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1.
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, Mr=591.40, F(000)=608, Dc=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.  相似文献   

2.
合成了3个超分子化合物[M(4,4′-bipy)2(H2O)4]·(4,4′-bipy)2·(3,5-diaba)2·8H2O(M=Co (1),Ni (2),Cd (3);4,4′-bipy=4,4′-联吡啶;3,5-diaba=3,5-二氨基苯甲酸阴离子),用红外光谱、元素分析及X-射线单晶衍射进行了表征。3个化合物的晶体都属于单斜晶系,空间群为P2/c。晶体学参数:化合物1:a=0.938 9(2) nm,b=0.775 1(1) nm,c=3.928 4(6) nm,β=90.14(2)°,V= 2.858 80(69) nm3,Z=4,Dc=1.397 g·cm-3,F(000)=1 266,μ=0.380 mm-1,R1=0.034 9,wR2=0.082 9;化合物2:a=0.938 3(2) nm,b=0.775 3(1) nm,c= 3.921 8(6) nm,β=90.09(1)°,V=2.852 80(68) nm3,Z=2,Dc=1.399 g·cm-3,F(000)=1 268,μ=0.420 mm-1,R1=0.036 6,wR2=0.080 5;化合物3:a=0.940 91(13) nm,b=0.778 85(11) nm,c=3.971 2(5) nm,β=90.10°,V=2.910 2(7) nm3,Z=2,Dc=1.433 g·cm-3,F(000)=1 308,μ=0.454 mm-1,R1=0.046 8,wR2=0.096 4。3,5-diaba未参与配位,在配位阳离子[M(4,4′-bipy)2(H2O)4]2+中,金属离子M(II)与来自2个4,4′-bipy的2个氮原子和4个水分子的氧原子配位,呈八面体的几何构型。分子中还存在未配位的4,4′-bipy。通过配位阳离子、游离4,4′-bipy及未配位的3,5-diaba间的丰富氢键,构建成具有三维结构的超分子化合物。  相似文献   

3.
A one-dimensional zigzag chain complex of Cd(FA)(pyim)(H2O) (1) (H2FA=4,4′-(hexafluoroisopropylid-ene)bis(benzoic acid) and pyim=2-(2-pyridyl)imidazole) was hydrothermal synthesized from Cd(NO3)2·4H2O, 4,4′-(hexafluoroisopropylidene)bis(benzoic acid) and 2-(2-pyridyl)imidazole. Single-crystal X-ray analysis revealed that the zigzag chains of 1 are linked into three-dimensional supramolecular networks by both O-H…O hydrogen-bonds and π…π stacking interactions. The crystal is of monoclinic, space group P21/n with a=0.856 34(10) nm, b=1.020 49(12) nm, c=2.809 0(3) nm, β=98.115(2)°, V=2.430 2(5) nm3, Dc=1.820 g·cm-3, Z=4, F(000)=1 320, Goof=1.009, R1=0.047 0, wR2=0.115 5. In addition, complex 1 exhibits strong photoluminescent emission at room temperature. CCDC: 733837.  相似文献   

4.
Three tin (Ⅳ) complexes with N,N-dialkyl dithiocarbamates Ph3SnS2CN(CH3)C6H5 (1),Ph3SnS2CN(C4H8NH) (2) and Sn(Cl)2(S2CNEt2)2 (3) have been synthesized. The crystal structures have been determined by X-ray sin- gle crystal diffraction. A crystal of the complex 1 is triclinic with space group P1, a=0.9485(3)nm, b=1.0491(3)nm, c=1.3631(4)nm, α=70.996(4)°, β=72.294(4)°, γ=79.609(4)°, Z=2, V=1.2168(6)nm3, Dc=1.453g·cm-3, μ=1.234mm-1, R=0.0442, wR=0.0858. A crystal of the complex 2 is monoclinic with space group P2(1)/c, a=1.2214(2)nm, b=1.1651(2)nm, c=1.5769(3)nm,β=99.039(2)°, Z=2, V=2.2162(7)nm3, Dc=1.532g·cm-3, μ=1.352mm-1, R=0.0267, wR=0.0591. A crystal of the complex 3 is triclinic with space group P1, a=0.7179(2)nm, b=0.9256(3)nm, c=1.5327(5)nm,α=93.857(4)°,β=98.992(4)°, γ=109.481(4)°, Z=2, V=0.9405(5)nm3, Dc=1.717g·cm-3, μ=2.076mm-1, R=0.0263, wR=0.0662. In the complexes 1 and 2 the tin atoms rendered five-coordination in a distorted tigonal bipyramidal structure and in the complex 3 the tin atom rendered six-coordination in a distorted octahedron structure. CCDC: 1, 179918; 2, 180024; 3, 180004.  相似文献   

5.
邓玉恒  刘娟  李宁  杨永丽  马宏伟 《化学学报》2007,65(24):2868-2874
在甲醇溶液中合成了一系列IIB过渡金属Zn(II), Cd(II)的二羟乙基二硫代氨基甲酸[(EtOH)2dtc]的配合物, 并对配合物M[(EtOH)2dtc]2L [M=Zn (1), Cd (2), L=2,2'-联吡啶; M=Zn (3), Cd (4), L=邻菲啰啉]进行了红外光谱、元素分析、热重分析表征工作. 热重分析表明配合物14中DTC配体比中性配体更易失去, 热分解最终产物为相应的氧化物. 对化合物1, 2做了X-ray单晶衍射分析, 1为单斜晶系, P21/c空间群, 晶胞参数a=0.72146(5) nm, b=2.61720(18) nm, c=1.59438(11) nm,b=97.899(2)°, V=2.9820(4) nm3, Z=4, m=1.133 mm-1, Dc=1.297 Mg•m-3; 2为三斜晶系, P-1空间群, 晶胞参数a=1.0075(2) nm, b=1.1580(2) nm, c=1.1777(2) nm, a=70.92(3)°, b=85.71(3)°, γ=81.02(3)°, V=1.2822(4) nm3, Z=2, m=2.118 mm-1, Dc=1.630 Mg•m-3.  相似文献   

6.
刘琦  徐正  郁开北 《无机化学学报》2006,22(6):1095-1098
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.  相似文献   

7.
通过新合成的吡啶基羧酸席夫碱配体(5-(吡啶基-3-亚甲基氨基)间苯二甲酸H2L),和镍盐反应制备了一个新的镍配合物{[Ni(HL)2(H2O)2]·2H2O}n(1),利用元素分析及X-射线单晶衍射对其进行了表征。结构分析结果表明标题化合物属于三斜晶系,P1 空间群,晶胞参数为a=0.764 79(11) nm,b=0.870 49(13) nm,c=1.081 13(16) nm,α=85.583(2)°,β=82.614(2)°,γ=81.565(2)°,V=0.704 82(18) nm3,Z=1,Dc=1.586 g·cm-3,μ=0.763 mm-1,F(000)=350。在配合物的结构中,Ni(Ⅱ)的配位构型为畸变的八面体。配合物中每个配体通过羧酸氧和吡啶氮原子和金属配位形成一维链状结构,并通过体系中丰富的氢键作用链接成为三维框架并加以稳定。  相似文献   

8.
利用水热技术,合成了2个新的配合物{[Co(Hbtc)(Pyphen)(H2O)]·H2O}n (1)和{[Cd2(btc)(Pyphen)2Cl]·2H2O}n(2) (H3btc=1,2,4-苯三酸,Pyphen=[2,3-f]吡嗪并[1,10]-菲咯啉),并通过X-射线单晶衍射、元素分析、热重分析和荧光进行了表征。配合物1属三斜晶系,空间群P1,a=0.643 44(13) nm,b=1.202 9(2) nm,c=1.371 6(3) nm,α=95.03(3)°,β=90.46(3)°,γ=103.54(3)°,V=1.027 7(4) nm3,Z=2,CoC23H16N4O8,Mr=535.31,Dc=1.730 g·cm-3,μ(MoKα)=0.900 mm-1,F(000)=546,GOOF=1.089,R=0.099 2,wR=0.249 0;配合物2属三斜晶系,空间群P1,a=0.968 93(8) nm,b=1.223 82(10) nm,c=1.592 21(14) nm,α=67.486 0(10)°,β=73.158 0(10)°,γ=78.468 0(10)°,V=1.660 9(2) nm3,Z=2,Cd2C37H23N8O8Cl,Mr=967.88,Dc=1.935 g·cm-3,μ(MoKα)=1.432 mm-1,F(000)=956,GOOF=1.051,R=0.077 9,wR=0.141 2。结构分析表明:配合物1为无限一维双链结构,配合物2为二维层状结构。此外,氢键和π-π相互作用在加固配合物的结构中起到重要作用。  相似文献   

9.
合成了3-(水杨酰肼)-丁基-2-酮肟H2L(1,C11H13N3O3)和2个镍的3-(水杨酰肼)-丁基-2-酮肟化合物[Ni(HL)(CH3COO-)(C5H5N)2](2)和[Ni(HL)2]·2C3H7NO(3)。化合物1晶体属单斜晶系,空间群为P21/n,晶体学参数为:a=0.451 87(2) nm,b=2.086 8(1) nm,c=1.224 48(9) nm,β=94.974(3)°,V=1.150 3(1) nm3Z=4,Dc=1.358 g·cm-3,μ=0.101 mm-1F(000)=496,R=0.0435,wR=0.142 5。化合物2晶体属单斜晶系,空间群为P21/n,晶体学参数为:a=1.362 39(8) nm,b=1.345 37(6) nm,c=1.438 54(7) nm,β=113.138(3)°,V=2.424 6(2) nm3Z=4,Dc=1.398 g·cm-3,μ=0.843mm-1F(000)=1 064,R=0.042 4,wR=0.116 6。化合物3晶体属单斜晶系,空间群为P21/c,晶体学参数为:a=1.104 22(7) nm,b=2.860 1(1) nm,c=1.114 13(7)nm,β=114.589(5)°,V=3.199 5(3) nm3Z=4,Dc=1.398 g·cm-3,μ=0.667 mm-1F(000)=1 416,R=0.057 6,wR=0.1535。在化合物1晶体中,酮肟分子之间通过分子间氢键形成二维网状结构。在化合物2中,每个镍(Ⅱ)离子由1个3-(水杨酰肼)-丁基-2-酮肟的2个氮原子和1个氧原子,2个吡啶分子中的2个氮原子和1个乙酸根中的1个氧原子形成畸变的NiN4O2八面体配位构型,存在分子内氢键O-H(肟)…O(乙酸根)和O-H(酚)…N(酰肼)。在化合物3晶体中,每个镍(Ⅱ)离子由2个3-(水杨酰肼)-丁基-2-酮肟的4个氮原子和2个氧原子配位,形成畸变的NiN4O2八面体配位构型。晶体中存在O-H…O和O-H…N两种分子内氢键和O-H…O分子间氢键。  相似文献   

10.
李国鹏  张武  陶偌偈 《无机化学学报》2009,25(12):2215-2219
one new complex, [Cu(aeop)Ni(dpt)(H2O)]·5H2O, [H4aeop=N′-(2-Aminoterephthalic acid)-N″-(1,3-Pro-panediamine) Oxamide], has been prepared by the diffusion method, where (aeop)4- as bridging ligand, dpt as end ligand and characterized by elemental analysis, IR and X-ray crystal structure determination. It crystallizes in the Triclinic system, P1 space group with a=0.885 92(4)nm, b=1.232 53(6)nm, c=1.301 24(6)nm, α=85.593 0(10)°, β=78.753 0(10)°, γ=89.382 0(10)°, V=1.389 43(11) nm3, Z=2. The crystal structure analysis shows that intermolecular O-H…O and N-H…O hydrogen bonds result in a 3D supermolecular construction. The complex was characterized by magnetic susceptibility and presents a antiferromagnetic interaction (J=-46.4 cm-1, g=2.24). CCDC: 727559.  相似文献   

11.
A Cd(II)-nitronyl nitroxide radical complex with dicyanoaurate(I) bridges [Cd(NIT4Py)2][Au(CN)2]2, was synthesized and characterized by elemental analyses, IR spectrum and X-ray diffraction single-crystal structure analysis. Crystal data for the complex: triclinic, space group P1, a=0.720 9(11) nm, b=0.960 3(15) nm, c=1.284(2) nm, α=75.38(2)°, β=85.46(2)°, γ=68.38(2)°, V=0.800(2) nm3, Z=1, and R1 [I>2σ(I)]=0.055 8. The title complex consists of infinite one-dimensional chains of [Cd(NIT4Py)2][Au(CN)2]2, in which [Cd(NIT4Py)2] moieties are conne-cted by [Au(CN)2]- μ2-bridging ligands. Each cadmium(II) ion is six-coordinated in a distorted and centrosymmetric octahedral environment. CCDC: 258357.  相似文献   

12.
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   

13.
Cd(NO3)2·4H2O与配体4′,5′-二氮-9′-(4,5-二(硫乙基)-1,3-二硫杂环戊烯-2-叶立德)-芴(L)在甲醇和二氯甲烷的混合溶剂中生成配合物Cd(NO3)2(L)2。晶体的空间群是Pbcn(#60),晶体学参数分别是a=1.578 7(2) nm,b=0.987 96(11) nm,c=2.719 5(3) nm。V=4.241 6(8) nm3Z=4。2个硝酸根离子各提供1个氧原子,2个配体L各提供2个氮原子,形成了镉的6配位结构。晶体结构显示分子通过平面之间的π-π相互作用沿b轴形成柱状结构,这些柱通过中心原子镉(Ⅱ)的配位连接形成二维层状结构,再通过2个硫乙基上的短距离S…S接触进一步形成了三维结构。对其 1H NMR、UV-Vis和荧光光谱进行了研究。  相似文献   

14.
A dinuclear Cd(Ⅱ) complex [Cdz (N3)2LzCl2]2·H2O (1) [L=4'-(4-eyanophenyl)-2,2':6',2"-terpyridine]was synthesized by reaction of ligand L with CdCl2 and NaN3 using solvothermal method and its structure was determined by X-ray crystal structure analysis. The structure indicates that the complex crystallizes in monoclinic, space group C2/c with a=1.644 5(16) nm, b=1.441 9(12) nm, c=1.9181(18) nm,β=100.349(11)°. V=4474(7) nm3, Z=2, Dc=1.570Mg·m-3,μ=1.120 mm-l, F(000)=2 100, and final R1=0.039 3, wR2=0.0811. The result shows a Cd(Ⅱ) ion was sixcoordinated by a tridentate 4'-(4-cyanophenyl)-2,2' :6',2"-terpyridine ligand and one bridging nitrogen atom of the azide group in the basal position and an chloride atom and the other bridging nitrogen atom of the azide group in the axialone, to form a distorted octahedral-pyramidal geometry. CCDC: 673291.  相似文献   

15.
A novel 1-D Cd(Ⅱ) coordination polymer, [Cd(p-BDOA)·2H2O]n(I) ( p-BDOA2-=benzene-1,4-dioxyacetate dianion) has been synthesized and characterized by elemental analysis, IR, PL, TG and X-ray single crystal diffraction. The Crystal crystallizes in monoclinic system, the space group is C2/c, with the crystal cell parameters a=1.175 1(1) nm, b=0.551 0(1) nm, c=1.827 7(2) nm, β=96.14(2)°, and V=1.176 6(3) nm3,, Mr=372.60, R=0.045 9, wR=0.127 9. The Cd(Ⅱ) ion has a trigonal prism coordination configuration that defined by four carboxyl O atoms from two different p-BDOA2- ligands and two water molecules. Adjacent Cd(Ⅱ) ions are linked by carboxylate groups with the bidentate coordination mode, giving rise to a chain structure with the adjacent Cd…Cd distance of 1.526 3(5) nm. Furthermore, such chains are linked by hydrogen bonds to form supramolecular network. The results of PL and TG show that the complex exhibits intense fluorescent emissions and its chain skeleton is thermally stable up to 419 K. CCDC: 220443.  相似文献   

16.
通过使用浓硫酸对2,2′-二羟基-1,1′-二萘的磺化与成环反应得到一种新配体,7-氧杂-二苯芴-3,11-二磺酸。通过水热方法得到了它的两个化合物,[CdL(bipy)2(H2O)][Cd(bipy)2(H2O)2]·L·H2O (1)和[CdL(phen)2(H2O)]·5H2O (2),并通过X-射线单晶衍射分析进行结构表征。化合物1P1空间群结晶,晶胞参数为a=1.205 5(6),b=1.576 4(8),c=1.954 5(10) nm,α=75.755(9),β=88.093(10),γ=89.035(10)°。化合物2P21/ c空间群结晶,晶胞参数为a=2.104 0(7),b=1.358 0(4),c=1.428 9(5) nm,β=94.543(6)°。在化合物1中,有两个独立的镉(Ⅱ)离子不对称单元,在其中镉(1)离子和两个联吡啶上的四个氮原子,磺酸配体上的一个氧原子及一个水分子配位;镉(2)离子和两个联吡啶上的四个氮原子和两个水分子配位。两种固体化合物在室温下均显示强的蓝色荧光。  相似文献   

17.
A two-dimensional cyanide-bridged Cu(Ⅱ)-Pt(Ⅱ) bimetallic complex has been synthesized by solution diffusion method using [Pt (CN)4]2- and [Cu (L)]2+ (L =3,10-diethanol-1,3,5,8,10,12-hexaazacyclotetradecane) as building blocks. Unexpectedly, the obtained complex Cu(DMF)2[Pt(CN)4] (1) is an analogue of the well-known Hofmann -type clathrate without macrocyclic ligand. Single-crystal X-ray diffraction reveals that 1 crystallizes in monoclinic, space group C2/m, a=1.624 8(6) nm, b=0.739 3(3) nm, c=0.695 5(3) nm, β=108.969(4)°. The crystal structure of 1 consists of two-dimensional corrugated metal cyanide sheets without interpenetration stacking along the a axis in an ABAB packing mode.  相似文献   

18.
报导了四个单核Co(Ⅱ)和Fe(Ⅱ)的配合物[Co(L1)2](ClO4)2·(CH3CN)(1),[Fe(L1)2](ClO4)2·(H2O)(2),[Co(L2)](ClO4)2(3),以及[Fe(L2)](ClO4)2·2H2O(4),(其中L1=4’-苯基-2,2’:6’,2”-三联吡啶,L2=N,N,N-三-(2-(2-吡啶甲叉氨基)乙基)胺)的合成和性质,以及配合物1、3的晶体结构.配合物1和3的晶体都属于单斜晶系.它们的晶胞参数分别为:1a=1.0855(4)nm,b=1.6201(5)nm,c=2.5236(5)nm,β=92.63(2)°,V=4.433(1)nm3;3a=2.8351(8)nm,b=1.0670(3)nm,c=1.9255(5)m,β=101.03(4)°,V=5717(2)nm3.2和4的氧化还原电位分别为E=0.78V和0.63V‘它们的d-d跃迁吸收最大值分别位于565和521nm处.  相似文献   

19.
新型一维麻花状超分子配合物的合成与结构   总被引:7,自引:1,他引:6  
具有特殊结构及性能的超分子化合物由于其结构上的新颖性及潜在的应用价值而成为人们关注的热点 .以一个苯环为间隔基两端含两个吡啶基团的配体 L1与 Pd( ) ,Pt( )形成 2 -索烃 [1 ] ,与Cd( NO3) 2 则形成具有一维平面结构的聚合物 [2 ] .以联苯为间隔基的配体 L2在 4 ,4′-二联吡啶共同作用下与 Pd( )形成 2 -索烃 [3] .同样以一个苯环为间隔基两端含两个咪唑基团的配体 L3与 Zn( NO3) 2 ,Ag NO3反应得到新型多聚轮烷配合物 [4,5 ] .研究结果表明 ,配体或配位金属离子等的微小差别即导致形成结构不同的超分子化合物 .但这些超分子…  相似文献   

20.
A palladium(Ⅱ) complex, [PdLCl]2· [PdCl4], [L=4-bromo-2,6-bis(N,N-diethylaminomethylene)pyridine], was synthesized and its crystal structure was determined by X-ray analysis. The complex crystallizes in monoclinic system with space group Cc, a=0.845 1(17) nm, b=1.836 5(4) nm, c=2.715 8(5) nm,β=93.99(3)°, V=4.204 8(15) nm^3, Z=4, R,=0.037 7 and wR2=0.076 9. The coordination geometry of the Pd atom in the cation is a slightly distorted square planar, with one pyridyl N and two N atoms of the diethylamine ligand, together with one Cl atom. The dihedral angle between the square planar (N3PdCl) and the pyridyl ring is 10.3(4)°. CCDC: 623421.  相似文献   

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