异双核配合物[CuCo(TS)(H2O)]·H2O的晶体结构和热分析性质研究

The single-crystal of [CuCo(TS)(H₂O)·H₂O],where TS is the schiff base N,N＇-bis(3-carboxylsalidene)trimethylenediamine, was obtained and its crystal structure was determined by the single-crystal X-ray diffraction method at room temperature. It crystallizes in the monoclinic system, space group P2₁/c. The lattice parameters are a=11.855(2)?, b=14.722(3)?, c=12.080(2)?, β=117.32(3)°, V=1879.4(7)?³ , Z=4 with R₁=0.0330. The structure is made of heterobinuclear units . The copper atom is coordinated by two nitrogens, two phenolic oxygens, in a square-planar manner. And the cobalt atom is coordinated by two phenolic oxygen atoms, two equatorial carboxyl oxygen atoms and one axial water oxygen atom, in a distorted square pyramid. Two metal atoms are bridged by two phenolic oxygens. In the crystal packing, the neutral molecules built layers. Within these layers the molecules are connected through hydrogen bonds. And the thermal property of the complex according to crystal structure is also investigated.     

双核配合物[Cu2(TS)(H2O)]·CH3OH的自组装制备和晶体结构

The binuclear complex [Cu₂(TS)(H₂O)]·CH₃OH, where TS denotes the binucleating ligand derived from the schiff base N,N′-bis(3-carboxylsalidene)trimethylenediamine, was obtained from the self-decomposition of mononuclear complex Na₂CuTS·H₂O. It crystallizes in the monoclinic system, space group P2₁/c. The lattice parameters are a=11.935(2)?,b=15.667(3)?,c=11.621(2)?,β=111.60(3)°,V=2020.2(7)?³, Z=4 with R=0.0467. The structure is made of binuclear units, in which two copper atoms are bridged by two phenolic oxygen atoms. The “inside”copper atom is coordinated by two nitrogens, two phenolic oxygens in a planar coordi-nation site, the copper atom deviates from the mean plane by 0.47?. The “outside” copper atom is five coordinated by two phenolic oxygen atoms、two equatorial carboxyl oxygen atoms and one axial water oxygen atom in a distorted tetragonal cone site, the copper atom is pulled out of the equatorial plane by 0.46?.     

含硫镍金属镍配合物[Ni(C13H7Br2NOS)2(DMF)]·(C3H7O)的合成与晶体结构

The complex, Ni[(C₁₃H₇Br₂NOS)₂(DMF)]·(C₃H₇O) (DMF=N,N′-dimethylformamide), was synthesized and characterized by the element analysis, IR and X-ray diffraction single crystal structure determination. The title complex crystallizes in monoclinic system, space group P2₁/n, with a=8.297 6(15) nm, b=12.866(2) nm, c=31.889(3) nm, β=95.024(2)°, and V=3 391.3(9) nm³, Z=4, R=0.075 2, wR=0.176 8. The nickel iron is six-coordinated by three O atoms, two N atoms, one S from the Schiff base and one O atom from DMF ligand, forming a octahedron coordination geometry. Schiff bases are bridged by the two S atoms. The molecules in the crystal are linked through intermolecular Br…Br, C-H…O, S…Br interactions. Its electrochemical property is reported. CCDC: 675768.     

配合物[Sm(o-MOBA)3(phen)·H2O]2·4H2O的合成与晶体结构

The title complex [Sm(o-MOBA)₃(phen)·H₂O]₂·4H₂O has been synthesized by the reaction of SmCl₃·6H₂O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system, space group P1 with a=1.203(10) nm, b=1.293(10) nm, c=1.306(11) nm, α=64.50(10)°, β=81.93(10)°, γ=74.81(10)°. The molecular structure shows that the Sm³⁺ ion coordinates to nine atoms. The carboxylate groups are bonded to the samarium ion in three modes: monodentate, bidentate chelating, tridentate chelating-bridging. CCDC: 603740.     

混合价三核锰配合物Mn3O(O2CCCl3)6(py)2(H2O)的合成、晶体结构及磁性

A new mixed-valence trinuclear oxo-centered manganese complex Mn₃O(O₂CCCl₃)₆(py)₂(H₂O) was prepared by the reaction of NⁿBu₄MnO₄ with Mn(OAc)₂·4H₂O, trichloroacetic acid and pyridine in absolute EtOH. The crystal structure was determined. The complex crystallizes in monoclinic, space group P2₁/c, unit cell parame-ters, a=14.951(1), b=20.791(2), c=17.882(1)?,α=γ=90°, β=102.67(1)°. Variable temperature solid state magnetic susceptibility study shows that the complex has an antiferromagnetic exchange interaction. CCDC: 183369.     

一维链状超分子化合物[Zn(dafo)2(H2O)2](NO3)2(dafo=4，5-二氮芴-9-酮)的合成、表征和晶体结构

A novel one-dimensional chain complex [Zn(dafo)₂(H₂O)₂](NO₃)₂ was synthesized. It has been characterized by IR, UV, TGA, Elemental analysis and X-ray diffraction analysis. The crystal belongs to triclinic system, P1 space group. The Crystallographic data are: a= 0.702 7(14) nm, b= 0.828 95(17) nm, c= 10.225(2) nm, α = 95.02(3)°, β = 91.45(3)°, γ = 99.85(3)°. The crystal structure data indicate that the Zn(Ⅱ) ion was coordinated with the four nitrogen atoms of two dafo and two oxygen atoms of two coordination water molecules, respectively. The complex has a one-dimensional chain structure, which is formed by hydrogen bonds.     

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.     

牛磺酸合铜螯合物的合成及晶体结构

The new chelate complex formulated [Cu(NC₂H₆SO₃)(phen)(CH₃CO₂)]·2H₂O (phen is o-phenanthroline) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to triclinic system with space group and unite cell parameters： a=7.298(1)?， b=11.573(2)?， c=11.942(3)?;α=69.77(1)°， β=80.05(1)°， γ=76.39(1)°， V=915.2(3)?³， Z=2， F(000)=478. D_c=1.680g·cm^-3， μ=1.354mm^-1， S=1.045. In the crystal structure Cu(Ⅱ) ion is five-coordinated to form a distorted tragonal cone. CCDC： 193112.     

Cu[C5H3N(CCH3=N-C6H5)2]2(PF6)2配合物的合成、晶体结构和热分解反应动力学

The title complex Cu[C₅H₃N(CCH₃=N-C₆H₅)₂]₂(PF₆)₂ has been synthesized by reaction of Schiff base C₅H₃N(CCH₃=N-C₆H₅)₂ and cupric sulfate in toluene solution. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 1041.85. The crystal structure belongs to triclinic system with space group P1 and cell parameters: a=12.6470(10)?, b=14.123(2)?, c=15.613(2)?;α=66.150(10)°,β=79.470(10)°,γ=78.290(10)°, V=2481.6(5)?³, Z=2, D_c=1.394Mg·m^-3 and F(000)=1064. The final R[I >2σ(I)]:R₁=0.0668, wR₂=0.1927; R(all data): R₁=0.1133, wR₂=0.2357. The Cu(Ⅱ) was coordinated by six nitrogen, at the same time the Cu(Ⅱ) formed a distorted octahedron, besides the angles and planes of this compound were discussed . The result of kinetics of the thermal decomposition indicated that the first step of it is 2 series chemical reactions, the function of machanism is f(a)=(1-a)², and the activation energy is 144.64E/kJ. CCDC: 180872.     

一种新的三维超分子化合物[Ni(H2O)6(fum)]·2(hmt)·4H2O的合成和晶体结构(fum=反丁烯二酸根；hmt=六次甲基四胺)

The synthesis of nickel supramolecular compound with hexamethylenetetramine and fumarate ligands is reported. The compound [Ni(H₂O)₆(fum)]·2(hmt)·4H₂O (1) (fum=fumarate; hmt=hexamethylenetetramine) were characterized by elemental analysis, crystal structure, IR. Compound 1 crystallizes in the triclinic system, space group P1, and with Z=1. Cell parameters: a=0. 934 6(1), b=0.933 8(1), c=0.938 8(2) nm, α=79.46(1)°, β=77.84(1)°, γ=61.29 6(7)°. Every metal ion has a octahedral coordination geometry formed by six oxygen atoms from six water molecules, and the relative independent components [Ni(H₂O)₆]²⁺, fumarate anions, hmt and H₂O molecules are linked together by two kinds of hydrogen bonds (O-H…O, and O-H…N) to form a three-dimensional structure. CCDC: 256355.     

[Cu(TO)2(H2O)4](PA)2的合成和晶体结构

[Cu(TO)₂(H₂O)₄](PA)₂ was prepared by mixing the aqueous solution of 1,2,4-triazol-5-one(TO) and Cu(PA)₂. The molecular structure and crystal structure of the title complex was determined by X-ray single crystal diffraction method. The crystal is triclinic, space group with a=0.7321(1)nm,b=0.7474(2)nm,c=1.3649(3)nm;α=88.65(2)°,β=85.63(1)°,γ=63.35(1)°;V=0.6655(2)nm³,Z=1. The Cu²⁺ coordinated with two TO molecule through its 2-nitrogen atom and four water molecules and showed an octahedral configuration.     

2D氢键网状Mg(Ⅱ)配合物的合成和晶体结构

The title complex [Mg(H₂O)₆]·(L)·(H₂O) [L=2-formyl-benzenesulfonate-hydrazine] was synthesized by the reaction of magnesium chloride hexahydrate with 2-formyl-benzenesulfonic acid sodium-hydrazine in the CH₃CH₂OH/H₂O. It was characterized by elemental analysis, IR and X-ray single crystal structure analysis. The crystal of the title complex [Mg(H₂O)₆]·(C₁₄H₁₂N₂O₇S₂)·(H₂O) belongs to triclinic, space group P1 with a=0.781 09(12) nm, b=0.781 27(13) nm, c=0.995 68(19) nm, α=102.054(2)°, β=92.331 0(10)°, γ=105.500(2)°, V=0.569 59(17) nm³, Z=1, D_c=1.559 Mg·m^-3, μ=0.334 mm^-1, F(000)=280, and final R₁=0.033 9, wR₂=0.091 6. The complex comprises a six-coordinated magnesium(Ⅱ) center, with a O₆ distorted octahedron coordination environment. The molecules are connected by hydrogen bonds to form two dimensional network structures. CCDC: 716601.     

[Co(3,3-tri)(amp)Cl][ZnCl4]一对邻位差向异构体的晶体结构

The crystal structures of a pair isomers of [Co(3,3-tri)(amp)Cl][ZnCl₄] (here 3,3-tri = N-(3-Aminoprop- yl)-1,3-propanediamine; amp=2-(Aminomethyl)pyridine) have been determined by single crystal X-ray diffrac-tion. They are the epimers with the only difference of the orientation of the Sec-NH proton in 3,3-tri ligand. The crystals with the anti-epimer (m1[ZnCl₄]·CH₃OH·H₂O) are monoclinic, space group C2/c with eight molecules in a unit cell of dimensions a=30.401(5)?,b=8.0469(13)?,c=18.817(3)?,β=93.346(3)°,V=4595.3(12)?³,D_c=1.708g·cm^-3,Z=8,F₀₀₀=2416,R=0.0462,R_w=0.1304. The crystals of the syn-epimer (m2[ZnCl₄]·H₂O) are triclinic, space group P1 with two molecules in a unit cell of dimensions a=8.9752(12)?,b=9.8855(12)?,c=12.6886(16)?,α=89.228(3)°,β=76.447(2)°,γ=80.428(3)°,V=1078.8(2)nm³,D_c=1.721g·cm^-3,Z=2,F₀₀₀=568,R=0.0313,R_w=0.0929. The crystal parameters, such as bond lengths and angles, are well consistent with the data of an ab initio computational result (RHF/LANL2DZ opti-mised structure). The average error for bond length is about 1.6%, only two of them in the isomer m3 (Co-N2 and Co-N4) are over 3%, (3.09% and 4.28% respectively). The errormax for bond angle is 2.52%, the bond angles with an over 2% error are only 3.6% out of all bond angles.     

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.     

[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.     

配合物[Cu(HPHAc)2(py)2](H2PHAc=苯羟乙酸，py=吡啶)的合成和晶体结构

The novel copper(Ⅱ) complex with α-hydroxyphenylacetic acid (H₂PHAc) and pyridine (py) ligands, [Cu(HPHAc)₂(py)₂], has been synthesized and characterized by elemental analysis and IR spectroscopy. Its crystal structure was determined by single crystal X-ray diffraction techniques. The crystal belongs to monoclinic with space group C2/c. The cell parameters are: a=1.712 5(3) nm, b=1.533 2(2) nm, c=0.963 42(14) nm, β=111.866(2)°, V=2.347 6(6) nm³, and D_c=1.483 Mg·m^-3, Z=4, F(000)=1 084. The structure was refined to final R₁=0.071 4, wR₂=0.166 1. The complex has a six-coordinated distorted octahedral geometry, in which copper(Ⅱ) ion coordinates with two carboxylic oxygen atoms and two hydroxyl oxygen atoms from the two α-hydroxyphenylacetic acid ligands, two nitrogen atoms from the two pyridine ligands. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 255346.     

一维链状化合物[Ag(L)]·H2O的合成、晶体结构和荧光性质

The title compound, [Ag(L)]·H₂O,1, where HL=4-(isonicotinamido)benzoic acid, was synthesized in methanol solution and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic, space group P2₁/c with a=0.571 8(8) nm, b=1.357 2(18) nm, c=1.558 0(2) nm, β=91.090(2)°, V=1.209 0(3) nm³, Z=4, D_c=2.009 g·cm^-3, F(000)=722, R_int=0.042 9, R=0.027 1, wR=0.055 6. In complex 1, the Ag atoms are linearly coor-dinated by one O atom and one N atom of two ligand molecules. Each L- ligand in turn uses its one carboxylate group and one pyridinyl groups to connect two metal centers, then the one-dimensional (1D) chains is formed. On the other hand, the 1D chains are further connected by O1W-H1WB…O2 hydrogen bonds and Ag-O weak interactions to give a two-dimensional (2D) layer, finally, the 2D net extents to three-dimensional (3D) supramolecular framework by O1W-H1WB…O1 as well as N2-H2…O2 interactions. CCDC: 762259.     

四（1-乙烯基咪唑）二异硫氰酸镉的晶体结构和电化学性能

A complex [Cd(NCS)₂(Vim)₄] (where Vim=1-vinylimidazole) was synthesized and it′s crystal structure was determined by X-ray diffraction technique. The compound crystallizes in the Monoclinic space group P2₁/c with the parameters: a=0.858 50(17) nm, b=0.909 90(18) nm, c=1.782 3(4) nm, β=100.14(3)°, V=1.370 5(5) nm³, Z=2. In the structure, each Cd atom is coordinated by four 1-vinylimidazole ligands and a pair of monodentate isothiocyanic groups, affording a compressed octahedral CdN₆ core. The NCS^- anions are trans and four N atoms from the 1-vinylimidazole ligands define the equatorial plane. From the cyclic voltammogram measurement in H₂O, we know that the electrode reaction was a quasi-reversible process. CCDC: 630897.     

过渡金属-碱土金属铜钙四核配合物Cu2Ca2L2(H2O)6·2H2O的合成和晶体结构

The transition metal and alkaline earth metal tetranuclear complex Cu₂Ca₂L₂(H₂O)₆·2H₂O where H₄L represents the Schiff base N-3-carboxylsalicylideneglycylglycine was prepared and its crystal structure was determined by the single-crystal X-ray diffraction method at room temperature. It crystallizes in the monoclinic system, space group C2/c. The lattice parameters are a=2.128 2(2) nm, b=1.231 73(14) nm, c=1.32342(15) nm, β=93.619(2)°, M_r=939.81, D_c=1.803Mg·m^-3, F(000)=1 928, Z=4 with R₁=0.046 6. Each copper atom is coordinated by two nitrogen atoms, one carboxylate oxygen atom and one phenolic oxygen atom, in a square-planner manner. And each calcium atom is coordinated by three water oxygen atoms, three carboxylate oxygen atoms and one phenolic oxygen atom in a distorted pentagonal bipyramid. Two pentagonal bipyramids are connected by two carboxyl groups. CCDC: 239969.     

镧与β-丙氨酸配合物{[La2(β-ala)6(H2O)4](ClO4)6·H2O}n的合成及晶体结构

The complex, {[La₂(β-ala)₆(H₂O)₄](ClO₄)₆·H₂O}_n, was synthesized in aqueous solution and its crystal structure was determined by X-ray diffraction method .The crystal is triclinic with space group of .The cell pa-rameters are a=0.946(1)nm, b=1.2917(1)nm, c=2.1726(3)nm,α=76.79(1)°, β=80.85(1)°,γ=83.35(1)°, V=2.5429(5)nm³, Z=2, D_c=1.958g·cm^-3.The complex is an one-dimensional infinite chain. The coordination number of lanthanum ion is nine, forming a distorted tricapped trigonal prism.