环状二核铜配合物[Cu(nphth)(phen)(H2O)]2·2H2O的水热合成与晶体结构

在水热反应条件下,合成了一个新配合物,[Cu(nphth)(phen)(H₂O)]₂·2H₂O(nphth=3-硝基邻苯二甲酸阴离子,phen=邻菲 咯啉),经元素分析、红外、热重、单晶衍射表征了配合物。该配合物为单斜晶系,空间群P2₁/n,结构参数：a=0.999 8(1) nm,b=1.044 5(1) nm,c=1.820 6(1) nm,β=91.423(1)°,V=1.900 7(2) nm³,Z=2,R=0.039 4,wR=0.096 5。结构分析表明,配合物为分立环状二核结构,并通过分子间氢键和π-π作用扩展为二维超分子网络结构。     

[Mn(H2O)(phen)2(PAc)](ClO4)的合成、红外光谱及晶体结构

The complex [Mn(H₂O)(phen)₂(PAc)](ClO₄) was synthesized and investigated by elemental analysis, molar conductivity, IR spectrum and X-ray diffraction methods, where phen=1,10-phenanthroline and PAc=phenylac-etate group. The complex crystallizes in the triclinic space group,P1 , with a=0.9289(2)nm,b=1.2425(2)nm,c=1.4791(3)nm,α=114.34(3)°,β=91.25(3)°,γ=104.65(1)°,V=1.4893(4)nm³,Z=2,F(000)=686,D_c=1.489g·cm^-3,μ=0.589mm^-1. The Mn(Ⅱ) ion has a six-coordinate distorted-octahedral geometry with the four nitrogen atoms of two phen ligands,a coordinated-water oxygen atom, and a carboxylate oxygen atom of PAc^-. There is π-π stacking interaction between two phen rings from two neighbor molecules.     

[Co(ptma)(amp)Cl]2+体系的一反式经式异构体(m3[ZnCl4]·0.5H2O)的晶体结构

在合成[Co(bpma)(tn)Cl]²⁺体系配合物的实验中,得到[Co(ptma)(amp)Cl]²⁺体系的一反式(ptma中仲胺上的氢相对于Cl)经式异构体(m3[ZnCl₄]·0.5H₂O),其中bpma=N,N′-二(2-吡啶基甲基)胺,tn=1,3丙二胺,ptma=N-(2-吡啶基甲基)丙二胺,amp=2-(氨基甲基)吡啶。此配合物异构体构型选择性形成的原因可能主要是其结构中配体间C-H…π相互作用使之更稳定的结果。利用单晶X-射线衍射法测定的晶体学参数:单斜晶系,空间群C2/c,a=1.55978(19)nm,b=1.33324(16)nm,c=2.2077(3)nm,β=94.832(3)°,V=4.5748(10)nm³,D_c=1.696g·cm^-3,Z=8,F₀₀₀=2360,μ(MoKα)=23.72cm^-1,R=0.0475,R_w=0.1204。配合物离子中Co³⁺为六配位。晶胞中含8个配合物阳离子,8个[ZnCl₄]^2-阴离子及4个水分子,对映体的比例为1∶1。     

[Cd(HO-BDC)(phen)·H2O]n的合成和晶体结构研究

A novel coordination ploymer [Cd(HO-BDC)(phen)·H₂O]_n (where HO-BDC is 5-Hydroxyisophthalic acid and phen is 1,10-phenanthroline) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2/c, with a=0.876 4(2) nm, b=1.233 0(3) nm, c=1.761 2(4) nm, β=109.152(9)°, V=1.797 8(7) nm³, Z=4, M_r=490.73, D_c=1.813 g·cm^-3, F(000)=976, μ=1.258 mm^-1, the final R=0.043 8 and wR=0.098 9 for 2 880 observed reflections with I>2σ(I). The structural analysis shows that the complex has a one-dimensional chain structure. CCDC: 609770.     

二聚体[Ni(TSSB)(Phen)(H2O)]·4H2O的合成、表征、晶体结构及热分解研究

The new compound, [Ni(TSSB)(Phen)(H₂O)]·4H₂O (TSSB=Taurine Salicylic Schiff Base, phen=O-Phenanthroline) has been synthesized and characterized by IR, elemental analysis and X-ray diffraction. The compound crystal data: triclinic, space group P1, a=1.049 7(2), b=1.122 5(2), c=2.384 3(4) nm, α=87.676(3)°, β=82.957(3)°, γ=62.924(3)°; V=2.482 3(7) nm³, Z=4; D_c=1.488 g·cm^-3, μ=0.920 mm^-1, F(000)=1 160, Goof=1.032, (Δρ)_max=899 e·nm^-3, (Δρ)_min=-624 e·nm^-3. The compound is a dimmer. In the complex, two Ni(Ⅱ) were coordinated by three oxygen atoms and three nitrogen atoms while the O atoms of Ac^- groups did not coordinate. The Ni(Ⅱ) formed a distorted octahedron geometry. The compound is an three dimensional net connecting with hydrogen bonding. CCDC: 275474.     

配合物[CdCl(HL)(dpp)(H2O)]n·nH2O的合成、晶体结构与荧光性能研究

Under hydrothermal condition, the reaction of 3-hydroxy-1-adamantaneacetic acid (H₂L) with CdCl₂ and 1,3-di-4-pyridylpropane (dpp) has afforded a new Cd(Ⅱ) compound, [CdCl(HL)(dpp)(H₂O)]_n·nH₂O(1), which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is triclinic, space group P1 with a=1.091 0(1) nm, b=1.131 8(1) nm, c=1.246 4(1) nm, α=88.52(1)°, β=71.34(1)°, γ=68.11(1)°, V=1.345 2(1) nm³, Z=2, M_r=591.40, F(000)=608, D_c=1.460 g·cm^-3, μ=0.947 mm^-1, the final R=0.040 1 and wR=0.104 0 for 4 950 observed reflections (I>2σ(I)). Complex 1 consists of one-dimensional chains deriving from CdCl(HL)(H₂O) units linked by dpp ligands, and lattice water molecules decorate between the chains. The O-H…O and O-H…Cl hydrogen bonds lead to the formation of a 2D layer structure. CCDC: 756099.     

一维链状镉配位聚合物[Cd(phen)(2，4，6-TMBA)2(H2O)]n的水热合成、晶体结构及热稳定性

在甲醇和水的混合溶剂中用2，4，6-三甲基苯甲酸(2，4，6-TMBA)、邻菲咯啉(phen)、高氯酸镉为原料采用水热法合成了一维链状配位聚合物Cd(phen)(2，4，6-DMBA)₂(H₂O)。该配合物晶体属四方晶系，空间群I4₁。晶体中镉原子与1个邻菲咯啉的2个N原子、2个2，4，6-三甲基苯甲酸酸根中的3个羧基氧原子及1个水分子中的氧原子配位，晶胞参数:a=2.042 5(7) nm，c=1.395 2(5) nm，V=5.820(3) nm³，D_c=1.454 g·cm^-3，Z=8，F(000)=2 608，GooF=1.064，R₁=0.034 8，wR₂=0.070 4。形成六配位的变形八面体结构。对晶体进行了热稳定性分析，结果表明:配合物在240.0 ℃以下稳定性好。     

[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[Mn(phendione)(PDC)(H2O)2]·2H2O的合成与晶体结构

The title compound [Mn(phendione)(PDC)(H₂O)₂]·2H₂O (H₂PDC=pyridine-2，6-dicarboxylic acid) has been prepared in aqueous solution and characterized by single X-ray diffraction structure determination， elemental analysis， IR spectroscopy， and thermal analyses. The compound crystallizes in Monoclinic system， space group C2/c， a=1.017 51(11) nm， b=1.483 25(11) nm， c=1.461 21(13) nm， β=109.86(10)°， V=2.074 1(3) nm³， Z=4， F(000)=1 028， μ=0.701 mm^-1， D_c=1.609 g·cm^-3， R₁=0.028 9， wR₂=0.078 8 [I>2σ(I)]. Crystal structure reveals that complex consists of one-dimensional chain framework bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in PDC^2-. Furthermore， the complexes form a three-dimensional super-molecular structure through hydrogen bonds. CCDC: 648570.     

双核镍配合物[Ni2(p-PhDTA)(2,2′-bipy)2(H2O)2]·4H2O的合成与晶体结构

A novel dinuclear complex of [Ni₂(p-PhDTA)(2,2′-bipy)₂(H₂O)₂]·4H₂O (p-PhDTA^2-=para-phenylenediamine-N,N,N′,N′-tetraacetate)has been synthesized. The complex was characterized by elemental analysis, IR spectra, thermo-analysis and X-ray diffraction. The crystal belongs to triclinic, space group P1 with a=0.976 3(7)nm, b=0.989 41(7) nm, c=1.084 29(8) nm, α=65.661 0(10)°, β=75.234 0(10)°, γ=85.616 0(10)°, Z=2, V=0.925 44(12) nm³, D_c=1.568 g·cm^-3, R₁=0.031 5, wR₂=0.081 4. In the complex, the central Ni(Ⅱ) ion is coordinated in a distorted octahedral geometry, defined by two carboxyl O atoms and one N atom from same p-PhDTA^2- group, two N atoms from 2,2′-bipyridine ligand and one water molecule. The two nickel (Ⅱ) ions are linked by p-PhDTA^2- group into a dinuclear structure and extensive hydrogen bonds link the complex into a 2D supramolecular network. CCDC: 294084.     

［La(CH2ClCOO)2(NO3)(phen)(H2O)］n的合成和晶体结构

合成了混合阴离子配合物［La(CH₂ClCOO)₂(NO₃)(phen)(H₂O)］_n。配合物经元素分析、IR、DTA-TG和UV等表征。用X射线单晶结构分析解析了标题配合物的晶体结构，三斜，空间群P1，晶胞参数为a=10.533(2)?，b=13.136(3)?，c=7.776(1)?，α=96.59(1)°，β=95.76(1)°，γ=108.42(2)°，V=1003.3(3)?³，Z=2,Dc=1.940 g/cm³, F(000)=572, μ(Mo Kα)=24.36 cm^-1。     

[Ni(dien)2]2[Mn(NCS)6]·H2O的合成、晶体结构

The crystal of [Ni(dien)₂]₂[Mn(NCS)₆]·H₂O was synthesized and the structure of its single crystal was determined by X-ray diffraction. The crystal is monoclinic system, space group P2₁/c with a=16.544(3),b=15.137(2), c=17.334(3)?, β=99.90(1)°, V=4276.3(12)?³, Z=4, D_c=1.479g·cm^-3, M_r=951.55, F(000)=1998, μ=1.489mm^-1, R=0.0399, R_w=0.0958. IR was also determined.     

双核配合物[Cu2(L-Asp)(phen)3(NO3)](NO3)·4H2O的合成及晶体结构

The new complex [Cu₂(L-Asp)(phen)₃(NO₃)](NO₃)·4H₂O (L-Asp=L-aspartic acid and phen=1,10-phenanthroline) has been synthesized and its crystal structure has been determined. The complex crystallizes in the monoclinic with space group P2₁/c, The cell parameters are: a=1.261 3(2) nm, b=1.500 8(4) nm, c=2.230 7(4) nm, β=99.55(1)°, and V=4.164 1(16) nm³，D_c=1.587 g·cm^-3. The complex contains two six-coordinated copper ions, and these two copper ions are connected together by L-aspartate to give rise to a binuclear structure. Hydrogen bonds and π-π stacking interactions are observed in the complex. CCDC: 249250.     

桥联双核配合物[(DPC)2Co2(H2O)5]·2H2O的合成与晶体结构

The new complex formulated [(DPC)₂Co₂(H₂O)₅]·2H₂O (HDPC^- is pyridine-2,6-dicarboxylate) 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=0.83850(10) nm, b=2.7386(4) nm, c=0.9610(2) nm, β=98.280 (10) °, V=2.1838(6) nm³, Z=4, D_c=1.746 g·cm^-3, μ=1.597 mm^-1. In the crystal the two Co²⁺ are in distorted octahedrons. The part of [Co(DPC)₂] possess an approximate D_2d symmetry, while the part of [OCo₍₂₎(OH₂)₅] has an approximate C₂ symmetry.     

配合物[Cu2(phen)2](SiW12O40)(H2O)7的合成、晶体结构及电化学分析

The title complex has been synthesized by the reaction of silicotungstic acid, 1,10-phenanthroline (phen) monohydrate and cupric acetate. The crystal structure belongs to triclinic system, space group P1 with a=1.158 46(15) nm, b=1.658 8(2) nm, c=1.664 4(2) nm, α=82.090(2)°, β=76.001(2)°, γ=86.531(2)°, and V=3.072 6(7) nm³, D_c=3.887 g·cm^-3, Z=2, F(000)=3 196. R₁=0.086 7, wR₂=0.185 8. The structure shows that the copper(Ⅱ) atom is coordinated with two nitrogen atoms from the one phen and three oxgygen atoms from three water, forming a distorted square-pyramid configuration The cyclic voltametric behavior of the complex is also reported. CCDC: 298807.     

镧系四元混合阴离子配合物［Pr(CH3CH2COO)2(NO3)(phen)2］合成和晶体结构

在含水溶剂、酸性环境中合成了镧系四元混合阴离子配合物［Pr(CH₃CH₂COO)₂(NO₃)(phen)］₂并解析了其晶体结构,三斜,空间群P1,a=0.9650(2) nm, b=1.2949(4) nm,c=0.8994(2)nm, α=95.37(3)°,β=111.05(2)°,γ=102.87(2)°,V=1.0037(5) nm^{3, Dc=1.758 g·cm-3, Z=1, F(000)=528, μ(MoKα)=24.64 cm-1, R=0.024, R_W=0.034。四个丙酸根呈二种配位方式,Pr3+为九配位。}     

一维链状锌配位聚合物{[Zn(H2O)2(L)(phen)]·3H2O}n的合成、晶体结构和性能研究

合成了一种锌配位聚合物{[Zn(H₂O)₂(L)(phen)]·3H₂O}_n (1), 其中, H₂L=1-氨基-8-萘酚-3, 6-二磺酸并利用元素分析、红外、紫外、荧光、热重和X-射线单晶衍射分析进行了表征。标题配合物属正交晶系, Pnma空间群, a=1.698 90(12) nm, b=0.661 88(11) nm, c=2.480 40(14) nm, V=2.789 1(5) nm³, Z=4, M_r=634.92, D_c=1.512 g·cm^-3, R=0.058 6, wR=0.121 4。标题配合物呈现一维链状结构, 链内L²-和phen配体之间存在π-π堆积作用, 链与链之间通过氢键扩展为二维超分子网络。     

配合物[1-(4′-bromo-2′-fluorobenzyl)pyridinium]2[Ni(mnt)2]和[1-(4′-bromo-2′-fluorobenzyl)pyrazinium]2[Ni(mnt)2](mnt2-=maleonitriledithiolate dianion)的合成及晶体结构

本文报道两个含双(马来二氰基二硫烯)镍(Ⅱ)配合物阴离子的离子对化合物。对阳离子为1-(4′-溴-2′-氟苄基)吡啶 盐时,生成配合物1。晶体数据:三斜晶系,空间P1群,a=0.7086(2)nm,b=1.0968(3)nm,c=1.1775(3)nm,α=69.914(5)°,β=89.495(5)°,γ=74.765(5)°,V=0.8259(4)nm³,Z=1。对阳离子为1-(4′-溴-2′-氟苄基)吡嗪鎓盐时,生成配合物2。晶体数据:单斜晶系,空间群P2₁/n,a=0.71554(17)nm,b=1.4262(3)nm,c=1.6725(4)nm,β=100.396(4)°,V=1.6788(7)nm³,Z=4。两个配合物中,阴离子为拟平面结构,镍原子均位于对称中心。变换对阳离子上的芳环种类对晶体的堆积结构产生影响。     

[Cu(PTA)(Phen)2](p-MBA)(H6O)配合物的合成、晶体结构及电化学分析

The crystal structure of the title complex with the stoichiometric formula [Cu(PTA)(Phen)₂](p-MBA)(H₆O) (Phen=1,10-phenanthroline, PTA=terephthalic acid, p-MBA=p-toluic acid) has been determined by single-crystal X-ray diffraction. The crystal (C₄₈H₄₀CuN₄O₁₀, M_r=896.38) belongs to the monoclinic space group C2/c, with the following crystallographic parameters: a=1.778 6(3) nm, b=1.912 5(3) nm, c=1.389 9(2) nm, β=114.686(2)°, V=4.295 7(12) nm³, D_c=1.386 g·cm^-3, Z=4, μ(Mo Kα)=0.574 mm^-1, F(000)=1 860, final GooF=1.019, R=0.054 0, wR=0.148 3 for 2 644 observed reflections (I>2σ(I)). The crystal structure shows that the copper(Ⅱ) ion is coordinated with two oxygen atoms from one terephthalic acid molecule and four nitrogen atoms from two 1,10-phenanthroline molecules, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 298809.     

四元混配配合物[Ce(CH2=C(CH3)-COO)2(NO3)(phen)]2的合成、表征及晶体结构

A new complex with mixed-quadriligand [Ce(CH₂=C(CH₃)-COO)₂(NO₃)(phen)]₂ has been synthesized in aqueous solution of slight acidity and characterized by elementary analysis, IR and TGA. The crystal structure determination shows that the complex belongs to triclinic, space group P1, a=9.614?, b=10.047?, c=11.821?, Z=2, α=100.88(3)°, β=106.29(3)°, γ=97.93(2)°, V=1054(5)?³, D_c=1.741g·cm^-3, F(000)=546.00, μ(MoKα)=22.06cm^-1. And the crystal is consisted of a binuclear molecule. The coordina-tion of Ce³⁺ is nine.