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1.
以4-甲酰基-2,2,5,5-四甲基四氢呋喃-3-酮和间甲基苯胺为原料,经缩合反应制得配体(Z)-4-[(间甲苯胺基)亚甲基]-2,2,5,5-四甲基二氢呋喃-3(2H)-酮(L);以Cu(CH_3COO)_2为铜源,L经配位反应合成了一个新型的铜(Ⅱ)配合物[Cu(L)_2]_n(I),其结构经FT-IR,X-射线单晶衍射和元素分析表征。I属单斜晶系,P2(1)/c空间群,晶胞参数a=11.361 3(19)?,b=24.564(4)?,c=12.026(2)?,α=γ=90°,β=110.452(3)°,V=3 144.6(9)?~3,Dc=1.226 g·cm~(-3),Z=4,R_1=0.051 5,wR_2=0.113 2。  相似文献   

2.
Two coordination polymers based on the mixed ligands of biphenyl-3,3?-disul-fonyl-4,4?-dicarboxylate(BPDSDC4–)and 2,2?-bipyridine(2,2?-bpy),{[Cd(BPDSDC)0.5(2,2?-bpy)(H2O)]·(H2O)}n(1)and{[Cd(BPDSDC)0.5(2,2?-bpy)2]·(H2O)}n(2)were synthesized.Both compounds crystallize in the monoclinic system,space group P21/n.For 1,a=7.5737(2),b=17.4284(5),c=13.5982(5)?,β=90.788(3)°,V=1794.76(10)?^3,Z=4,C17H15N2O7SCd,Mr=503.77,Dc=1.864 g/cm^3,μ=1.378 mm^?1,F(000)=1004,the final R=0.0299 and wR=0.0644 for 3137 observed reflections with I>2s(I).For 2,a=13.3097(2),b=10.66240(10),c=17.6583(3)?,β=91.779(2)°,V=2504.74(6)?^3,Z=4,C27H21N4O6SCd,Mr=641.94,Dc=1.702 g/cm^3,μ=1.008 mm^?1,F(000)=1292,the final R=0.0244 and wR=0.0583 for 4594 observed reflections with I>2s(I).The Cd(II)atoms in both compounds are six-coordinated.In 1,the Cd(2,2?-bpy)units are connected by BPDSDC4–ligands to generate a one-dimensional(1D)ribbon structure.The 1D ribbons are linked by the hydrogen bonds and π···π interactions to give a three-dimensional(3D)structure.In compound 2,the Cd(2,2?-bpy)2 units are linked by the BPDSDC^4–ligands to form a 1D chain.Compounds 1 and 2 show luminescent emissions.  相似文献   

3.
在甲醇溶液中,5-氯水杨醛和8-羟基喹啉乙酰肼经缩合反应合成了新化合物--一水合(E)-N'-(5-氯-2-羟基苯亚甲基)-2-(8-羟基喹啉基)-乙酰肼Schiff碱(1),其结构经1H NMR,IR,元素分析和X-射线单晶衍射表征.1属正交晶系,P2_12_12_1空间群,晶胞参数:a=4.748(5) (A),b=15.818(14) (A),c=22.802(2) (A),α=β=γ=90.00 °,V=1 712.0(3) (A)~3,Z=4,Dc=1.450 g·cm~(-3),μ=0.253 mm~(-1),F(000) =776,R_1=0.072 5,wR_2=0.102.1通过氢键相互作用,连接成一维无限链结构.  相似文献   

4.
An organic-inorganic compound [Cu(2,2′-bpy)2][{Cu(2,2′-bpy)2}2W12O40(H2)]·4H2O (Mr = 4048.00) was prepared from the hydrothermal reaction of Na2WO4·2H2O, CuCl2·2H2O, 2,2′-bipyridine (2,2′-bpy) and H2O at 160 ℃ for 4 days. The compound crystallizes in the monoclinic system, space group P21/n with a = 18.9196(8), b = 20.4212(8), c = 21.8129(9) , β = 96.992(3)°, V = 8365.0(6) 3, Dc = 3.214 g/cm3, Z = 4, μ(MoKα) = 17.269 mm-1 and F(000) = 7324. Of the 119837 total reflections, 17315 were unique (Rint = 0.0489). The final R = 0.0385 and wR = 0.0770 for 11142 observed reflections with I > 2σ(I). Single-crystal X-ray diffraction reveals that the structure is composed of [{Cu(2,2′-bpy)2}2W12O40(H2)]2- anions, discrete [Cu(2,2′-bpy)2]2+ cations and lattice water molecules, and the anion is made up of a {W12O40(H2)}6- α-Keggin core decorated with two {Cu(2,2′-bpy)2}2+ groups through bridging oxygen atoms.  相似文献   

5.
在水热条件下,将铜金属配合物插入到铀酰有机框架化合物中,合成了两例新型铀/铜异金属杂化配合物[Cu(bipy)(UO_2)(bdc)_2·H_2O]_n(1),{[Cu(phen)(UO_2)(bdc)(bc)(H_2O)]·H_2O}_n(2)(bipy=2,2~′-联吡啶,bdc=对苯二甲酸,phen=1,10-邻菲罗琳,bc=苯甲酸),并通过X射线单晶衍射对其结构进行了表征。配合物1属于单斜晶系,P2_1/c空间群,M_r=833.99,a=7.9077(5)?,b=23.1076(13)?,c=14.6172(8)?,β=101.4180(10)°,V=2618.1(3)?~3,Z=4,D_c=2.116 g·cm~(-3),μ=7.056 mm~(-1),F(000)=3003,最终偏离因子R=0.0210,wR=0.0560。配合物2属于单斜晶系,P2/c空间群,M_r=829.99,a=7.9327(2)?,b=11.6546(3)?,c=13.8618(4)?,β=96.2230(10)°,V=1274.01(6)?~3,Z=2,D_c=2.164 g·cm~(-3),μ=7.247 mm~(-1),F(000)=786,最终偏离因子R=0.0273,wR=0.0749。在对苯二甲酸配体桥联下这两个配合物都具有三维异金属网络结构(CCDC:860177,1;CCDC:857137,2)。此外,测试了配合物1和2的固态紫外-可见吸收光谱并研究了配合物1的固态荧光性能。  相似文献   

6.
采用水热法合成了一个新的超分子化合物[PyBImH_2]·[Sn Cl6](Py BIm=2-(4-吡啶基)苯并咪唑),并用元素分析、红外光谱、荧光光谱及X射线单晶衍射对其进行了表征。化合物属于正交晶系,Pbcn空间群,晶胞参数:a=7.1468(3),b=15.0493(6),c=16.1195(8),V=1733.72(13)3,Z=4,Dc=2.025g/cm3,Mr=528.63,μ(Mo Kα)=2.395mm~(-1),F(000)=1024,R_1=0.0264,wR_2=0.0665。Sn~(4+)与6个氯离子配位,形成八面体的配位几何。配位阴离子[SnCl_6]~(2-)与阳离子[PyBImH_2]~(2+)通过氢键及π-π堆积作用形成三维超分子结构。  相似文献   

7.
用4,5-二氮芴-9-酮(dafo)、邻苯二甲酸和硝酸铜合成了二价铜的一维链状超 分子化合物[Cu(dafo)_2(H_2O)_2]-(OPA)_2(OPA=邻苯二甲酸一价阴离子),其结构 通过单晶X射线衍射法确定。该化合物是单斜晶系,空间群为P2(1)/c。晶胞参数: a = 0.71093(16)nm, b = 1.5724(4)nm, c = 1.5357(3)nm, α=90.000(5) °, β =102.220(4) °,γ=90.000(5) °, V = 1.6778(6)nm~3, Z = 2, F(000) = 814, M_r = 794.17, D_c = 1.527 g/cm~3, μ = 0.727 mm~(-1), R_1 = 0.0406, wR_2 = 0.0930.单晶结构分析表明该化合物具有一维链状结构,该结构是通过氢 键这种弱相互作用形成的。  相似文献   

8.
在水热条件下,合成了2个配位聚合物{[Mn(Hbidc)(2,2′-bpy)(H_2O)_2]·1.5H_2O}n(1)和{[Cd(Hbidc)(phen)][Cd(phen)_2Cl_2]}n(2)(H_3bidc=苯并咪唑-5,6-二羧酸,2,2′-bpy=2,2′-联吡啶,phen=菲咯啉),并通过X射线单晶衍射、红外、元素分析、X射线粉末衍射和热重对配合物结构进行了表征。配合物1是一维无限zig-zag链结构,可以通过O-H…O和N-H…O氢键的相互作用形成三维超分子结构。配合物2也是一维无限链结构。此外,测试了配合物1和2的固体紫外吸收光谱和研究了配合物2的固体荧光性能。  相似文献   

9.
本文报道了[Cu(2,2’-联吡啶)_2Cl](BF_4)配合物的合成和晶体结构。晶体属单斜晶系,空间群P2_1/n,晶胞参数为:a=10.761(1),b=12.069(1),c=16.146(3)A,β=104.7(1)°,Z=4。在CAD-4四园衍射仪上收集衍射强度数据;重原子法解出结构,并经全矩阵最小二乘法修正结构,最后的偏离因子R=0.05,R_W=0.058。 结构测定得出[Cu(2、2’-bpy)_2Cl]~+配阳离子中的Cu原子为五配位的,它是由两个2,2’-联吡啶上的4个N原子和1个Cl原子配位而成。CuN_4Cl配位球略有畸变的三方双锥的构型。  相似文献   

10.
报道了一种新的杂多化合物[HN(C_2H_5)_3]_4-[Mo_3~VMo_6~(VI)V_7~(IV)O_(40)(PO_4)]·2[N(C_2H_5)_3]的合成,并用元素分析、EPR、IR谱、及X--射线单晶衍射等手段进行了表征。结果表明,该杂多酸盐属于单斜晶系,空间群P21/n,a=14.0841(3),b=14.2505(3),c=19.6089(3)?b=94.213(1),V=3925.0(1)?,Z=2,Dc=2.171g/cm3,Mr=2566.18,m=2.284mm-1,F(000)=2516,R=0.0477,wR=0.0945.杂多阴离子是1个16金属笼状物,笼中心包含1个PO4四面体客体。  相似文献   

11.
以Co(ClO_4)_2·6H_2O/Cu(ClO_4)_2·6H_2O、1,4-双(咪唑基-1-基)丁烷(bib)/1,4-双(咪唑基-1-基)苯(bix)和4,4-(1,3-苯基双(亚甲基氧基))二苯甲酸(H_2pmda)为原料,在水热条件下反应,得到了2个配合物{[Co(bib)_3](ClO_4)_2}_n(1)和{[Cu_3(bix)_(4.5)](ClO_4)_3}_n(2)(H_2pmda未参与反应),对它们进行了元素分析、红外光谱、荧光光谱、单晶和粉末X射线衍射表征。配合物1属于三方晶系,R空间群,a=b=1.39337(5)nm,c=1.74054(13)nm,V=2.9265(3)nm~3,M_r=828.59,D_c=1.410g·cm~(-3),F(000)=1293,μ=0.639mm~(-1),Z=3,R_1=0.0611,wR_2=0.1937(I(2σ(I))。配合物2也属于三方晶系,P空间群,a=b=2.33441(15)nm,c=0.71511(9)nm,V=3.3749(5)nm~3,M_r=1561.28,D_c=1.536g·cm~(-3),F(000)=1602,μ=1.131mm~(-1),Z=2,R_1=0.0439,wR_2=0.1090(I(2σ(I))。单晶结构分析表明配合物1为含有36元环的二维网状结构,配合物2为含有84元环的二维网状结构,并通过氢键或π-π堆积使它们扩展成超分子结构。此外,还研究了2个配合物的荧光性质。  相似文献   

12.
用硫酸钴、4,4'-联吡啶和2-磺酸基乙基膦酸合成了一个新颖的钴化合物:[Co_2(H_2O)_8(C_(10)H_8N_2)_2]·(HO_3PCH_2CH_2SO_3)(SO_4)(H_2O)_4,并对其进行了红外.元素分析、热重测试,通过单晶衍射仪测定了其晶体结构.结果表明,配合物属单斜晶系C2/c空间群,分子式为C_(22)H_(45)Co_2N_4O_(22)PS_2,分子量为930.57,晶胞参数为a=19.8456(18),b=11.2957(10),c=34.719(3)(A),β=106.095(3)°,晶胞体积为7477.9(12)(A)~3,Z=8,Dc=1.653 g/cm~3,F(000)=3856,μ=1.131 mm~(-1),最终残差因子R_1=0.0726,wR_2= 0.1719(相对于5612个I>2σ(I)的可观测衍射点).在这个化合物中,二齿配体4,4'-联吡啶把Co(II)桥连成[Co(4,4'-bipy)]~(2+)链.化合物中的[Co(4,4'-bipy)]~(2+)链有三个不同的朝向.2-磺酸基乙基膦酸没有参与配位而是做为一个有机模板剂填充在[Co(4,4'-bipy)]~(2+)链形成的空隙中.  相似文献   

13.
通过溶剂热技术,制得一种新型的Cd~(2+)配合物[Cd(L)_2(ba)_2]_2(1,L=4'-(4-甲基苯)-4,2':6',4″-三联吡啶,Hba=苯甲酸),其结构经IR,元素分析和单晶射线衍射表征。1属单斜晶系,空间群为P2_1/c,晶胞参数a=1.095 5(2)nm,b=1.404 1(3)nm,c=3.045 5(8)nm,β=103.37(3)°,V=4 557.6(18)3,D_c=1.459g·cm~(-3),Z=2,R_1=0.045 5,wR_2=0.094 0[I2σ(I)]。结构分析表明:1为零维双核结构,通过π…π堆积作用拓展为二维层状超分子。  相似文献   

14.
Two novel compounds, {[Co2(epda)2(4,4-bpy)(H2O)2]·3H2O}n1 and {[Co2(epda)2(bpe)(H2O)2]3H2O}n2(H2epda=5-ethyl-pyridine-2,3-dicarboxylic acid, 4,4’-bpy=4,4’-bipyridine and bpe=1,2-di(4-pyridyl)ethylene) were solvothermally synthesized and characterized by elemental analysis, IR spectroscopy, therm ogravimetric analysis (TGA), and singlecrystal X-ray diffraction. Complex 1 is of monoclinic system, space group P21/c with a=13.344(5), b=14.724(5), c=8.267(3), β=105.840(4)°, V=1562.5(10)3, Dc=1.480 g/cm3, Mr=375.19, Z=4, F(000)=712, μ=1.121 mm-1, the final R=0.0512 and wR=0.1260 for 2890 observed reflections with I>2σ(I). 2 belongs to the monoclinic system, space group P21/c with a=14.224(4), b=14.726(4), c=8.287(2), β=99.696(4)°, V=1711.1(9)3 , Dc=1.402g/cm3, Mr=388.21, Z=4, F(000)=740, μ=1.027 mm-1 , the final R=0.0354 and wR=0.0862 for 12237 observed reflections with I>2σ(I). Both complexes present intimately related structures featuring infinite Co-carboxylate layers of [CoⅡ(epda)(H2O)]n pillared by 4,4’-bpy (or bpe) molecule to produce the microporous frameworks, unambiguously indicating that pore dimensions of the framework are regulated by the N,N’-donor pillars.  相似文献   

15.
标题化合物[Cu(phen)2Cl](PA)由CuCl2*2H2O、邻菲咯啉(phen)、苦味酸(HPA)经水热反应得到.用元素分析、UV-Vis、IR及X-射线衍射法表征.晶体结构用直接法解出,并用全矩阵最小二乘法进行修正.化学计量式C30H18ClCuN7O7,Mr=687.51,晶体属于单斜晶系,空间群P1(#2),晶胞参数a=7.5002(15),b=11.885(2),c=15.738(3)?,α=91.702(4)、β=90.357(4)、γ=104.294(4)°,Z=1,Dc=1.680mg/m3,F(000)=698,偏离因子R=0.0591,wR=0.1539,共收集2921个衍射点(I>2σ(I)).一个结构单元中包含两个分子,分子内通过氢键和库仑力把配合物和三硝基苯酚连在一起,分子间通过氢键和π-π相互作用堆积成二维层状结构.4个N1个Cl与Cu原子以三角双锥配位.  相似文献   

16.
在常规水浴条件下成功合成了一例基于单缺位Dawson型二聚的多酸基稀土衍生物[TMA]_8[Tb(H_2O)_8]H_3[Tb(H_2O)_2P_2W_(17)O_(61)]_2·49H_2O (1),并对其进行了红外、X射线单晶衍射等结构表征以及荧光性能研究.X射线单晶衍射结构分析表明,该化合物属于三斜晶系,P-1空间群.其晶胞参数为a=1.313 76(3)nm,b=1.814 70(5) nm,c=1.990 26(6) nm,α=93.549 0°,β=97.273 0(10)°,γ=96.656 0(10)°,Z=1,Mr=10 461.62,V=4.660 9(2) nm~3,μ=22.528 mm~(-1),R_1=0.033 7,wR_2=0.067 0 [I>2σ(I)].此外,化合物1具有Tb~(3+)离子本征荧光发射峰.  相似文献   

17.
Two coordination polymers, namely {[Co(L)(H2O)]·H2O}n(1) and [Mn(L)(phen)]n(2, H2L = 5-(pyridin-4-yl)isophthalic acid, phen = 1,10-phenanthroline), have been hydrothermally synthesized and characterized by elemental analysis, IR, TG, magnetic properties, and single-crystal X-ray diffraction. 1 belongs to the triclinic system, space group P1 with a = 7.2188(7), b = 10.0835(8), c = 10.2069(7) ?, α = 113.713(7), β = 99.490(7), γ = 104.516(8)o, V = 628.24(9) ?3, C13H11NCoO6, Mr = 336.16, Z = 2, Dc = 1.777 Mg/m3, μ(MoKα) = 1.395 mm–1, F(000) = 342, S = 1.041, the final R = 0.0381 and wR = 0.0819 for 3744 observed reflections(I 2σ(I)) and R = 0.0448 and wR = 0.0874 for all data. 2 belongs to the monoclinic system, space group P2/c with a = 12.9185(3), b = 10.4343(2), c = 31.7650(6)?, β = 101.282(2)o, V = 4199.08(13)?3, C50H30N6Mn2O8, Mr = 952.68, Z = 4, Dc = 1.507 Mg/m3, μ(MoKα) = 5.447 mm–1, F(000) = 1944, S = 1.128, the final R = 0.1003 and wR = 0.1052 for 8247 observed reflections(I 2σ(I)) and R = 0.2595 and wR = 0.2625 for all data. Single-crystal X-ray diffraction studies show that compound 1 features a 2D sheet structure based on a dicobalt(II) subunit, which is further extended into a 3D metal-organic supramolecular framework by O–H···O hydrogen bond. Compound 2 also possesses a 2D sheet, which is held together into a 3D supramolecular architecture via C–H···O hydrogen bond and π-π stacking interactions. Magnetic studies for compound 2 show antiferromagnetic coupling between the adjacent metal centers, with J = –11.8 cm–1 and g = 2.12 for 2.  相似文献   

18.
Dibenzoyl peroxide undergoes oxidative addition on metallic copperpowder with 2,2′-bipyridine(or imidazole)in a mixed solvent(methanol andtetrahydrofuran),and affords the Cu(Ⅱ)complexes-[Cu(Ce(C_6H_5COO)_2(2,2'-bipy)]H_2O(1)and[Cu(C_6H_5COO)_2(C_3H_4N_2)_2](2).The structure was solved by direct methodsand Fourier synthesis.C_(24)H_(20)N_2O_5Cu (1),Mr=479.78,space group P2(1)/c,a=6.986(7),b=18.833(I),c=17.021(3),α=γ=90°,Z=4,V=2218.1~3,Dc=1.443g/cm\+3,R=0.055Rw=0.062.Complex(2),C_(20)H_(18)N_4O_4Cu(2),Mr=441.74,space group P2(1)/n,a=8.699(4),b=9.840(6),c=12.399(5),α=γ=90°,β=100.8°,Z=4,V=1010.9~3,Dc=1.654g/cm\+3,R=0.055,Rw=0.062.  相似文献   

19.
赵恒武  李斌 《结构化学》2012,31(1):61-66
Hydrothermal reactions between a new flexible multicarboxylate ligand of 3-(2-carboxy-phenoxy)-benzoic acid(H2L) and transitional metal cations of M2+(M = Cu2+,Ni2+) in the presence of the secondary ligands of 1,10-phenanthroline(phen),2,2'-bipyridine(2,2?-bpy),and 4,4'-bipyridine(4,4'-bpy) afford two novel coordination polymers Ni2(H2O)2L2(phen)(μ-4,4'-bpy)(1) and CuIIL(2,2'-bpy)(2).Both compounds were characterized by X-ray crystallography.Crystal data of 1:C31H24N3NiO7,Mr = 609.24,monoclinic,space group P21/c,a = 17.560(8),b = 10.528(5),c = 30.613(15) ,V = 5659(5) 3,Z = 4,Dc = 1.430 g/cm3,F(000) = 502,μ = 0.739 mm-1,R = 0.0902,wR = 0.1346(I > 2σ(I)),S = 1.002.Crystal data of 2:C24H16CuN2O5,Mr = 475.93,monoclinic,space group P21/n,a = 9.8904(13),b = 11.0782(16),c = 18.321(3) ,β = 11.0782(16)°,V = 1993.8(5) 3,Z = 4,Dc = 1.585 g/cm3,F(000) = 972,μ = 1.137 mm-1,R = 0.0433,wR = 0.0723(I > 2σ(I)) and S = 1.004.Compound 1 displays a one-dimensional(1D) zigzag chain structure constructed from phen ligands and the deprotonated ligands of L2-,which further forms a ladder-shaped supramolecular architecture via the bridge of 4,4'-bpy ligand.Complex 2 also possesses a ladder-shaped architecture based on the dinuclear CuII units.  相似文献   

20.
A new 4-chlorobenzoic acid bridge Co(Ⅱ) complex [Co2(2,2(')-bpy)2(μ-L)2(L)2(μ- H2O)] (HL = 4-chlorobenzoic acid) has been obtained by hydrothermal synthesis, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group C2/c with a = 22.537(5), b = 16.212(3),c = 15.306(3)(A), β= 124.37(3)°, V = 4616.1(16) (A)3, Mr = 1070.45, Dc = 1.540 g/cm3, Z = 4, μ = 1.012 mm-1, F(000) = 2176, the final R = 0.0338 and Wr = 0.0810. The title complex is composed of dinuclear [Co2(2,2(')-bpy)2(μ-L)2(L)2(μ-H2O)] molecules. Each Co(Ⅱ) atom is coordinated by two nitrogen atoms from one 2,2'-bipyridine ligand, three oxygen atoms from three 4-chlorobenzoic ions and another oxygen atom from one water molecule. The two Co(Ⅱ) atoms are connected by two 4-chlorobenzoic ions and one bridged water molecule. The dinuclear molecules are interlinked by hydrogen bond and π-π stacking interactions into a three-dimensional supramolecular network.  相似文献   

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