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.     

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.     

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.     

异核配合物[Co(Ⅲ)(Hdmg)2(H2O)2Mn(Ⅱ)Cl3]的合成与晶体结构

A new coordination compound Co(Ⅲ)(Hdmg)₂(H₂O)₂Mn(Ⅱ)Cl₃ was synthesized and its crystal structure was determined. The crystal data are as follows: crystal system, orthorhombic; space group, C222₁(#20); a=1.18315(3) nm, b=1.28631(5) nm, c=1.14355(2) nm, V=1.74037(9) nm³, Z=4, D_c=1.857 g·cm^-3, F(000)=980.00, μ(MoKα)=21.69 cm^-1, R₁=0.030, wR₂=0.92. The coordination geometries around Co(Ⅲ) and Mn(Ⅱ) atoms are distorted octahedral and distorted trigonal bipyramidal, respectively. The Hdmg chelates Co(Ⅲ) and bridges to two Mn(Ⅱ) atoms to form a polyheteronuclear helical structure along the c axis.     

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.     

异双桥二维镍(Ⅱ)配位聚合物 ∞2[Ni(μ-4，4′-bpy)2/2(μ-L)4/2](HL=2-indolyl-formic acid)的水热合成和晶体结构

The allo-bisbridge 2D coordination polymer _∞²[Ni(μ-4，4′-bpy)_2/2(μ-L)_4/2](HL=2-indolyl-formic acid) has been obtained by using hydrothermal synthesis, and the results of X-ray single crystal diffraction analysis show that the compound crystallizes in monoclinic system, space group C2/c (No.15) with a=2.300 2(5) nm, b=1.129 1(2) nm, c=0.974 0(2) nm, β=109.85(3)°, V=2.379 2(8) nm³, D_c=1.494 g·cm^-3, Z=4, F(000)=1 104, μ=0.860 mm^-1, R=0.032 2, wR=0.088 8. The crystal structure consists of the [Ni(μ-4,4′-bpy)_2/2(μ-L)_4/2] complex molecules, in which the Ni atom is octahedrally coordinated by two N atoms from two different 4,4′-bpy molecule ligands and four O atoms from four different L- anion ligands. TG analysis indicate that title coordination polymer possesses relatively high thermal stability. CCDC: 252833.     

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.     

配合物[Co(phen)2(m-chlorobenzoic acid)2·(H2O)]·(H2O)2的水热合成、晶体结构电化学分析

The title complex has been synthesized with m-chlorobenzoic acid, 1,10-phenanthroline and cobalt perchlorate anhydrous in the solvent mixture of water and methanol. Crystal data for this complex: triclinic, space group P1, a=0.870 7(3) nm, b=1.284 4(4) nm, c=1.692 9(5) nm; α=75.430(5)°, β=77.562(5)°, γ=86.346(5)°, V=1.789 4(9) nm³, D_c=1.456 g·cm^-3, Z=2, F(000)=806. Final GooF=1.065, R₁=0.068 4, wR₂=0.127 5. The crystal stru-cture shows that the Cobaly ion is coordinated with four nitrogen atoms from two 1,10-phenanthroline molecules and two oxygen atoms from one m-chlorobenzoic acid molecule and one water molecule respectively, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 619087.     

一维链状铁(Ⅱ)配位聚合物的合成与晶体结构

A coordination polymer, namely [Fe(DPPZ)(dipic)]_n (1) (DPPZ=dipyrido[3,2-a∶2′,3′-c]phenazine and H₂dipic=pyridine-2,6-dicarboxylic acid), has been obtained by using hydrothermal synthesis method. The crystal structure was determined by X-ray single crystal structure analysis with the following data: Monoclinic, P2₁/c, a=0.794 95(16) nm, b=3.601 1(7) nm, c=0.734 32(15) nm, β=106.07(3)°, V=2.020 0(7) nm³, Z=4, M_r=503.25, D_c=1.655 g·cm^-3, F(000)=1 024, μ(Mo Kα)=0.795 mm^-1, R=0.038 5 and wR=0.081 0. Complex 1 has octahedral coordination geometry and forms 1D zigzag coordination chains that organize into an unusual 3D supramolecular motif through noncovalent bonds, such as π-π stacking interactions and C-H…O hydrogen bonds. The result of TG analysis indicates that the title complex is stable till 290 ℃. CCDC: 716602.     

2′-(4-氟基苯亚甲基)-3，5-二羟基苯甲酰腙Ni(Ⅱ)配合物的合成、表征、晶体结构及光谱性质

In ethanol, a new mononuclear nickel(Ⅱ) complex incorporating Schiff base ligands, [NiL₂](DMF)₄ (HL=2′-(4-fluorobenzylidene)-3,5-dihydroxybenzoylhy drazide) has been synthesized and characterized by IR, UV-Vis, elemental analysis and X-ray crystal structure analysis. The single crystal structure has been determined by single-crystal X-ray diffraction structure analysis. The crystal belongs to monoclinic system, space group P2₁/c with a=1.617 3(2) nm,b=1.798 5(2) nm, c=0.737 61(10) nm, β=91.953(3)°, V=2.144 3(5) nm³, Z=2, μ=0.526 mm^-1, D_c=1.390 g·cm^-3, F(000)=940, R_int=0.105 3. In the compound nickel(Ⅱ) atom is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The complex has the centrosymmetry and the nickel(Ⅱ) ion is located in the center. CCDC: 675522.     

二茂铁甲酸(三邻氯苄基)锡配合物的合成、结构和量子化学研究

The novel complex tri(o-chlorobenzyl)tin ferrocenecarboxylate have been synthesized.The crystal structure of the complex has been determined by X-ray diffraction.The crystal belong to orthorhombic with space group Pbca with a=0.1242(5), b=1.7242(7), c=3.0583(13)nm, V=5.928(4)nm³,Z=8, D_c=1.623g·cm^-3,μ(MoKα)= 0.1631cm^-1,F(000)=2896,R₁=0.0461,wR₂=0.0931. The bond lengths of Sn-C is 0.2148(4), 0.2152(6) and 0.2176(5)nm, respectively. The Sn-O is 0.2073(4)nm. The tin atom has a distorted tetrahedral geometry. The study on title complex has been performed,with quantum chemistry calculation by means of G98W package and taking Lanl2dz basis set. The stability of the complex, some frontier molecular orbital energies, the populations of the atomic net charges in complex and composition characteristics of some frontier molecular orbitals have been investigated. CCDC: 184267.     

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.     

[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.     

配合物Cu(C15H12N2O3)(C5H5N)的合成和晶体结构

The title coordination compound with N-substituted-salicyl Schiff ligand, Cu(C₁₅H₁₂N₂O₃)(C₅H₅N), has been synthesized. The coordination compound crystallizes in orthorhombic system, space group Pbca with a=2.037 62(7) nm, b=0.698 45(2)nm, c=2.508 76(9)nm, V=3.570 4(2) nm³, Z=8, F(000)=1 688, D_c=1.529 g·cm^-3, M_r=410.91, μ=1.250 mm^-1, R=0.031 3 and wR=0.077 0. In the coordination compound, one phenolate oxygen, one carbonyl oxygen and one hydrazine nitrogen atom from the dianionic ligand N-salicylaldehyde-N′-(4-methoxybenzoyl) hydrazone and one pyridine nitrogen atom coordinate to Cu(Ⅱ) ion, forming a distorted square plane. CCDC: 218182.     

新型一维Cd(Ⅱ)配位聚合物的合成、晶体结构和光致发光性质

A new 1D chain coordination polymer [Cd(dpq)(ox)_0.5Cl]_n(1) (dpq=dipyrido[3,2-d:2′,3′-f]quinoxaline and ox=oxalate) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR and single crystal X-ray diffraction analysis. Compound 1 (CdClC₁₅H₈N₄O₂): monoclinic, space group P2₁/c, a=0.854 04(5) nm, b=2.094 90(13) nm, c=0.839 22(5) nm, Z=4, V=1.438(15) nm³, M_r=424.11, D_c=1.959 g·cm^-3, F(000)=828.0, μ=1.719 mm^-1, S=1.028, the final R=0.025 8 and wR=0.057 5. The crystal structure analysis indicates that the cadmium ion is coordinated by two oxygen atoms from a oxalate, two chelating nitrogen atoms from a dpq molecule and two Cl^- anions. The adjacent Cd(Ⅱ) ions are linked by Cl^- anions and oxalate ligands in alternate sequence to form a 1D chain coordination polymer and the adjacent chains are further connected by π-π stacking interactions to form a 2D supramolecular network. Moreover, the title compound exhibits blue emission in the solid state at room temperature. CCDC: 680748.     

镉(Ⅱ)-环丙沙星化合物的合成、晶体结构、抗菌与抗肿瘤活性

A new Cadmium(Ⅱ)-Ciprofloxacin ionic compound, (HCPFX)₂[CdCl₄]·3H₂O, is synthesized and its crystal structure is determined. The crystallography data are as follows, monoclinic, space group P2₁/c, a=1.010 39(6) nm, b=1.399 89(9) nm, c=2.822 45(18) nm, β=95.765 0(10)°, V=3.972 0(4) nm³, Z=4, D_c=1.627 g·cm^-3, F(000)=1 984. R₁=0.054 0, wR₂=0.150 3 (I>2σ(I)). In the title compound, four chloride ions are coordinated to the cadmium ion forming a slightly distorted tetrahedron. Both Ciprofloxacin and the compound were assayed against gram-positive and gram-negative bacteria by doubling dilutions method, the compound shows the same minimal inhibitory concentration (MIC) as the Ciprofloxacin against S. Aureus, M. Lutens, E. Coli and P. Aeruginosa bacteria. The inhibitory effect of the two compounds on leukemia HL-60 cell line has been measured by using MTT (Methyl-Thiazol-Tetrozolium) assay method. The results indicate that the complex has very strong inhibitory effect on HL-60 cell line. CCDC: 259367.     

配合物[Cu(o-ABA)2(2，2′-bipy)]·(H2O)的水热合成、晶体结构及电化学性质

The title complex has been synthesized by o-acetamidobenzoic acid and 2,2′-bipyridine(bipy) in the mixture solvent of water and methanol. It crystallizes(C₂₈H₂₆CuN₄O₇, M_r=594.07) in Triclinic space group P1 with a=0.805 3(4) nm, b=0.845 5(4) nm, c=2.001 8(9) nm; α=100.797(8)°, β=93.054(7)°, γ=97.297(7)°, V=1.323 9(10) nm³, D_c=1.490 g·cm^-3, Z=2, F(000)=614. R₁=0.035 9, wR₂=0.080 5. The crystal structure shows that the copper atom is coordinated with four oxygen atoms from two o-acetamidobenzoic acid and two nitrogen atoms from the 2,2′-bipyridine, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 619084.     

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.     

一维链状铜(Ⅱ)配合物的合成及晶体结构表征

The 1D-chain polymer of [Cu(Ⅱ)₃L₃(H₂O)]_n, (H₂L=3-(3,5-dichloro-2-hydroxybenzylid-eneamino)propanoic acid) has been synthesized by reaction of 3,5-dichlorosalicylaldehyde, β-alamine and copper nitrate in ethanol solution. The crystal structure was determined by X-ray diffraction method. The crystal structure belongs to mono-clinic system with space group C2/c and cell parameters: a=3.853 7(3) nm, b=0.777 38(18) nm, c=2.656 36(2) nm, β=116.924(2)° and V=7.095 4(17) nm³, M_r=998.85, Z=8, D_c=1.870 g·cm^-3 and F(000)=3 992. The two Cu(Ⅱ) atoms are coordinated with four atoms from Schiff base, and another one is coordinated with five atoms. The square bridging links three metal centers through a novel μ-4,4,5 coordination model, which is further assembled into 1D chain coordination polymer. The 1D chain is further constructed a 3D network by strong O-H…O and C-H…O hydrogen bonds. The coordination polymer presents a good thermal stable property through the thermal analysis. CCDC: 679005.     

水合二(对叔丁基苄基)二氯化锡的合成及晶体结构

The organotin hydration di(p-tert-butylbenzyl)tin dichloride has been synthesized. The crystal structure of complex has been determined by X-ray diffraction. The crystal belongs to orthorhombic space group Pmma with a=1.108 4(2) nm, b=3.492 0(7) nm, c=0.626 36(12) nm, V=2.424 3(8) nm³, Z=4, D_c=1.376 g·cm^-3, μ(Mo Kα)=12.82 cm^-1, F(000)=1 024, R₁=0.085 9, wR=0.225 7. The bond lengths of Sn-Cl are 0.236 0(2) nm and 0.250 8(4) nm, the Sn-C is 0.212 1(11) nm, the Sn-O is 0.233 2(12) nm. The tin rendered five-coordinate in a distorted trigonal bipyramidal configuration. CCDC: 648618.