,6-TMBA)₂(H₂O)₃]_n·2nH₂O(1), where 2,4,6-TMBA=2,4,6-trimethylbenzoic acid, was synthesized and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic, space group C2/c with a=2.929 9(6) nm, b=1.036 4(2) nm, c=8.222 04(17) nm, V=2.494 7(9) nm³, Z=4, M=471.40, D_c=1.255 g·cm^-3, μ=0.571 mm^-1, F(000)=996, R_int=0.029 4, R=0.037 6 and wR=0.094 9. The Mn atoms are octahedrally coordinated by two O atoms of two ligands and four O atoms of water. The carboxyl group coordinates to Mn(Ⅱ) in the mode of monodentate, while the O atoms of water molecules coordinates in bridging mode. The complex shows a one-dimensional chain structure bridged by water molecules. CCDC: 297750.     

[Co(HOC10H6COO)2(H2O)4]配合物的合成、晶体结构和性质研究

Complex [Co(HOC₁₀H₆COO)₂(H₂O)₄] was synthesized by reaction of hydroxy-2-naphthoic acid with CoCl₂·6H₂O. The compound was characterized by elemental analysis, IR and the structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2₁/n with a=0.675 8(2) nm, b=0.518 15(14) nm, c=2.962 9(9) nm, β=94.925(8)°. V=1.033 6(5) nm³, Z=2, D=1.624 Mg·m^-3, F(000)=522. The Co atom has an octahedron coordination geometry and was six-coordinated with two oxygen atoms from two carboxylate ligands and four oxygen atoms from four water molecules. The complex molecules were linked by different hydrogen bonds to form a 2D network. The complex has thermal stability and shows a strong fluorescent emission at 421 nm (λ_ex=342 nm). CCDC: 250903.     

离子化合物{[2-(3′-pyridyl)benzimidazoleH2]2+·[SbCl4]-·Cl-}4的水热合成、晶体结构及抑菌活性

A new ionic compound {[2-(3′-pyridyl)benzimidazoleH₂]²⁺·[SbCl₄]^-·Cl^-}₄ was synthesized by the hydrothermal reaction of o-diaminobenzene, nicotinic acid with SbCl₃ in 1∶1 HCl solution. The structure was characterized by chemical analysis, elemental analysis and IR patterns. The single crystal structure was determined by X-ray single crystal diffraction. It crystallizes in monoclinic system, space group P2₁/n with a=2.107 9(4) nm, b=1.482 0(3) nm, c=2.113 4(4) nm, β=93.44(3)°, Z=4, V=6.590(2) nm³, D_c=2.001 g·cm^-3, μ=2.480 mm^-1, F(000)=3840, R₁=0.0468, wR₂=0.1163. The single crystal structure indicates that the four chlorines coordinated to the antimony atom forms a distorted triangle bipyramid configuration together with the lone electron pair on the Sb atom. The [SbCl₄]^- to 2-(3′-pyridyl)benzimidazole cation and Cl^- by weak interaction forms the ionic crystal. It has been proved that the title compound has antibacterial activity. CCDC: 283824.